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Designed with speed in mind.   Their no-glass carbon-fiber construction results in a shaft that’s light, strong, quiet and deadly.


Straight to a variance of +/- .006″ and decked out with high-performance Vanetec vanes for optimum flight trueness.


100% carbon-fiber construction


These arrows come from the factory  31.25″ (We can cut them for you at your desired length)


8.7 gpi weight; .350″ spines; Shaft OD: .298″; Shaft ID: .245″

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15 Best Carbon Fiber Arrow Shafts Bulk of 2021

After hours researching and comparing all models on the market, we find out the Best Carbon Fiber Arrow Shafts Bulk of 2021. Check our ranking below.

2,648 Reviews Scanned

Rank No. #3

SinoArt Carbon Arrows 100% Carton Fiber Shaft 340/400/500 Spine Press-Fit Nocks Vanes Arrows for Bow Pack of 6 or 12 (12pack, 400Spine)

  • ➹SHAFT: Constructed from 100% high-mod carbon, resulting in our lightest micro-diameter shaft available to date. This allows room for more point weight to be used up front which drastically improves flight characteristics and long range, extreme pin point accuracy.
  • ➹FEATHERS: Fletched with Blazer Vanes. Length 2inches,2 orange 1 white.
  • ➹ITEM SPECIFICATIONS: Spine 340/500/Straightness ±.006/ID .224”/OD .29”, come with Aluminum inserts, After adjustment of the shaft length need for glued arrow.
  • ➹CHECKED 100% WITH perfect Laser straightness, also they are equally SPINE CHECKED FOR CONSISTENCY
  • ➹6-pack or 12-pack of 32-inch arrows give you high strength whether it be in the field hunting or on the 3D course

SaleRank No. #13

Carbon Express Maxima XRZ 350 Archery Arrow Shafts – 12 Pack

  • BACKBONE TECHNOLOGY – Integrates thin strands of Kevlar into the weave for added durability and strength to the center of the shaft (Green fibers around the center section). Promotes leading 360 degree spine consistency
  • 100% CARBON WEAVED – Designed for quicker recovery and Tri-spine RED ZONE Technology – For industry leading broad head flight.
  • ULTIMATE LIGHTWEIGHT HUNTING ARROW – Four times more accurate than single spine. Built for speed and a flatter trajectory
  • ITEM SPECIFICATIONS – Stock Length, 31.5”, Size/Diameter, 350/.340” spine, 8.4 gpi, Weight tolerance +/- 1 grain, Straightness factor +/- .0025”, Inside diameter .244” For archers looking for an edge over the competition
  • READY TO GO – 12 Pack shafts, heavy enough to carry to far-off targets, and light enough to zip through the air all with high end Carbon Express top notch quality!

Rank No. #14

12 Pack 500 Spine 30 Inch Archery Red Pattern Carbon Arrow Shafts with Aluminum Inserts for Compound Recurve Bows Target Practice(30inch 12pack)

  • Red gold foil pattern decor the products unique design good looking easy to spot while shooting plus accurate and functional
  • Contain with rotated plastic knocks and glued-in insert can attach to lighted knocks/arrowheads for your multipurpose
  • Need low draw weight 35-50 lbs 2 length for your choice; please check the Product Description to find your matching size
  • High quality carbon fiber with straightness +/-0.006” inner diameter 0.246” in great weight anti-splinter for safety and long lasting use
  • Low hand shock with good speed in good performance makes flight always pointed the right way perfect for beginner/Arrows DIY

Rank No. #15

Huntingdoor 30″ Archery Carbon Target Arrows Hunting Arrows with Adjustable Nock and Replaceable Field Points for Compound Bow or Recurve Bow (12 Pack)

  • Weight: 36g.OD:7.9mm.ID:6.2mm(0.246). Spine:550-600.Package included:12 pcs carbon arrows.For draw weight of 35-55 pounds compound bow recurve bow.
  • Huntingdoor Carbon Target Arrows, the shaft made of high quality carbon fiber, after many tests, not easy to crack, strong and durable,suitable for compound and recurve bow,perfect hunting targeting archery practice and outdoor shooting arrows
  • Durable smooth carbon shaft,good straightness,improved wall thickness for added durability,good performance and high speed ,low hand shock with good speed.Don’t shot at concrete wall or any hard substance.
  • Screw-on 100 grain field points with standard thread,ready to shoot.Rotatable NOCK,if you want use them for your recurve bow or longbow,you need adjust the orientation of the Nocks.
  • Great plastic fletch make your use more convenient and simple,colored plastic vanes make flight always pointed the right way,reduce air disturbance,helps you shoot more accurately.

Rank No. #16

Targeting Arrows 30” Inch Carbon Fiber Hunting Arrows Outdoors Archery Blue and White Porcelain Shaft with Replace Arrow Tips and Removable Nock for Compound Bow-12 Pcs (Blue and White Porcelain)

  • 30 inch carbon fiber arrow rod, used for composite bow, cross bow, traditional bow and long bow, suitable for field hunting or archery practice.
  • The 100grain replaceable broadhead and detachable nock can provide stable target penetration, which is suitable for children or adults to practice archery.
  • Made of carbon material, it has strong durability and durability, can ensure stable flight and speed, and can be reused.
  • It is very suitable for wild hunting. The bright and conspicuous colors make it easy for you to find the arrow shaft in archery, even in the field with poor vision.
  • If you have any questions or dissatisfaction with our products, please contact us. We will try our best to solve the problem for you and make your shopping free from worries.

Rank No. #18

LQ Industrial Mini Arrow Cutter 3-22mm Red Archery Pipe Tube Cutting Saw Tool for Fiberglass and Carbon Arrow

  • Material: Alloy steel. Packing: 1 pc.
  • Dimensions: 58mm(2.28in)x39mm(1.54in)x19mm(0.75in).
  • Alloy steel material, high strength, durable, simple and easy to operate, cutting sharp and neat.
  • Suitable for cutting 3mm-22mm pipes/arrows.
  • How to use: Put the arrow shaft in the middle of the pulley and tighten the screws manually. Hold the arrow shaft with one hand and turn the arrow cutter with the other hand. Repeat the operation 3-4 times.

SaleRank No. #19

Wlien 30Inch Carbon Arrows for Compound & Recurve Bow Practice Shooting, 500 Spine with Removable Tips (Pack of 12)

  • Specification: Shaft length: 30” (Whole length: 31.5”), Outer diameter: 0.307” (7.8mm), Inner diameter: 0.244” (6.2mm), Weight: 35g, Spine: 500.
  • Material: Carbon fiber arrow. Precision carbon hunting arrows made for extended durability and long lasting target practice.The 100 grain tips are nickel plated stainless steel which is perfect for target practice & outdoor shooting, the screw tips are with insert can be changed.
  • Advantage: The nock are not glued, so it can be adjustable for your bow. The O-ring at the screw tip can prevent the tip from falling.
  • Package: 12 pack of carbon arrows, 6 nocks for free.
  • Used: We recommend using these arrows for draw weight 40-60 pounds recurve bow, compound bow or long bows.

Rank No. #20

REEGOX Carbon Arrows Vital Seeker Hunting Arrows with 100 Grain Field Points Practice Target Arrows for Archery Compound Bows and Recurve Bow (12 Pack)

  • 🟡The Vital Seeker carbon arrow is constructed of a high strength carbon fiber matrix that delivers unmatched durability, straightness and target penetration.
  • 🟡Highest considerations for quality components will make you feel confident whether you are on the target line or in the field chasing the trophy of a lifetime.
  • 🟡Material: Carbon. Shaft Length: 30inch. Spine: 400. Inner Diameter: 0.244inch(6.2mm).
  • 🟡The 3-inch quality vanes provide superior accuracy in flight. These carbon arrows are field ready with pre-installed inserts and screwed in 100 grain field points.
  • 🟡Nocks are not fixed by glue but tightly assembled. The arrows can be adjustable for your bow by using a coin to rotate. 6 extra nocks for you to replace.

Last update on 2021-10-31 / Affiliate links / Product Titles, Images, Descriptions from Amazon Product Advertising API

How Do You Buy The Best Carbon Fiber Arrow Shafts Bulk?

Do you get stressed out thinking about shopping for a great Carbon Fiber Arrow Shafts Bulk? Do doubts keep creeping into your mind? We understand, because we’ve already gone through the whole process of researching Carbon Fiber Arrow Shafts Bulk, which is why we have assembled a comprehensive list of the greatest Carbon Fiber Arrow Shafts Bulk available in the current market. We’ve also come up with a list of questions that you probably have yourself.

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We provide an Carbon Fiber Arrow Shafts Bulk buying guide, and the information is totally objective and authentic. We employ both AI and big data in proofreading the collected information. How did we create this buying guide? We did it using a custom-created selection of algorithms that lets us manifest a top-10 list of the best available Carbon Fiber Arrow Shafts Bulk currently available on the market.

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  2. Features: What bells and whistles matter for an Carbon Fiber Arrow Shafts Bulk?
  3. Specifications: How powerful they are can be measured.
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  6. Customer Reviews: Closely related to ratings, these paragraphs give you first-hand and detailed information from real-world users about their Carbon Fiber Arrow Shafts Bulk.
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We always remember that maintaining Carbon Fiber Arrow Shafts Bulk information to stay current is a top priority, which is why we are constantly updating our websites. Learn more about us using online sources.

If you think that anything we present here regarding Carbon Fiber Arrow Shafts Bulk is irrelevant, incorrect, misleading, or erroneous, then please let us know promptly! We’re here for you all the time. Contact us here. Or You can read more about us to see our vision.

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Outlaw Fletched 100% Carbon Hunting Arrows 144 pack



The 144 pack box is perfect for dealers looking to sell individual shafts. Boxes come pre-packed, simply unwrap in place on your floor for display ready for sale.

We’ve been asked a million times for a durable 19 Series hunting arrow, that’s affordable, so we went above and beyond to answer the call.

This arrow was designed specifically for the toughest outdoorsman; it was built using superior carbon technology to handle the ruggedness and abuse encountered while hunting–and their price tag will keep you smiling! Designed with the perfect balance of speed and kinetic energy this shaft is extremely versatile for the range or the woods. Just like any Outlaw, they have been tested, beaten, and bloodied–and they keep coming back for more!

Try some, and see for yourself why they’re the only Outlaw that CAN be trusted!

Safety First


.005 Straightness or Straighter

+/- 2 Grain Weight Tolerance


  • Flo-Yellow Nocks – 10 Grains
  • Outlaw Inserts – 14 Grains
  • 2″ Vanes | Flo-Yellow, Red – 21 Grains
  • Shipped in 144 Pack Box

Don’t forget extra components


Not sure what size is right for you. Check out our sizing chart.

Spine Inner Diameter Outer Diameter GPI
300 .2445″ .300″ 9.1
350 .2445″ .297″ 8.6
400 .2445″ .294″ 8.1
500 .2445″ .285″ 7.4
600 .2445″ .278″ 6.8
700 .2445″ .275″ 6.1

Hot Melt is NOT recommended for use with Black Eagle Arrow shafts.
NO Cleaner for Outside or Inside the shaft is recommended! Use Q-Tip or Paper towel.

Arrows – Easton Archery – Best Target & Hunting Arrows Since 1922

What advantage does the X10 have over other shafts?  Are there any disadvantages?

There are several advantages- the smaller diameter of the X10 shaft presents less surface area and a smaller cross section, which is very helpful in windy conditions at longer distances.  The X10 is also designed with three distinct, custom spine zones- and specifically, a less stiff and- importantly- lighter tail section, which improves clearance and finger release consistency, compared to the much stiffer and heavier tail sections of parallel shafts (or even so-called “tri-spine” shafts from other makers). 

Most importantly, the X10 has a high ballistic coefficient – it correctly balances mass weight and momentum for better performance from recurve bows at longer distances, especially in windy conditions.

The main disadvantage of the X10 is the fact that smaller diameter arrows at higher momentum potentials require better target materials to help prevent excess penetration or pass through.  Another factor is that more care is needed when gluing components, which is also due to the small diameter.  For the same reason, removing points requires a little more care and time in order to avoid overheating.  Also, the cost to produce the X10 is considerably more due to the materials and techniques required to hit the required tolerances.

What’s the effect of cutting an X10/ACE from the rear/How come there’s no chart to tell us the effect/Why doesn’t Easton recommend cutting these shafts from the back?

Cutting X10 (or, to a somewhat lower degree, the ACE) shafts from the rear of the shaft results in an effectively stiffer arrow reaction, one that is disproportionate to cutting the same amount from the front of the shaft.  This is because of the long taper on the rear of the shaft, and how the arrow reacts to “loading” on release.  As the shaft is cut from the rear the “tail spine” of the shaft gets stiffer.  However, the exact answer to the effective amount of change varies by a number of variables, the biggest of which is the relative string amplitude at release of the archer – something no chart can account for completely.  Generally, up to one inch can shift the shaft an equivalent of halfway toward the next stiffer shaft size- however, this reduces the effective forgiveness feature of the shaft design, which is why it’s generally not recommended.  Better to use the correct size arrow, or slightly reduce bow weight

What is the best centershot setting for the X10?

A common error made by intermediate shooters using X10 shafts is that they apply “textbook” centershot settings to the X10.  These settings work fine for the shafts weaker than 650, but for stiffer shafts, less centershot is needed than for ordinary parallel shafts.  This is because of the relatively large barrel on the shaft.  The larger size X10’s tend to dynamically self-compensate for centershot and so generally they should be aligned closer to center than conventional shafts.  A simple walk-back test can be used to confirm the correct setting.

Why are there “weight codes” on high end Easton A/C shafts?  Is this important?

With aluminum arrows,, the specific stiffness- the stiffness for a given mass of material- is always exactly the same for a given alloy.  The great thing about aluminum arrows is that you can get shafts to exactly match ones you had 20 years ago and 20 years into the future.

It’s generally not so with carbon fiber arrows, which have a significant stiffness variation in production compared to aluminum.  In order to cope with this, Easton first specially selects the carbon fiber and does a few proprietary things to eliminate as much of this variation as possible, and then they build shafts of the exact same spine (static stiffness).  Since there’s some variation in the carbon from batch to batch, some shafts of the exact same spine might still be a few grains lighter or heavier than others.  So, Easton goes to the trouble of exactly weight sorting the shafts, putting them in weight categories (C1, C2, etc) to ensure that not only do you have a perfect spine (which is the most important consideration) but the shaft weights are uniform as well.  In addition, they further ensure every dozen shafts are within 0.5 grains.  Frankly, Easton overdoes this a little bit-  there’s so little difference (potentially, none after cutting) between a batch of, for example, category C3 arrows and a batch of category C4 arrows, that once cut, assembled and fletched, they can be mixed with no issues. 

How do you find the best brace height for the recurve bow?

Use your ears!  More often than not, the “best” brace height for a given recurve bow is where that bow shoots most quietly.  Unsurprisingly, this is usually well within the manufacturer’s recommendation range.  Remember, some bows, when braced too high, can become very “twitchy” with respect to vertical stability.   Too low, and armguard/wrist contact may increase considerably.

How much point or shaft should be ahead of the plunger at full draw for recurve?

For a variety of reasons outside the scope of this article, the answer is that at least two centimeters of shaft (not including point) should be past the plunger center at full draw.  More is OK within reasonable limits, but less should be avoided when practical.

What size of tab should archers use?

Tab sizes are generally similar to dress glove sizes.  If one uses a small glove, generally a small tab will do the job.  The important thing to remember is the string should not strike the fingertips on release- if it does, it’s likely that the tab leather is too short.

What leather thickness should a tab be, or how many layers should an archer use?

This is an individual issue for most, but as a general guide, comfort is important and the tab layers should be thick enough to prevent finger pain.  Sometimes, it is possible to get more comfort with fewer layers- for instance, two layers of Cordovan feels about the same as one layer of Cordovan, one layer of thin rubber, and one layer of suede.  However, the two Cordovan layers are thinner overall, last longer, and often behave better in wet weather than a solution incorporating suede backing.

How long or short should the leather be cut on a tab? 

Some top shooters never trim their tabs at all, while some others cut it to the bare minimum.  You can determine the minimum cut length for your (broken-in) tab by heavily dusting it with talc (baby powder), shooting a few shots, and looking to see where the talc has been scraped off by the string.  Usually, a point about 3-4 mm past this ridge of powder represents unused leather which can be trimmed.  However, it’s worth noting that Korean star Park, Sung-hyun’s incredible 1405 FITA World Record score was shot with a completely untrimmed Cavalier tab with a cordovan face.

What size of finger spacer is advised?

This depends on so many variables that it’s hard to give a blanket answer.  However, one should avoid the use of a too-thick spacer, or one that causes pain.  Spacers should be modified as needed to eliminate pain, or even discarded in cases where they cause problems.

Why do so many archers make alterations to their grips?

One reason is that it has become quite stylish to imitate the grips of top shooters.  Changing grips is for some a fun activity and it usually has immediate effects (good or bad!)  So, it has become quite popular to adjust the grip.  The problem is that a lot of people don’t understand all of the issues that manifest themselves when they make big changes to their grip.  For instance, going from a neutral to a high grip changes much more than just the wrist angle- it affects effective draw, shot timing, bow dynamics, and much more!   Interestingly, a number of top shooters shoot unmodified factory grips exclusively.  One reason is that it’s hard to get two custom grips that feel exactly the same.

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Fabrication of three-dimensional interconnected superlattices of nanoparticles and their lithium-ion storage properties – bonds of nature


  • batteries
  • Inorganic chemistry
  • Nano-manufacturing and nano-coating
  • Nanoparticles


Three-dimensional superlattices consisting of nanoparticles represent a new class of condensed materials with collective properties resulting from the interaction of interactions between close-packed nanoparticles.Despite recent advances in self-assembly of nanoparticle superlattices, constituent materials have been limited to those achievable as monodisperse nanoparticles. In addition, self-assembled superlattices of nanoparticles, as a rule, are weakly bound due to the surface coating of the ligands. Here we report on the creation of three-dimensional interconnected superlattices of nanoparticles with face-centered cubic symmetry without preliminary synthesis of the constituent nanoparticles. We show that mesoporous carbon frameworks obtained from self-assembled supercrystals can be used as a reliable matrix for the growth of superlattices of nanoparticles with different compositions.The resulting interlocking nanoparticle superlattices embedded in a carbon matrix are particularly suited for energy storage applications. We demonstrate this by incorporating tin oxide nanoparticle superlattices as anode materials for lithium-ion batteries, and the resulting electrochemical performance is explained by their unique architecture.


Three-dimensional (3D) superlattices consisting of nanoparticles (NPs) are becoming a new and important class of nanostructured materials 1 , the properties of which can be rationally tuned by controlling the size, shape and composition of NPs.In particular, interparticle interactions in NP superlattices can lead to collective properties that are significantly different from isolated NP 1, 2, 3 . The existing methods for growing NP-superlattices are based on self-assembly of monodisperse colloidal NPs caused by solvent evaporation or destabilization of the anti-solvent 1 . Recent progress in self-assembly of NP has been witnessed by the growth of a rich array of single and multicomponent superlattices NP 4.5 , 4.5 , 8 , 9 , 10 , which are widely used in electronic and optoelectronic devices …, catalysis and energy storage.

Self-assembly of colloidal NPs is a complex process involving various driving forces and interactions (for example, van der Waals, Coulomb, Dipolar) 1 . As a consequence, successful assembly of NP superlattices with long-range order requires careful control of many parameters, such as NP size distribution, surface-coating ligands, solvent evaporation kinetics, and so on. In addition, self-assembled NP superlattices usually suffer from poor electrical conductivity due to the large interparticle spacing supported by ligands of capping 1, 11 .Consequently, post-surface treatment such as ligand exchange is necessary to improve electronic adhesion, which unfortunately can lead to serious structural defects such as cracks 12, 13 . Another major obstacle hindering the prospects of NP superlattices is the limited choice of monodisperse NP building blocks, despite recent advances in colloidal synthesis 1, 14 .

In this paper, we report an approach that can overcome the aforementioned limitations associated with self-assembly methods by allowing three-dimensional interconnected, tightly coupled NP superlattices to be grown without first synthesizing the NP constituents.The resulting connected NP superlattices embedded in three-dimensional continuous carbon cages represent a new class of superlattice materials that have shown surprising promise for energy storage applications. Superlattices SnO 2 NP were selected as a model system to study lithium ion storage properties, which exhibit exceptional cyclic stability and speed capability when used as anode lithium ion battery (LIB).


Manufacturing procedure

Figure 1a schematically illustrates the general manufacturing procedure. In short, starting from self-assembled supercrystals Fe 3 O 4 NP, we obtain three-dimensional continuous, highly ordered mesoporous carbon frameworks by carbonization of surface coatings with oleic acid (OA) ligands followed by the removal of NP Fe 3 O 4 . Subsequent impregnation of carbon frameworks with the required precursors leads to 3D NP superlattices upon hydrolysis and / or thermal annealing.The NP constituent composition can be modulated by selecting suitable precursors, while the NP size can be adapted by controlling the size of the original NP Fe 3 O 4 . The reason for choosing NP Fe 3 O 4 as the starting material is that the scalable production of Fe 3 O 4 NP superlattices can be achieved by self-assembly 14, 15 . In addition, Fe 3 O 4 is an inexpensive and thermally stable material that can be easily removed by acid etching.

( and ) Schematic representation of the manufacturing procedure (sectional view). ( b , c ) SEM and HRSEM images of carbonized supercrystals Fe 3 O 4 NP, respectively. Scale bars, 1 μm and 200 nm, respectively. ( d ) SAXS structures of carbonized supercrystals Fe 3 O 4 NP and mesoporous carbon frameworks, respectively. ( d , e ) TEM images of mesoporous carbon cages with different lattice projections.Bar scale, 50 and 20 nm, respectively. Inset at ( e ) is a slightly magnified SEM image of mesoporous carbon scaffolds. Scale bar, 1 micron. Red arrows at ( f ) indicate interlocking windows. ( g ) adsorption-desorption isotherms N 2 and the corresponding pore size distribution (insert) of mesoporous carbon frameworks. The red arrow indicates small pores corresponding to the interconnected windows observed at ( f ).

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It is worth noting that while the structure of our mesoporous carbon cages appears to be similar to that of previous mesoporous carbons prepared from a solid template (i.e., silica opals or mesoporous silica) 16, 17, 18, 19, 20, 21, 22 , we must emphasize that this is the first preparation of ordered mesoporous carbons from inorganic nanocrystals. There are several unique features associated with this preparation strategy that results in mesoporous carbons with characteristic structural and textural properties.First, surface-coated OA ligands, which are a necessary component for the growth and self-assembly of Fe 3 O 4 nanoparticles, simultaneously serve as a carbon source, forming mesoporous carbon atoms with ultrathin pore walls (~ 2 nm) and such the same topological structure as a supercrystalline template Fe 3 O 4 NPs. This is in stark contrast to previous rigid template approaches where additional carbon precursors (i.e. polymers or prepolymers) must be used to fill the matrix voids, and the resulting mesoporous carbons typically have the reverse structure of template 16, 17.18, 19, 20, 21, 22 . Also, unlike previous approaches, in which silica opals or mesoporous silica act only as a matrix 16 , 17 , 18 , 19 , 20 , 21 , 22 used here NP 3 Fe 3 O 4 also serve as a graphitization catalyst (discussed below), taking into account partially graphite frameworks at low temperatures (500 ° C). More importantly, the unique structure of our carbon cages provides interlocking, tightly coupled NP superlattices that cannot be easily accessed by conventional self-assembly methods.

Mesoporous carbon frameworks

Monodisperse Fe 3 O 4 (~ 11 nm) nanoparticles stabilized with OA are synthesized by the literature method 14 (supplementary Fig.1a), and Fe 3 O 4 NP superlattices are grown using a conventional self-assembly process associated with drying (Supplementary Fig. 1b) 4 . The content of surface-coated OA ligands, determined by thermogravimetric analysis (TGA), is ~ 15.9 wt.% (Supplementary Fig. 1c), which corresponds to a ligand coverage area of ​​~ 3.83 nm -2 (i.e. ~ 1455 OA molecules per NP). Supplementary Note 1). It was found that the preliminary addition of squalane (~ 1 wt%) to the NP solution promotes the growth in grams of microcrystalline NP nanocrystals with well-developed faces 15 , although squalane is not critical for the subsequent formation of mesoporous carbon frameworks (Supplementary Fig.1d). The assembled NP supercrystals are then heated at 500 ° C in an argon atmosphere, producing gray powders resulting from the carbonization of OA (Supplementary Fig.2a). Carbon species account for ~ 11 wt% of NP carbonized supercrystals determined from TGA data (Supplementary Fig. 2b). Scanning electron microscopy (SEM) and high-resolution SEM (HRSEM) establish that both faceted morphology and long-distance ordering NP are well preserved in carbonized supercrystals Fe 3 O 4 NP (Fig. 1b, c and additional Figures 2c– ). e). These results strongly suggest that cracks and other structural defects that have been observed in many previously reported thermally treated NP superlattices 23 , 24 are largely prevented in our experiments, probably due to three-dimensional crystal-like morphology, as well as long distance structural ordering of our supercrystals Fe 3 O 4 NP.The small-angle X-ray scattering (SAXS) pattern of carbonized supercrystals Fe 3 O 4 NP shows at least four scattering peaks, which can be attributed to 111, 220, 311, 420 reflections of well-crystallized face-centered cubes. (FCC) structure (Fig. 1d, black curve), consistent with the highly ordered superlattice structure observed in HRSEM (Fig. 1c and supplementary Fig. 2f). The unit cell parameter calculated from the SAXS data is 22.8 nm.

Etching with HNO 3 or HCl is used to treat carbonized NP supercrystals. Complete removal of Fe 3 O 4 nanoparticles yields black carbon powders after washing and drying (Supplementary Figure 3a) that exhibit a highly ordered porous structure as revealed by SEM (Supplementary Figure 3b) and transmission electron microscopy (TEM, Fig. 1e, f and supplementary figure 3c, d). SAXS (Fig.1d, red curve) and SEM (Fig.1e, inset) indicate that porous carbon frameworks have the same fcc structure and faceted morphology inherited from supercrystals Fe 3 O 4 NP, while the pore size (~ 10 nm) is slightly smaller than the diameter of Fe 3 O 4 NPs, probably due to shrinkage of the framework during pickling processes and / or after drying. Interestingly, high-resolution TEM (HRTEM) and Raman spectroscopy suggest that the pore walls of the carbon frameworks are partially graphite (Supplementary Figure 4), which is notable given the low carbonization temperature (500 ° C).We attribute the formation of partially graphite frameworks at such a low temperature to the use of NPs Fe 3 O 4 , since transition metals such as Fe and Co and the corresponding metal oxides are widely used as catalysts for graphitization 25, 26, 27 . We assume that carbon particles resulting from the thermal decomposition of OA molecules lead to partial reduction of Fe 3 O 4 nanoparticles (most likely, surface atoms) into metallic iron, which simultaneously contributes to the graphitization of the surrounding carbon layers into partially graphite walls since.Despite the thickness of the thin walls (~ 2 nm, additional Figure 4b), the degree of graphitization of carbon frameworks can be further increased by heat treatment at 1200 ° C in argon, converting the pore walls into low-layer graphene, while maintaining structural ordering (Supplementary Fig.4c ). Even more interesting, TEM experiments with tilt along the [011] zone axis clearly show that adjacent pores are connected through small windows with dimensions of ~ 3 nm (Fig. 1f, indicated by red arrows), resulting in a three-dimensional continuous porous structure.Presumably, the formation of interconnected windows is explained by a small sintering of neighboring nanoparticles Fe 3 O 4, occurring in the process of carbonization.

The porous structure of carbon frameworks is additionally characterized by adsorption-desorption isotherms N 2 , which show a type IV curve with an acute stage of capillary condensation occurring in the range of relative pressures (P / P 0 ) 0.8–0.85 (Fig. 1, d). ), a typical feature of mesoporous materials 28 .The Brunauer – Emmett – Teller surface area and pore volume are determined to be ~ 1500 m 2 g -1 and ~ 2.5 cm 3 g -1 , respectively. The pore size distribution curve determined using the Barrett – Joyner – Halenda model assumes a bimodal porous structure (Fig. 1g, inset). Large pores at ~ 10 nm correspond to distant NPs Fe 3 O 4 , while small pores in the 2–4 nm range correspond to interconnected windows observed in TEM.

Interconnected NP superlattices

The continuous three-dimensional porosity and large surface area of ​​the carbon cages are expected to promote diffusion of precursors, which is critical for the subsequent growth of NP superlattices. As a proof of concept, tetraethoxysilane is selected as the precursor for SiO 2 NP superlattices, which are obtained by re-infiltration of the precursor followed by hydrolysis. Notably, detailed structural features such as facets and surface terraces originating from Fe 3 O 4 NP supercrystals are also observed in the product (Fig.2a, b and supplementary fig. 5), which indicates a high degree of NP 3D ordering. The flexibility afforded by this approach and the robustness of the carbon cages make it easy to customize NP formulations by simply selecting suitable predecessors. For example, pure carbon NPs of superlattices can be realized by impregnating carbon frameworks with an aqueous solution of sucrose followed by drying and calcining (Fig. 2c, d). Energy dispersive X-ray spectroscopy (EMF) and elemental mapping confirm that the resulting superlattices consist of carbon nanoparticles (Supplementary Fig.6). As far as we know, this is the first preparation of three-dimensional carbon NPs of superlattices, since monodisperse carbon NPs with a ligand coating are not yet available for self-assembly 29 .

( and ) SEM image of SiO 2 NP superlattices showing faceted morphology. Scale bar, 500 nm. ( b ) HRSEM image of SiO 2 NP superlattices showing surface terraces and NP ordering at large distances.Scale bar, 100 nm. ( c , d ) SEM and TEM images of 3D carbon NP superlattices, respectively. Bar scale, 100 and 50 nm, respectively.

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To further illustrate the generality of the approach, we will fabricate superlattices from crystalline metal oxide nanoparticles such as SnO 2 using SnCl 2 as a precursor. Thermal annealing at 350 ° C in argon is carried out to crystallize the embedded NPs.TEM assumes that the crystallization process does not violate the ordered structure of the SnO 2 NP superlattices (Fig. 3a and additional Fig. 7), while SAXS confirms the fcc geometry with a lattice constant of 21.2 nm (Fig. 3b). Powder X-ray diffraction (XRD, Fig. 3c) and HRTEM (Fig. 3d) establish that the constituents SnO 2 NP are highly crystalline with a tetragonal crystal structure. In addition to SnO 2 , other types of metal oxide nanocrystal superlattices can be prepared in a similar manner using metal alkoxides or anhydrous inorganic salts as precursors.For example, three-dimensional superlattices consisting of anatase nanocrystals TiO 2 are formed by impregnating carbon frameworks with titanium isopropoxide (TIP), followed by hydrolysis and thermal annealing (Supplementary Fig. 8). In addition, NP superlattices of multicomponent phases such as mixed metal oxides and phosphates are also available using a premixed precursor (Supplementary FIG. 9). Apparently, the NP composition can be changed by changing the ratio of the two precursors.For example, superlattices Ti 0.3 Sn 0.7 O 2 NP are obtained when a mixture of SnCl 2 and TIP is used as a precursor, and the uniform distribution of Ti and Sn, as shown by elementary mapping, indicates that that the homogeneous filling of Ti 0.3 Sn 0.70.7 O 2 NP in the carbon frame (Supplementary Fig.9c – e). The ability to fabricate such multiphase NP superlattices is particularly important since they are generally difficult to self-assemble due to the difficulty of producing corresponding monodisperse NPs.

( and ) TEM image of SnO superlattices 2 NP. Scale bar, 20 nm. ( b , c ) SAXS pattern and X-ray diffraction pattern of SnO 2 NP superlattices, respectively. ( d ) HRTEM image of SnO 2 NP superlattices showing high crystallinity of embedded NP SnO 2 . Scale bar, 5 nm. Red arrows indicate NP connections.

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Storage properties of Li-ion

One unique structural feature of NP superlattices resulting from our approach is that neighboring NPs are connected to each other through interconnected windows in carbon cages, as shown in Fig.3d, where the compounds SnO 2 NP can be clearly observed (indicated by red arrows). This connection configuration can significantly improve the electronic coupling between densely packed NP 30, 31 , which is highly desirable for applications requiring high electrical conductivity. Compared to self-organizing NP superlattices, another important feature of our NP superlattices is that the NP constituents are embedded in a continuous and partially graphite carbon matrix. Such a carbon coating can further facilitate electron transport and accommodate changes in NP volume, which is especially beneficial for energy storage devices 32, 33, 34 .To demonstrate this, SnO 2 NP superlattices have been selected as anode materials for LIB, which exhibit superior electrochemical performance in terms of cycling stability and speed. The reason for choosing the superlattices SnO 2 NP is that SnO 2 is attracting more and more attention to the storage of Li ions due to its high theoretical capacity (780 mAh g -1 ) and environmental friendliness 35, 36, 37, 38 , 39, 40, 41, 42, 43, 44 .

To investigate their electrochemical characteristics, LIB anodes based on SnO 2 NP superlattices are cycled based on a half-cell configuration. The carbon content in the SnO 2 NP superlattices is ~ 28 wt%, determined from the TGA data (supplementary Fig.10a). Electron microscopy shows that SnO 2 NP superlattices are uniformly distributed in the electrode with well-preserved structural ordering before the cycle (Supplementary Fig.10b-d). In fig. 4, a shows cyclic voltammograms of SnO 2 NP superlattices in the potential range from 3.0 to 0.05 V (compared to Li / Li + ) at a scan rate of 0.5 mV from -1 . The irreversible peak at 0.75 V in the first lithiation process is explained by the reduction of SnO 2 to Sn, as well as the formation of an interfacial phase of a solid electrolyte (SEI) 39 . The two peaks at 0.7 and 1.3 V in the first delithiation process correspond to the removal of Li x Sn and the partially reversible reaction of SnO 2 with Li + , respectively, in accordance with the previous results 37, 38 .The cyclic stability of SnO 2 NP superlattices was investigated by the galvanostatic charge / discharge method. The first discharge process results in a capacity of 1570 mAh g -1 at a relatively high current density of 600 mA g -1 , while the subsequent charging process provides a capacity of 676 mAh g -1 (Supplementary FIG. 11). This irreversibility is probably caused by the formation of SEI, as well as the incorporation of lithium into carbon cages 36 . Despite the loss of first cycle capacitance commonly seen for SnO 2 36, 37 , our SnO 2 NP superlattices exhibit excellent cyclic stability, which is manifested by maintaining a specific capacity of 640 mAh g -1 after 200 cycles and stabilized Coulomb efficiency of more than 98% from the 10th cycle (Fig.4b). LIB anodes based only on mesoporous carbon frameworks are also tested under the same conditions, which demonstrate a stable capacity at 185 mAh g -1 after 200 cycles (Fig. 4, b, pink curve), which indicates the high capacity of our SnO superlattices 2 NP. primarily refers to the embedded SnO 2 NP. To better evaluate the charge / discharge characteristics of our SnO 2 NP superlattices, we synthesize colloidal NP SnO 2 with a similar diameter (~ 13 nm, supplementary Fig.12) 45 , which are cyclically repeated under the same conditions in control experiments. As expected, uncoated NP SnO 2 showed a rapid capacity decline over 50 cycles (Fig. 4b, olive curve), presumably caused by grinding and / or aggregation of NP SnO 2 in the absence of carbon protection. For comparison, carbon-coated SnO 2 NP (carbon content: ~ 26 wt%) Show better cycling stability, but their capacity quickly disappears below 100 mAh g -1 after 50 cycles (Fig.4b, blue curve). The cyclic characteristics of our SnO 2 NP superlattices are additionally evaluated at different current densities. As shown in fig. 4c, the electrode is capable of delivering a capacity of 300 mAh g -1, even at a current density of 3000 mA g -1 , and a capacity above 850 mAh g -1 is restored when the current density is switched back to 120 mA g -1 … This cyclic stability and speed capability is superior to that of most SnO 2 NP anodes previously reported 38, 39, 40, 41, 42, 43, 44 .

( and ) Typical cyclic voltammograms at a scan rate of 0.5 mV from -1 . ( b ) Cyclic characteristics at a current density of 600 mA g -1 and the corresponding Coulomb efficiency. Cyclic performance of 13 nm SnO 2 NP with and without carbon coating and carbon cages tested under the same conditions are also included for comparison. ( c ) Speed ​​test at current densities in the range from 120 to 3000 mA g -1 .( d ) TEM image and ( e , f ) corresponding EDS elemental display of SnO 2 NP superlattices after 200 cycles, showing the preservation of the ordered structure without NP aggregation. Scale bar, 50 nm.

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The superior battery performance of SnO 2 NP superlattices is due to their unique structural characteristics. First, our NP superlattices exist as micrometer-sized secondary particles inherited from the original Fe 3 O 4 NP supercrystals, which are believed to be the ideal architecture for LIB due to reduced surface areas between active materials and electrolyte 46 , 47 .Second, and perhaps most importantly, three-dimensional graphite carbon scaffolds, combined with interconnected NPs, provide a continuous path for electrons, facilitating electronic bonding within electrode components. In addition, the inherent flexibility of carbon scaffolds can buffer large volumetric expansions of embedded NP SnO 2 during cycles 35, 36 , reducing deformation of the entire electrode.

To investigate the structural evolution of our SnO 2 NP superlattices during cycling, ex situ XRD, SEM, TEM and EDS elemental mapping studies are performed after 200 cycles.Consistent with previous results for SnO 2 – main anodes 35 , 43 , XRD confirms the conversion of SnO 2 NP to Sn Sn after cycling (Supplementary Figure 13a), while broad diffraction peaks imply that the resulting Sn Sn are small in size without agglomeration. SEM shows that the morphology of secondary particles is largely retained after cycling (Supplementary Fig.13b, c), while TEM confirms that Sn-based NPs are homogeneously enclosed in carbon frameworks with good structural ordering without aggregation (Fig.4d-f and Supplementary Fig. 13d). These results strongly suggest that our carbon frameworks effectively suppress agglomeration and grinding of Sn-based nanoparticles, which may explain the superior cyclic stability of our SnO 2 NP superlattices. It should also be noted that the performance of LIB can be further improved by increasing the electrical conductivity of the carbon cages prior to precursor penetration, which can be achieved by increasing the degree of graphitization through heat treatment, as mentioned above.

Thus, we have developed a new approach to fabricating three-dimensionally interconnected, tightly coupled NP superlattices with fcc packing symmetry. The generality of the approach is illustrated by the growth of NP superlattices with different compositions, including oxides, carbon, mixed oxides, and phosphates. We also demonstrate the successful use of SnO 2 NP superlattices as anode materials for LIBs, as well as the excellent stability and cycling ability attributed to their unique architecture (i.e. 3D continuous and graphite carbon coating, NP compounds and supercrystal morphology).Given the fact that the fabrication procedure does not require the preliminary synthesis of monodisperse NP blocks, we expect that in the future a wider range of materials can be prepared in the form of interconnected NP superlattices, which can find various applications in electronics, catalysis and energy storage.,



Oleic acid (OA, 90%), squalane and 1-octadecene (ODE, 90%) were purchased from Aldrich. Sodium oleate was obtained from TCI.Ferric chloride hexahydrate (FeCl 3 6H 2 O), titanium isopropoxide (TIP), anhydrous tin chloride (SnCl 2 ), anhydrous tin tetrachloride (SnCl 4 ), tetraethoxysilane (TEOS), anhydrous zirconium tetrachloride (ZrCl 4 ), cetyltrimethylammonium bromide (CTAB) and triethyl phosphate were purchased from Aladdin. All chemicals were used without further purification.

Synthesis and self-assembly Fe

3 O 4 NPs

Monodisperse OA-stabilized Fe 3 O 4 NPs with a diameter of ~ 11 nm were synthesized in accordance with the published method 14 .In a typical synthesis, 72 g of iron oleate and 11.4 g of OA were dissolved in 400 g of ODE in a three-necked flask, and the resulting solution was heated at 320 ° C in an atmosphere of N 2 in for 1 hour. After cooling to room temperature, ethanol and isopropanol were added to precipitate Fe 3 O 4 nanoparticles, and the precipitates were dispersed in hexane to form a stable colloidal solution with a concentration of ~ 10 mg ml -1 . For self-assembly of Fe 3 O 4 NP supercrystals, squalane (~ 1 wt.%) And then the solvent was allowed to evaporate at ambient conditions. Complete evaporation of the solvent made it possible to obtain faceted supercrystals Fe 3 O 4 NP with dimensions on a micrometer scale.

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Manufacturing of three-dimensional interconnected superlattices NP

Assembled Fe 3 O 4 NP assembled supercrystals were heated in a quartz tube furnace at 500 ° C for 2 hours in argon, converting the surface-coated ligands to carbon.Then the carbonized NP supercrystals are refluxed in a solution of HNO 3 or HCl to remove the embedded NP Fe 3 O 4 . The resulting mesoporous carbon frameworks obtained by centrifugation are washed with deionized water to obtain black powders after drying. To grow interconnected NP superlattices, dried porous carbon frameworks were impregnated with the desired precursors by wet impregnation followed by hydrolysis and / or thermal annealing.

Preparation of SiO superlattices

2 NP

5 mg of dried mesoporous carbon powder was dissolved in 1 ml of TEOS. After stirring for 6 hours, the precipitated powder collected by centrifugation was washed with ethanol to remove excess TEOS. Hydrolysis of TEOS was caused by the addition of ammonia hydroxide, resulting in the conversion of TEOS to SiO 2 . This soak / wash cycle was repeated twice to completely fill the SiO 2 NP carbon cages.

Preparation of carbon nanopowder superlattices

Three-dimensional carbon NP-superlattices were synthesized using sucrose as a precursor. Briefly, 0.5 g sucrose and 0.1 g concentrated H 2 SO 4 were first dissolved in 1 ml H 2 O to form a mixture to which 5 mg of dried mesoporous carbon powder was added with constant stirring. After 2 hours, the precipitated powder collected by centrifugation is washed with H 2 O to remove excess sucrose and H 2 SO 4 .Thereafter, the product was placed in an oven at 100 ° C for 2 hours and then at 160 ° C for another 2 hours. The black powder was then impregnated in a diluted sucrose solution (0.05 g sucrose, 0.02 g H 2 SO 4 and 1 ml H 2 O) for 2 hours. After washing and drying, the product was heated under argon atmosphere at 600 ° C for 2 hours to carbonize sucrose, obtaining 3D carbon NP superlattices.

Preparation of SnO superlattices

2 NP

50 mg of mesoporous carbon powder was mixed with a solution of SnCl 2, dissolved in ethanol (0.1 g ml -1 ), and the resulting suspension was stirred for 2 hours.Thereafter, the black powder was collected by centrifugation, and the precipitated powder was washed with ethanol to remove excess SnCl 2 . Hydrolysis of the precursor was initiated by the addition of ammonium hydroxide. This soak / wash cycle was repeated twice to fully load the SnO 2 carbon cages. Thermal annealing at 350 ° C in argon for 1 hour was carried out to crystallize the embedded NP SnO 2 .

Preparation of TiO superlattices

2 NP

TIP was used as a precursor for the production of TiO 2 NP superlattices.Briefly, 50 mg of dried mesoporous carbon powder was mixed with a TIP solution dissolved in isopropanol (0.5 g ml -1 ). After stirring for 6 hours, the black powder was collected by centrifugation, and the precipitated powder was washed with isopropanol to remove excess TIP. The subsequent hydrolysis of TIP was initiated by exposure to air, resulting in the conversion of TIP to TiO 2 . This impregnation / washing cycle was repeated twice to completely fill the carbon cages with TiO 2 .After drying, the product was heated at 350 ° C in an argon atmosphere for 1 hour to crystallize the embedded TiO 2 nanoparticles.

Obtaining superlattices Ti

x Sn 1 – x O 2 NP

A homogeneous mixture of TIP and SnCl 2 with different molar ratios dissolved in ethanol was used as a precursor for the growth of Ti x Sn 1 – x O 2 NP superlattices. In a typical synthesis of superlattices Ti 0.3 Sn 0.7 O 2 NP 0.4 mmol TIP and 0.6 mmol SnCl 2 were dissolved in 1 ml of ethanol to form a homogeneous solution to which 5 mg dried powder of mesoporous carbon with stirring.After 24 hours, the product was centrifuged and washed with ethanol to remove excess precursor. Hydrolysis of the precursor was initiated by the addition of ammonium hydroxide. This impregnation / washing cycle was repeated twice to completely load the carbon cages Ti 0.3 Sn 0.7 O 2 NP. After drying, the product was heated at 350 ° C in argon for 1 hour to crystallize the embedded Ti 0.3 Sn 0.7 O 2 NP.

Preparation of zirconium phosphate NP superlattices

NP superlattices of zirconium phosphate (ZrP) were prepared using a homogeneous mixture of ZrCl 4 and triethyl phosphate as precursor.Briefly, 0.45 mmol of ZrCl 4 and 0.45 mmol of triethyl phosphate were mixed in 2 ml of ethanol to form a homogeneous solution to which 5 mg of dried mesoporous carbon powder was added with vigorous stirring for 2 hours. Thereafter, the product was centrifuged and washed with ethanol to remove excess precursor. The precipitated powder was then placed in an oven at 110 ° C for 2 hours to induce the formation of ZrP NP superlattices.

Synthesis of 13-nm SnO nanoparticles

2 in control experiments

In control experiments, colloidal SnO 2 NPs with a similar size as our SnO 2 NP superlattices were synthesized by a literature method 45 .In a typical synthesis, 10 ml of cationic surfactant (CTAB) solution (0.08 mol l −1 ) was mixed with 10 ml of NH 3 .H 2 O (25% aqueous solution) to form a homogeneous solution , into which 4.65 g of SnCl 4 was added under vigorous stirring. After 4 h, the product was filtered and washed with distilled water for several times. The product was then heated at 400 ° C in air for 2 h to increase the crystallinity, leading to SnO 2 NPs with a mean diameter of 13 nm.Sucrose was used as the carbon source for the formation of carbon-coated SnO 2 nanocomposite. In a typical preparation of SnO 2 / C nanocomposite with a carbon content of ~ 26 wt%, 0.35 g of SnO 2 NPs was mixed with a sucrose solution (0.4 g in 5 ml H 2 O), and the resulting mixture was pre-heated at 180 ° C in an oven for 3 h. The dried powder was then heated in a quartz furnace at 500 ° C for 5 h in argon, resulting into carbon-coated SnO 2 nanocomposite.


TEM images, HRTEM images, scanning TEM images, elemental mapping, and EDS spectra were obtained using a Tecnai G2 20 TWIN microscope operated at 200 kV. SEM images and EDS spectra were recorded using a Zeiss Ultra-55 microscope operated at 5 and 10 kV, respectively. XRD was carried out on a Bruker D4 X-ray diffractometer, while SAXS was performed on a Nanostar U small-angle X-ray scattering system using Cu Kα radiation (40 kV, 35 mA). Nitrogen adsorption – desorption isotherms were recorded on a Tristar 3000 instrument.Before measurements, the samples were degassed at 300 ° C for 5 h. Raman spectra were collected at room temperature on an XploRA Raman system. TGA measurements were carried out on a Perkin – Elmer Pyris 1 thermogravimetric analyzer.

Electrochemical measurements

The battery performance was evaluated by galvanostatic cycling of 2025-type coin cells assembled in an argon-filled glove box, with SnO 2 NP superlattices as the working electrode and lithium foil as the counter and reference electrode.The electrolyte was a 1.0 M LiPF 6 solution in a mixture of ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate (1: 1: 1 in volume), and a polypropylene film (Celgard-2300) was used as the separator. The working electrodes were prepared by a slurry-coating procedure. The slurry consisted of SnO 2 NP superlattices, acetylene black (Super P) and polyvinylidene fluoride binder with a mass ratio of 7: 2: 1 dissolved in N -methyl-2-pyrrolidinone. This slurry was spread on a copper foil, which acted as a current collector.The electrodes were dried at 90 ° C for 4 h in air, and then at 90 ° C in vacuum for another 12 h. Cyclic voltammetry was carried out on an electrochemical workstation (Autolab 204 N), while galvanostatic measurements were performed on a Neware cell test instrument, which was cycled between 0.005 and 3.00 V (versus Li / Li + ) at various current densities.

Additional information

How to cite this article: Jiao, Y. et al. Fabrication of three-dimensionally interconnected nanoparticle superlattices and their lithium-ion storage properties.Indigenous Commun. 6: 6420 doi: 10.1038 / ncomms7420 (2015).

Additional information

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    Additional information

    Supplementary Figures 1-13 and Supplementary Note 1


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Facile Preparation of Internally Self-assembled Lipid Particles Stabilized by Carbon Nanotubes

The following results are a) dispersion stability, b) lipid particle size distribution, c) self-assembly type, and d) evidence for lipid coating of CNTs. The stability of dispersions (Figure 2) was monitored using a 5-megapixel camera with autofocus and LED flash.

Figure 2. Schemes of CNT types (A) MWCNT-OH, (B) MWCNT-COOH, and (C) SWCNT and photographs of the corresponding emulsions. Stable emulsions were obtained only in a specific region (shaded) where the CNT lipid ratio was optimal; below and above a stable emulsion is not formed due to too few or too many nanotubes, respectively. The arrow indicates a typical CNT lump in an unstable emulsion. These measurements were carried out for the range of DU-CNT dispersions; representative of these are given here (Figure reproduced from Ref. [50] with permission from the Royal Society of Chemistry). Please click here to view a larger version of this figure.

Small angle X-ray scattering (SAXS) patterns were recorded in order to determine the lattice type of the internal nanostructure of stabilized isasomes (3A). SAXSpace chamber connected to analytical X-ray generating equipment (ISO-DEBYEFLEX3003) with a sealed-tube Cu-anode operating at 40 kV and 50 mA. The X-ray tube is cooled using a closed loop of water. The SAXSpace collimation unit converts a diverging polychromatic X-ray beam into a vertically oriented line of a Cu-K & alpha shaped beam radiation with a wavelength, A, of 0.154 nm.For SAXS experiments, a high-resolution mode was chosen, which permits to detect the minimum scattering vector, Q min, 0.04 nm -1 (Q = (4π / λ) sinθ, where 2θ is the scattering angle) … Stopping the semitransparent beam allows you to record the attenuated main beam profile for accurate zero scatter vector determination and transmission correction. Each of the test specimens is enclosed in the same vacuum-tight, reusable 1 mm quartz capillary to ensure exactly the same scattering volume.The capillary was placed in a temperature controlled sampling stage, equipped with a Peltier element that was connected to a water cooling thermostat to get rid of excess heat. All experiments were performed at 25 ° C with a temperature stability of 0.1 ° C. A vacuum pump was used to evacuate the chamber with the sample reaching a minimum pressure of ~ 1 mbar. 1D scattering patterns were recorded from a micro-strip X-ray detector. This detector has one photon count and has a Sensitive area of ​​64 × 8 mm 2, including 1280 channels each with a channel size of 0.05 × 8 mm (V × h).The sample-detector distance was 317.09 mm. Each sample was exposed three times for 300 seconds, and their integral scattering profiles were averaged.

SAXStreat software was used to correct the scattering indicatrix in relation to the position of the primary beam. The SAXS data was further transmitted corrected by setting the attenuated scattering intensity at Q = 0 to unity and subtracting the background using the SAXSQuant software. The scattering vector d was calibrated with silver behenate, which has a known grating spacing of 5.84 nm 69. All recorded diffraction patterns can be indexed with space group Pn3m (diamond bicontinuous cubic phase), in which 110, 111, 200, 211, 220 and 221 reflections were identified (Figure 3A). la The parameter ttice, a, in phase Pn3m was determined by the linear regression method using the following lattice equation

a = 2 π / d NN × √ (h 2 + K 2 + L 2) (1)

where H, K and L are Miller indices.

The size distribution and dispersed particle size of lipids (Figure 3B) were determined using a laser particle size analyer.

Figure 3. > (A) SAXS model of the phase Pn3m observed for bulk Phytantriol (PT) and corresponding dispersions prepared with 5 wt% Pt in excess water using F127 and various CNT stabilizers. The 3-D schematic shown on the right shows portions of the unit cell of phase Pn3m, which is a bicontinuous cubic phase, the structure of which is based on a double diamond (D) type minimum surface.The blue arrows show the water canals meeting at a tetrahedral angle then the hydrophobic and water regions are color coded in yellow and blue respectively. The characteristic peaks for phase Pn3m are indexed as √2, √3, √4, √6, √8, √9 and the corresponding Miller indices are shown in parentheses. All of the above peaks are visible in bulk PT, and the first four reflections are open to dispersion; nevertheless, this is sufficient to determine the nanostructures Pn3m and estimate their lattice parameters.The peaks highlighted by asterisks indicate the coexistence of a cubic phase of the type Ia3d, which usually forms with a low water content, and thus no dispersions are seen. lipid particles with ‘cubic nanostructures’ in their interior are commonly referred to as ‘cubosomes’. (B) Size distribution of cubosomes obtained using various stabilizers as measured by static light scattering. Please click here to view a larger version of this figure.

Interactions between CNTs and lipid particles were studied using Raman spectroscopy (Figure 4). Samples: Carbon nanotubes, lipid and CNT-stabilized lipid particles were dehydrated, first with nitrogen gas and then holding them in a vacuum desiccator for about 20 minutes. The spectra were recorded using a Horiba Jobin-Yvon LabRAM HR800 spectrometer, equipped with an Andora CCD electromagnet (CCD) for light detection and a video camera to guide the spectral collection. The 532 nm excitation line of the Nd: YAG laser was used to collect spectra in the range 100-4,000 cm 1 using a 600 g grating mm – 1 flashed at 750 nm…. A 50X long working distance objective with a NA of 0.50 was used to acquire spectra and the confocal aperture was set at 100 µm. Before starting measurements, the instrument is calibrated with the 520.8 cm 1 silicon spectral line. All spectra were collected at RT (25 ° C) by placing the sample on calcium fluoride slides. Spectra were acquired using a 532 nm laser and accumulated 5 times with 1% exposure for 10 sec. LabSpec 6 spectroscopy software suite is used for raw data preprocessing and immediate data interrogation.

ftp_upload / 53489 / 53489fig4.jpg “/>
Figure 4. Raman spectra for dehydrated (A) pure lipid, MWCNT-COOH and CNT-stabilized lipid nanoparticles containing 5.0 μg / ml MWCNT -COOH, (b) pure lipid, MWCNT-OH and lipid nanoparticles containing 5.0 μg / ml MWCNT-OH, and (C) pure lipid, SWCNT and lipid nanoparticles containing 0.3125 μg / ml SWCNT All curves represent an average of ten spectra, where the intensity, in arbitrary units, is plotted as a function of the wavelength.Vertical lines are used to guide the eyes, and to make it easier to detect blue shifts in the G and G ‘bands. These experiments were carried out for DU. (D) Schematic diagram of the possible finishing of lipids (self-assembly) on a CNT surface (Fig. Reproduced from [50] with permission from the Royal Society of Chemistry). Please click here to view a larger version of this figure.

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Choosing a Casio watch for diving yourself

Imagine, the water column surrounds you from all sides, weightlessness and the ability to move in all directions completely changes the feeling of yourself in space, you are aware of every breath, every moment.

Diving is not just a sport, it is love for life.

In diving, timing is especially important and in this article we will choose a diving watch from Casio


  • Basis of the requirement for a diver’s watch.
  • GWF-A1000C-1AER
  • MTD-1053D-2A
  • BA-110RG-7AER
  • GAW-100-1A
  • GA-2110ET-2AER
  • GA-2000-1A9ER
  • DW-5600SKE-7ER
  • for diver’s watch

Diving watch requirement:

  • Water resistance – more than 100 m.
  • Good readability
  • Materials resistant to water and salt
  • Additional functions – countdown timers, chronometer, etc.


The FROGMAN collection appeared back in 1993. This is a watch from a special collection designed for diving. The new version retains the distinctive asymmetrical design of the diver’s watch. But this is the first analog FROGMAN watch according to ISO standards, it is water resistant up to 200 meters.

Recall :


is an independent, non-governmental, international organization with experts who share best practices and develop voluntary consensus-based standards.

Designed for diving watches ISO 6425


FROGMAN has a Diving mode – a mode in which the hour and minute hands are aligned and move synchronously in the same direction, showing the countdown in real time.The second hand can move in both directions, depending on the display model, it is either underwater or going out to the surface.

The dive log will store up to 30 dive records.

At 3 o’clock, the tide sensor at the selected location on the selected date.

In addition:

  • This is the first watch on a combined bracelet, the length of which can be quickly adjusted, which makes it possible to wear it in everyday life, reducing the size of the wrist.And fluoroelastomer is softer and stronger than ordinary polyurethane and more resistant to the appearance of “salt” stains after prolonged contact with water.
  • The CARBON MONOCOQUE case is lightweight yet incredibly robust; ” monocoque ”- is a single unit together with the back cover, which only adds to the tightness.
  • Buttons are reinforced with extra spacers to withstand high pressure at depth.
  • Bluetooth® provides energy-efficient data transfer at the push of a button.You can connect to a smartphone and access the watch functions.
  • Smartphone time – automatically sets the time when connected to the phone.
  • Super bright backlight.
  • Impact resistance.
  • Resistance to magnetic fields.
  • Solar battery – allows you to recharge the watch battery using any type of lighting.
  • Radio signal reception (Europe, USA, Japan, China) After setting the clock to the local time zone, the watch will receive a radio calibration signal, ensuring that it always shows the correct time.In most countries, daylight saving time is also updated automatically.
  • LED-backlight provides long-term illumination in the dark.
  • Dual Time Display will allow you to see the local time and home time at the same time.
  • World time function displays the current time in major cities around the world. (300 cities in the application)
  • Date and day of the week
  • Stopwatch with the ability to measure up to 24 hours.
  • Timer – 1/1 sec. – 24 hours with a sound signal.The time can be preset from 1 second to 100 hours. The watch can then automatically start counting down at the set time.
  • Phone search function When you press a button on the watch, the smartphone will beep.
  • Automatic calendar.
  • Anti-reflective sapphire crystal.
  • Battery charge indicator.
  • The case is large enough at 56.7 x 53.3 x 19.7 mm to fit medium to large wrists.
  • The watch is assembled in Japan at the high-tech production facility of Casio in Yamagata.

The watch will withstand immersion.


And from the premium model, we will immediately move on to more than budget divers CASIO COLLECTION. The case with a diameter of 42.6 mm, 11.5 mm thick and the bracelet are made of stainless steel.

Steel bezel with anodized aluminum bezel in the color of the dial and minute markers, which visually increases the size of the watch.

Bezel rotation is unidirectional (counterclockwise) and discrete due to the ratchet mechanism.This allows you to mark a period of time on the scale, like on a timer. And turning only counterclockwise will exclude accidental displacement and erroneous timing. The edges of the bezel have protruding edges to prevent the fingers from slipping. One protruding dot, which you can feel, will help you assess the position of the bezel in the dark.

Screw-down transfer head with rubber seal provides 20 bar (200m)

Inside is a precision quartz movement caliber 2115.

Large hands and markers have a Neobrite light accumulator, which will allow you to read the time in the dark.

Functions: hours, minutes, seconds, date.

The discreet design looks presentable on the hand, and the quality and reliability of these divers at a very attractive price will not find competitors.

CASIO Baby-G BA-110RG-7A

One of the most striking Casio collections is Baby-G. Designed mainly for young people who prefer a sporty style.Like everything created by Casio, this watch meets the highest quality standards.

Designers have tried, and we see on the BA-110RG-7A a complex dial with a double time indication – analogue with arrows and digital on the liquid crystal display.

Dial with 3D structure, volumetric hour markers with light-accumulative coating. Volumetric indexes rise beautifully above the dial to add depth.

But the most important thing is water resistance up to 100 meters.The combined housing of a polymer casing and a steel inner container provides reliable protection due to the principle of the floating module, which creates a shock-absorbing effect.

In addition to LED backlighting, which is activated by pressing a button, the indexes have a light-accumulative coating. The dial is protected by mineral glass. Polymer strap – strong and durable with a standard buckle.

The quartz movement 5338 provides accuracy with an error of +/- 30 seconds per month, and the battery will allow you not to worry about replacement for 2 years.

Of course, Casio has endowed this watch with a number of useful functions:

  • Time display in 29 time zones, in 48 major cities in these time zones.
  • GMT
  • Stopwatch with a maximum measurement time of 24 hours and an accuracy of 1/100 sec, measurement modes – SPLIT and ADD.
  • Countdown timer for 24 hours of measurements.
  • Five daily alarms, one with snooze function. Hourly beep.
  • On / Off sound buttons.
  • Automatic calendar that does not require additional settings and shows the date, day of the week and month, which can be set up to 2099.
  • Displays the current time in 12 or 24 format.

Case size 43.4 mm x 46.3 mm, thickness – 15.8 mm

Ideal for an active lifestyle, this watch will take you underwater with ease.

Casio G-Shock GAW-100-1A

The result of the merger of the other two models is the balanced GAW-100-1A with a rich set of features and an affordable price.200 meter water resistance allows you to swim and dive.

Large luminescent markers and hands make it easy to read the time in the dark. Another advantage of the GAW-100 over its brethren is solar power and radio time synchronization. There are a dozen more useful functions on board like:

  • Automatic LED backlight, world time, stopwatch with an accuracy of 1 / 100th of a second up to 1 hour, timer up to 100 minutes with an accuracy of 1 second, 5 daily alarms, turning on / off the sound of buttons, the function of moving arrows will provide easy reading of data from displays by moving the hands, automatic calendar, 12/24-hour time display, battery level display.
  • Shock-resistant construction of the case made of steel and polymer protects the watch from shocks and vibrations.
  • Mineral glass protects the dial.
  • Polymer strap with classic buckle is comfortable and durable.

Diameter 55.1mm x 52.5mm, thickness 16.7mm, weight only 76.0g. Comfortable and reliable above and below water.

G-Shock GA-2110ET-2AER

The first thing you notice is the compact body compared to other G-Shocks.This is made possible with Carbon Core Guard. The casing has a multi-layer structure, and the inner module is enclosed in a polyurethane casing.

Strength achieved through carbon reinforcement. The dial is protected by an anti-reflective tempered mineral glass. Double electroluminescent backlight – for digital and analogue dials, will always make it easy to read the time. And here, too, there is a function of retraction of the arrows, if they overlap the LCD-display.

Durable polyurethane strap with steel buckle.The new strap attachment allows for quick replacement. An octagon-shaped polymer bezel adds a chiseled edge and dynamism to the watch. And of course, water resistance of 200 meters and a dozen useful functions – stopwatch, timer, world time, etc.

Diameter 48.5mmx45.4mm, thickness only 11.8mm. Weight 51g.

G-Shock GA-2000-1A9ER

This watch is protected by a lightweight and ultra-durable carbon-reinforced polyurethane case. The developers have further enhanced the strength of the case by adding carbon reinforcement to the inner polyurethane part.

The construction was reinforced with screws on the bezel for a hexagon and a polymer case back with special projections, which at the same time serve as a frame for attaching the strap.

The protective design of the buttons has also been redesigned and feels softer when pressed. The watch in black and bright yellow accents looks bright and stylish.

And due to the carbon fiber, the watch is practically not felt on the wrist. And the shape and dimensions allow it to be conveniently worn under clothes. The belt deserves special attention.Contrasting performance with black detailing on the outside is noteworthy.

These G-Shocks can now be extended horizontally. And here we have an updated strap mount, which will only take a few seconds to replace.

The multilayer dial is protected by mineral glass. Below it we see an “X” shaped design, transparent yellow arrows and a beveled window at 3 o’clock.

The mode indicator also received angular bevels in a modern style.The analog zone and digital windows are separately illuminated. It’s interesting to watch the LED slowly fade out.

Water resistance 200 meters and a standard set of Casio functions – stopwatch, timer, world time, folding hands for reading information from displays, etc.

G-Shock DW-5600SKE-7ER

Model 2021 in a translucent case made of black inverted dial. Stylistically very far from the usual divers, but they also have a water resistance of up to 200m, which will allow you to swim and dive.

This watch will definitely stand out. The already classic rectangular shape in translucent design looks both futuristic and vintage. The case measuring 48.9 mm x 42.8 mm and 13.4 thick is made of plastic and lead 53 g.

The LED indicator starts flashing immediately when the alarm clock, the end of the countdown timer or stopwatch.

And also:

  • Stopwatch – 1/100 sec.

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