CN109702211A - A kind of ultra-fine carbon dust and its preparation method and application - Google Patents
A kind of ultra-fine carbon dust and its preparation method and application Download PDFInfo
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- CN109702211A CN109702211A CN201910034512.2A CN201910034512A CN109702211A CN 109702211 A CN109702211 A CN 109702211A CN 201910034512 A CN201910034512 A CN 201910034512A CN 109702211 A CN109702211 A CN 109702211A
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Abstract
The present invention relates to a kind of ultra-fine carbon dusts and its preparation method and application, belong to powder technology field.By the way that short carbon fiber is carried out degumming process, ball milling and separation are then carried out under the auxiliary of soft alloy powder, obtain the ultra-fine carbon dust with special construction.The ultra-fine carbon dust epigranular that the present invention obtains, narrow particle size distribution, dispersion performance are good；Ultra-fine carbon dust also retains crystal structure of the carbon fiber on microcosmic, therefore intensity, high conductivity with carbon fiber simultaneously.The excellent characteristic such as inoxidizability.Long, process cycle complexity that present invention successfully solves the process flows of carbon ultrafine crushing technology, equipment investment are big, obvious to the integrity violations of graphite or fibrous crystal structure, and designed and preparation ultra-fine carbon dust is had excellent performance, and preparation process is simple, at low cost.
Description
Technical field
The present invention relates to a kind of ultra-fine carbon dusts, and in particular to a kind of ultra-fine carbon dust and its preparation method and application belongs to carbon
Field of material preparation.
Background technique
Ultra-fine carbon dust (including graphite powder, carbon fiber powder etc.) granularity is less than 10 μm, with fusing point is low, chemical activity is high, magnetic
The characteristics such as property strong, heat transfer is good, abnormal absorption to electromagnetic wave, are mainly used for conductive material (brush, carbon-point etc.), wear-resisting lubrication
Material (dry powder graphitic lubricant, piston cup etc.).Wherein, most noticeable just to belong to carbon fiber powder, it is that a kind of phosphorus content exists
The powdery carbon materials that the carbon fiber filament of 85% or more high-strength and high-modulus amount is obtained through secondary operation, it remains carbon fiber
Numerous excellent properties, and shape is tiny, large specific surface area, is easy to compound with matrix resin progress, it is such as mixed with thermoplastic resin
Conjunction can prepare fibre reinforced thermoplastic resin injection molding material, with thermosetting resin (such as epoxy resin, cyanate ester resin, span tree
Rouge etc.), the mixing such as curing agent can prepare thermosetting property molding compound, casting material, in metal-based carbon fiber composite material, ceramic base carbon fiber
Carbon fiber powder is also widely used in dimension composite material.
The broken and dispersion for making and using the i.e. powder of two hang-ups faced of superfine powder.Currently, the main powder of carbon dust
Broken technique includes the mechanical crushing process such as airflow milling, vibromill, Ball-stirring mill, and disperses that bonus point powder is mostly used to carry out ultrasound point
Scattered, mechanical dispersion, chemical dispersion etc..But superfine technique process flow is long, process cycle is complicated, equipment investment is big, and
The integrality of the crystal structure of meeting considerable damage graphite or carbon fiber, reduces the performances such as lubrication, thermal conductivity.In addition, ultra-fine
Powder in use easy to reunite is such as added in copper powder when preparing in graphite/carbon/carbon-copper composite material, in mixing with mash form
Superfine graphite powder self-assemble in the process causes to be unevenly distributed.
Chinese patent CN 105088421B discloses a kind of preparation method of carbon fiber powder, mainly solves the prior art
Present in the low problem of energy consumption high efficiency, the preparation method of carbon fiber powder used by the invention, including with
Lower step: (1) thermoplastic resin under continuous carbon fibre and molten condition is clipped, grind, be mixed to get carbon fiber-containing powder
The mixture of the last and described thermoplastic resin；(2) with the thermoplastic in the good solvent dissolution said mixture of above-mentioned thermoplastic resin
Property resin；(3) it is separated by solid-liquid separation and obtains the technical solution of the carbon fiber powder, preferably solve the technical problem, can be used for
In the industrial production of carbon fiber powder.
Chinese patent CN 104098081B discloses a kind of preparation process of small draw ratio carbon fiber powder, including following step
It is rapid: A, to prick beam；B, it bonds；C, slice or milling；D, it dissolves；E, it separates；F, it purifies.The invention provides a kind of small draw ratio carbon fiber
The preparation process for tieing up powder creates a kind of completely new production technology, is able to produce out draw ratio and the smaller carbon fiber powder of fineness,
And then the using effect of carbon fiber powder can be greatly improved, promote the development of industry and enterprise.
For the agglomeration traits for solving carbon fiber powder, Chinese patent CN 104088132B discloses a kind of carbon fiber powder surface
Method of modifying, step are first to carry out air calcination pretreatment to carbon fiber powder, then pretreated carbon fiber powder is immersed oxygen
It is modified to change liquid progress surface, finally modified carbon fiber powder is started the cleaning processing to obtain the modified carbon fiber powder in surface, it should
Inventive method, which has obtained modified carbon fiber powder, has good solvent wellability and dispersion stabilization, the interface with matrix compound tense
Binding ability is preferable.
Japan Patent JPH10273882A discloses a kind of side using polyacrylonitrile-based carbon fibre preparation carbon fiber powder
Method first makes polyacrylonitrile-based carbon fibre slow transit through the baking oven for being heated to 600~700 DEG C (by the time according to carbon fiber
Surface density size is 0.5 minute to 8 minutes) to remove the sizing agent on carbon fiber (otherwise carbon fiber is easily bonded when smashing),
Then prescinded, smashed, it is (multiple) grinding obtain carbon fiber powder, the length of this carbon fiber powder is generally 3~300 μm,
But the particle diameter distribution of carbon fiber powder obtained by the patent is wide, partial size is big, and difference of hardness is not suitable for as reinforcing material.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of ultra-fine carbon dust and preparation method thereof and answer
With.
A kind of ultra-fine carbon dust of the present invention, the ultra-fine carbon dust are by degumming carbon fiber under metal powder auxiliary through mechanical force
The broken soft ultra-fine carbon dust obtained, the ultra-fine carbon dust of hard, the ultra-fine carbon dust being embedded in inside metal powder；The metal powder
Non-rigid alloy powder.
A kind of ultra-fine carbon dust of the present invention, the section of the ultra-fine carbon dust of hard is at polygon；The number of edges of the polygon is big
In being equal to 4, the partial size of the ultra-fine carbon dust of hard is 1~3 μm.
In the present invention, soft ultra-fine carbon dust and the ultra-fine carbon dust of hard do not have difference on partial size, but in hardness and stone
There is certain difference, wherein soft ultra-fine carbon dust degree of graphitization for the ultra-fine carbon dust of hard is higher, firmly on Mo Huadu
Degree is more lower, and property is partially soft.This is because degumming carbon fiber has skin-core structure, since the cortex of carbon fiber is than core graphite
Change degree is higher and obvious, therefore hardness is partially soft, but the characteristic of graphite becomes apparent from, such as lubricity；The hardness of core is partially hard, but graphite
Characteristic is weaker.Therefore corresponding soft ultra-fine carbon dust forms for carbon fiber cortex is broken, and property is slightly soft, and degree of graphitization is higher, firmly
The ultra-fine carbon dust of matter, which is mostly that carbon fiber core is broken, to be formed, and property is hard, and degree of graphitization is slightly lower.
Ultra-fine carbon dust provided by the present invention is broken through mechanical force using degumming carbon fiber and obtains, and joined gold when broken
Belong to powder auxiliary, be effectively controlled the particle diameter distribution of ultra-fine carbon dust, makes the ultra-fine carbon dust of gained, epigranular, narrow particle size distribution,
Dispersion performance is good；Soft ultra-fine carbon dust and the ultra-fine carbon dust of hard remain crystal structure of the carbon fiber on microcosmic simultaneously, because
The excellent characteristics such as this intensity, high conductivity, inoxidizability with carbon fiber.
A kind of ultra-fine carbon dust of the present invention, the metal powder are soft alloy powder, the soft alloy be selected from silver, aluminium,
At least one of copper, titanium, iron, manganese, cobalt, nickel, chromium.
Preferably, the soft alloy is selected from least one of copper, iron, nickel.
A kind of preparation method of ultra-fine carbon dust of the present invention；Include the following steps,
Degumming short carbon fiber, soft alloy powder are subjected to ball milling acquisition mixed powder, mixed powder separates up to soft ultra-fine
The ultra-fine carbon dust of carbon dust, hard, the ultra-fine carbon dust being embedded in inside metal powder；
The revolving speed of the ball milling is 220~350r/min；The time of ball milling >=6h；
The mass ratio of the quality sum and ball milling ball of the degumming staple fiber and soft alloy powder is 1:5~8；
The volume ratio of the soft alloy powder and degumming short carbon fiber is 2~19:1~3.
Technical solution of the present invention carries out ball milling to degumming short carbon fiber using soft alloy as soft ball-milling medium, matches
Close rotational speed of ball-mill and ratio of grinding media to material of the invention, can be very good realize carbon fiber fine, obtain uniform particle sizes, narrowly distributing and
Remain soft ultra-fine carbon dust, the ultra-fine carbon dust of hard of carbon fiber microstructure.
The quality sum of preferred scheme, the degumming staple fiber and soft alloy powder and the mass ratio of ball milling ball are 1:
6~7.
Inventors have found that the revolving speed of soft alloy ball milling in other words is not added if it is the short carbon fiber using non-degumming
It is excessively high too low, it can not all obtain required partial size situation, the soft ultra-fine carbon dust of required structure, the ultra-fine carbon dust of hard.
Preferred scheme, the diameter of the degumming short carbon fiber is 6~8 μm, length is 1~4mm.
Further preferred, the diameter of the degumming short carbon fiber is 6~7 μm, length is 2~3mm.
Inventors have found that the length of degumming short carbon fiber also has certain shadow to the structure of the ultra-fine carbon dust of final gained
It rings, fiber is too long, and winding is easy when ball milling and is reunited, and too short, staple fiber can flock together, and increases difficulty for separation.
Preferred scheme, the partial size of the soft alloy are 30~250 μm.
Further preferred, the partial size of the soft alloy is 100~150 μm.
Preferred scheme, the revolving speed of the ball milling are 250~300r/min；The time of the ball milling is 6~14h.
Preferred scheme, the ball milling ball are selected from least one of stainless steel ball, sintered carbide ball and tungsten alloy ball.
Preferred scheme, the diameter of the ball milling ball are 3mm~10mm.
Further preferred, the diameter of the ball milling ball is 3mm~9mm.
Further preferably the ball milling napiform root is added according to ball milling bulb diameter by following proportion, is counted in mass ratio: 3mm:
4mm:5mm:6mm:7mm:8mm:9mm=3~5:7~9:10~12:18~22:10~14:7~9:5~7:1~2.
Preferred scheme, the isolated process include the following steps:
1) mixed powder is crossed into 400~600 meshes, obtains oversize A and screenings B, gained screenings B is that level-one is soft super
Fine carbon powder；The partial size of the soft ultra-fine carbon dust of level-one is 1~3 μm；
2) step 1 gained oversize A is added in alcohol and obtains mixed liquor, be ultrasonically treated 10min~30min, will mix
Liquid vacuum drying, obtains dry powder M, and dry powder M is crossed 400~600 meshes, obtains oversize C and screenings D, described
Screenings D is the soft ultra-fine carbon dust of second level；The partial size of the soft ultra-fine carbon dust of second level is 1~3 μm；
3) it by step 2 gained oversize C under vacuum conditions after 150~300 DEG C of heat treatment 30min~60min, then sets
Treated oversize C is added in alcohol and obtains slurries by 5~10min of isothermal holding in liquid nitrogen, and ultrasonic treatment 10min~
30min after being dried in vacuo slurries, obtains dry powder N, and dry powder N is crossed 400~600 meshes, obtain oversize E and
Screenings F, gained screenings F are the ultra-fine carbon dust of hard, and oversize E is the ultra-fine carbon dust being embedded in inside metal powder, described
The partial size for being embedded in the ultra-fine carbon dust inside metal powder is 1~3 μm.
As a further preference, 400~600 meshes in the step 1), in step 2), in step 3) are selected from ultrasound
Wave stainless steel vibratory sieve, superfine powder separation ultrasonic wave spin vibration sieve, any one in common vibrating screen.
As a further preference, vacuum drying temperature is 60~80 DEG C in the step 2), in step 3).
Carbon fiber is to be piled up by organic fibers such as flake graphites along fiber axial direction, is carbonized and is graphitized
Microcrystalline graphite material obtained from processing, therefore there is soft outside but hard inside characteristic.In mechanical milling process, degumming carbon fiber is first clamped in
It between soft alloy powder, then is crushed, in broken process, the soft carbon-coating selective crushing on carbon fiber surface layer partially enters ball
In grinding jar, remainder is remained in soft alloy powder, participates in further being crushed and inlaying, and internal hard carbon layer is then always
It is embedded between soft alloy powder, it is constantly broken.Therefore, it finally obtains soft ultra-fine carbon dust a part to remain in ball grinder, separately
A part is bonded in soft alloy powder surface, and the ultra-fine carbon dust of hard is then only embedded in soft alloy powder surface and insertion gold
Belong to inside powder.
The ultra-fine carbon dust of either soft or hard maintains the structure of similar carbon fiber in the present invention.Wherein, by
It is much larger than ultra-fine carbon dust in the partial size of soft alloy powder, the soft ultra-fine carbon dust for remaining ball grinder can directly sieve acquisition, institute
It must be the soft ultra-fine carbon dust of level-one of the present invention, and the soft ultra-fine carbon dust for being bonded in soft alloy surface passes through ultrasound
Vibration combines ultrasound screening can be obtained, and gained is the soft ultra-fine carbon dust of second level of the present invention, and is embedded in soft gold
The ultra-fine carbon dust of the hard of metal surface then needs to pass through heat expansion using huge difference of thermal expansion coefficients between graphite and metal powder
After shrinkage processing, separately won in conjunction with ultrasonic vibration, supersonic sieve.
Preferred scheme, the degumming short carbon fiber the preparation method comprises the following steps: by short carbon fiber beam in vacuum or protective atmosphere
Under, degumming short carbon fiber is obtained in 650~800 DEG C of 20~90min of heat preservation.
As a further preference, by short carbon fiber beam under vacuum or nitrogen atmosphere, in 700~800 DEG C keep the temperature 30~
60min obtains degumming short carbon fiber.
In the inventive solutions, the diameter of the length of degumming short carbon fiber and carbon mono-filaments in short carbon fiber beam
It is consistent with length.
Inventors have found that the temperature of degumming has a certain impact to the performance tool of final material, the temperature of degumming, which is crossed, to be exceeded
The low ultra-fine carbon dust that can not all obtain near-sighted carbon fiber structural.
Soft ultra-fine carbon dust is made annealing treatment, obtains superfine graphite powder by a kind of ultra-fine carbon dust of the present invention.
Soft ultra-fine carbon dust is incomplete graphited carbon dust, and by the high temperature anneal, it can be further improved soft
The degree of graphitization of the ultra-fine carbon dust of matter, reduces the hardness of powder.
Preferred scheme, the temperature of the annealing are 650~1000 DEG C, and the time of annealing is 5~30min.
Preferred scheme, the annealing atmosphere are vacuum or protective atmosphere.
The ultra-fine carbon dust being embedded in inside metal powder is applied to preparation by a kind of application of ultra-fine carbon dust of the present invention
Carbon particle enhances metal-base composites.
Of the invention designed and preparation ultra-fine carbon dust, granularity is only 1~3 μm, and narrow particle size distribution, and degree of purity is high,
Structural integrity and it is similar to carbon fiber, therefore its high heat-conductivity conducting for remaining carbon fiber, wearability and anti-oxidant etc. excellent
Characteristic.
Principle and advantage:
(1) raw material selects: using short carbon fiber as raw material, since carbon fiber surface has a large amount of active function
Group, therefore be directly crushed with long carbon fiber, it is easy to reunite between fiber, it can not be crushed, therefore select short carbon fiber, can avoid this
Problem.
(2) processing method of short carbon fiber: degumming-ball milling.Degumming tech is used first, this is because commercially available carbon fiber
Surface cladding solidification colloid layer, it is necessary to by degumming process, to remove carbon fiber surface sizing agent, so that subsequent (grinding) is handled
" constraint/limitation " of sizing agent can be released, and eliminates the impurity and active function groups of carbon fiber surface using degumming tech,
Otherwise percentage of damage is very low.Secondly ball-milling technology is selected, the optimization of rotational speed of ball-mill and mill ball and proportion can be very good to realize carbon
The fine of fiber.
Short carbon fiber is without degumming process or degumming process temperature be excessively high or high-energy ball milling revolving speed is too fast or mistake
Slowly, or hardmetal powder or inappropriate ratio of grinding media to material are selected, all cannot achieve the ultra-fine carbon dust of approximate carbon fiber structural
Preparation.
(3) present invention assists ball milling using soft alloy, and carbon fiber is by organic fibers such as flake graphites along fiber
Axial direction is piled up, and through microcrystalline graphite material obtained from carbonization and graphitization processing, therefore has soft outside but hard inside spy
Property.In mechanical milling process, degumming carbon fiber is first clamped between soft alloy powder, then is crushed, in broken process, carbon fiber surface layer
Soft carbon-coating selective crushing, partially enter in ball grinder, remainder remains in soft alloy powder, participates in further
It is crushed and inlays, and internal hard carbon layer is then embedded in always between soft alloy powder, it is constantly broken.Therefore, it finally obtains soft
Ultra-fine carbon dust a part remains in ball grinder, and another part is embedded in soft alloy powder surface, and the ultra-fine carbon dust of hard is then
It is only embedded in inside soft alloy powder surface and insertion powder.
Ultra-fine carbon dust prepared by the present invention, either soft or hard the structure for maintaining similar carbon fiber.Its
In, the soft ultra-fine carbon dust for remaining ball grinder can directly sieve (partial size of soft alloy powder is much larger than ultra-fine carbon dust) and obtain,
And the soft ultra-fine carbon dust for being bonded in soft alloy surface combines ultrasound screening can be obtained by ultrasonic vibration, and be embedded in soft
The ultra-fine carbon dust of hard of property metal surface then needs after metal powder expands with heat and contract with cold processing, in conjunction with ultrasonic vibration, ultrasound
Screening could obtain.
In the present invention, it on the one hand can effectively be controlled in mechanical milling process using soft alloy powder auxiliary is added
The partial size branch of the soft ultra-fine carbon dust of gained, the ultra-fine carbon dust of hard, on the other hand can also obtain and be embedded in metal powder powder
Internal ultra-fine carbon dust, wherein almost all of excellent characteristics of the soft and ultra-fine carbon dust of hard with carbon fiber, high rigidity,
The characteristics such as highly conductive, high temperature resistant, therefore the material prepared has good greasy property, electric conductivity, high temperature resistance etc., it can
Applying is including the field of industrial production such as lubrication, conduction, metallurgy, refractory material, such as electrographite brush, pure graphite pantograph, conduction
Coating, cell negative electrode material etc., performance are much better than existing using fine graphitic powder as the composite product of raw material.And it prepares
The more existing fine graphitic powder of technique is more simple, and cost is more cheap.In addition soft ultra-fine carbon dust and the ultra-fine carbon dust of hard
It can be applied to according to requirements different fields directly to use, such as by taking carbon slipper graphite as an example, in order to improve the hard of material
Degree and shock resistance, may be selected the ultra-fine carbon dust of hard, and using effect will be much better than the superfine graphite in currently available technology
Powder, although existing graphite powder graphite degree is high, conductive and lubricity is good, and hardness is lower, intolerant to abrasion.And if it is to conduction
With the demanding conductive coating of greasy property or electrographite brush, then resulting soft stone can be made annealing treatment using through soft carbon dust
Ink powder.And the resulting ultra-fine carbon dust being embedded in inside metal powder of the present invention, since outside is metal powder, inside is carbon
Powder is applied to metal-powder as a whole,
It is directly used in the metallic composite of preparation carbon particle insertion, it is uniform to obtain smooth particle by compacting-sintering process
Distribution and the uniform composite material of performance, solve in mixing process that carbon fiber or carbon dust are easy to reunite, are distributed in metallic matrix
The problems such as serious uneven.
In conclusion the present invention, using short carbon fiber as raw material, in conjunction with soft alloy powder, it is suitable to be combined using degumming process
High-energy ball milling raw material and technique and subsequent separating technology not only obtain the ultra-fine carbon dust of structural integrity and approximate carbon fiber, also
Separation obtains soft ultra-fine carbon dust, the ultra-fine carbon dust of hard and the ultra-fine carbon dust being embedded in inside metal powder powder, to make
Three classes powder gives full play to its advantage, obtains high graphitization degree in addition it can which soft ultra-fine carbon dust is carried out graphitization processing
Soft superfine graphite powder, obtains wider array of application.In addition, also can get and be largely internally embedded by the content of control carbon fiber
Such soft alloy of the ultra-fine carbon dust of hard (volume fraction is greater than 90%), then by subsequent aerobic high annealing, it will be internal
Oxidation of coal, to can get porous metals powder.
The present invention attempts for the first time, and the short carbon fiber prepared using degumming process technique passes through the height of appropriate ball milling parameter
Energy ball milling cooperates soft alloy particle diameter distribution controlling agent be added, and prepares ultra-fine carbon dust, and the present invention has preparation process letter
The equal function admirable of all kinds of ultra-fine carbon dusts of single (only degumming, ball milling), low in cost, gained and uniformly, has good market
Prospect.
Detailed description of the invention
Attached drawing 1 is the preparation flow figure of ultra-fine carbon dust provided by the invention；
Attached drawing 2 is the powder SEM pattern for directly obtaining commercially available short carbon fiber by high-energy ball milling in comparative example 1；
Attached drawing 3 is the powder SEM shape for obtaining the short carbon fiber of 1000 DEG C of degumming process by high-energy ball milling in comparative example 2
Looks；
Attached drawing 4 is that the short carbon fiber of 700 DEG C of degumming process is passed through excessively high (600r/min) in comparative example 3.
Attached drawing 5 is that the short carbon fiber through 700 DEG C of degumming process is in 250r/min high-energy ball milling method in embodiment 1, in conjunction with 800
DEG C annealing preparation powder SEM pattern；
Attached drawing 6 is the short carbon fiber 250r/min high-energy ball milling method through 700 DEG C of degumming process in embodiment 1, in conjunction with 800 DEG C
Make annealing treatment the powder Raman map of preparation；In figure, from top to bottom, it is followed successively by ultra-fine carbon dust, carbon fiber, degumming carbon fiber；
Attached drawing 7 is the short carbon fiber 250r/min high-energy ball milling method through 700 DEG C of degumming process in embodiment 1, in conjunction with 800 DEG C
Make annealing treatment the powder size distribution curve of preparation.
Specific embodiment
Below with reference to attached drawing of the invention, technical solution of the present invention is clearly and completely described, it is clear that retouched
The embodiment stated is only a part of the embodiment in technical solution recorded in the present invention, instead of all the embodiments.It is based on
The embodiment of the present invention, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, protection scope of the present invention is belonged to.
Embodiment 1
For the present embodiment 1 using commercially available carbon chopped fiber as object, the diameter of the commercially available short carbon fiber is 7 μm, length 2mm.True
Under empty condition, 700 DEG C of heat preservation 60min carry out degumming process；Then it is high that progress is added into ball-grinding machine together with electrolytic copper powder
Energy ball milling, the partial size of electrolytic copper powder be added are 100 μm；The volume ratio of electrolytic copper powder and degumming short carbon fiber is 4:1, and ball milling turns
Speed be 250r/min, Ball-milling Time 6h, ball milling ball be stainless steel ball, sphere diameter be 3mm~10mm (ball milling bulb diameter 3mm, 4mm,
The mass ratio of 5mm, 6mm, 7mm, 8mm, 9mm are 4:8:11:20:12:8:6:1), the quality of degumming staple fiber and electrolytic copper powder it
With with the mass ratio of ball milling ball be 1:6.
After ball milling is complete, after the powder in ball grinder is collected, chooses ball milling ball, separated.Step 1, mixed powder is set
In carrying out screening process in superfine powder separation ultrasonic wave spin vibration sieve, it is soft to retain screenings, that is, level-one for 400 mesh of sieve minimum mesh number
Ultra-fine carbon dust.Step 2, the copper powder that oversize, that is, surface is embedded in ultra-fine carbon dust is mixed with alcohol, additional ultrasonic treatment 20min,
Maintenance solution temperature is room temperature, then obtains soft ultra-fine carbon dust and surface is residual solution after ultrasound after 60 DEG C of vacuum drying
The copper powder of the ultra-fine carbon dust of hard is stayed, ultrasonic wave spin vibration sieve is further separated by superfine powder and is sieved, sieve minimum mesh number 400
Mesh retains the soft ultra-fine carbon dust of screenings, that is, second level.Step 3, oversize, that is, remained on surface hard ultra-fine carbon dust copper powder is passed through
After 150 DEG C of vacuum heat-preserving 30min, it is placed directly in liquid nitrogen and keeps the temperature 10min, then mixed with alcohol, additional ultrasonic treatment 20min,
Again by the solution after ultrasound after 60 DEG C of vacuum drying, the ultra-fine carbon dust of hard is obtained and the ultra-fine carbon that is embedded in inside electrolytic copper powder
Powder further separates ultrasonic wave spin vibration sieve by superfine powder and carries out screening process, and 400 mesh of sieve minimum mesh number, screenings is hard
The ultra-fine carbon dust of matter, oversize are the ultra-fine carbon dust being embedded in inside electrolytic copper powder.
The ultra-fine carbon dust (mixture of level-one, second level soft ultra-fine carbon dust and the ultra-fine carbon dust of hard) of the gained of the present embodiment 1 its
Pattern is original as shown in figure 5, degumming process combination soft alloy powder and suitable high-energy-milling as we know from the figure
Short carbon fiber beam, which is interrupted, to be in granular form, and partial size is about 1~3 μm.
The Raman map of the ultra-fine carbon dust of the gained of the present embodiment 1 is as shown in fig. 6, Raman spectrum analysis is shown, shown in fig. 5
Kernel structure is approximate with carbon fiber structural, and fault of construction is slightly increased.
The size distribution curve of the ultra-fine carbon dust of the gained of the present embodiment 1 is as shown in fig. 7, grain diameter is 1~3 μm, and granularity
It is narrowly distributing, symmetrical.
Application Example 1
It is copper-based applied to ultra-fine carbon particle enhancing is prepared by the ultra-fine carbon dust inside electrolytic copper powder is embedded in obtained by embodiment 1
Composite material, wherein the ultra-fine carbon dust being embedded in inside electrolytic copper powder application when with electrolytic copper powder as a whole, electrolytic copper powder
Copper substrate is ultimately formed, and ultra-fine carbon dust forms reinforcement.In following mass ratio, the ultra-fine carbon dust that is embedded in inside electrolytic copper powder
Quality refer to the gross mass of ultra-fine carbon dust and electrolytic copper powder.
By the resulting ultra-fine carbon dust being embedded in inside electrolytic copper powder of embodiment 1, the partial size of External electrolytic copper powder is 120 μ
M, by mass percentage: the ultra-fine carbon dust 99.0% being embedded in inside electrolytic copper powder, silicon carbide 1% is with powder is taken, in V-type mixing
Machine mixing, obtains mixed powder.The partial size for wherein matching the silicon carbide taken is 100 μm.By gained mixed powder at room temperature into
Row cold pressing, pressing pressure 450MPa, dwell time 20s, the Cu-base composites green compact of preparation is under hydrogen atmosphere protection
Pressure sintering, in 950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 12 DEG C/min, and pressure 0.85MPa is obtained
Ultra-fine carbon particle enhances Cu-base composites.The consistency of Cu-base composites is 98.3%, bending strength 827MPa.
Embodiment 2
For the present embodiment 2 using commercially available carbon chopped fiber as object, the diameter of the commercially available short carbon fiber is 6 μm, length 2mm.In nitrogen
Under the conditions of gas shielded, 800 DEG C of heat preservation 30min carry out degumming process；Then be added together with reduced iron powder into ball-grinding machine into
Row high-energy ball milling, the partial size of reduced iron powder be added are 150 μm；The volume ratio of reduced iron powder and degumming short carbon fiber is 2:3, ball
Mill revolving speed is 300r/min, and Ball-milling Time 6h, ball milling ball is stainless steel ball and sintered carbide ball, and sphere diameter is 3mm~10mm (ball
The mass ratio of ball radius 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm be 4:8:11:20:12:8:6:1), degumming staple fiber with
The quality sum of reduced iron powder and the mass ratio of ball milling ball are 1:7.
After ball milling is complete, after the powder in ball grinder is collected, chooses ball milling ball, separated.Step 1, mixed powder is set
In carrying out screening process in superfine powder separation ultrasonic wave spin vibration sieve, it is soft to retain screenings, that is, level-one for 500 mesh of sieve minimum mesh number
Ultra-fine carbon dust.Step 2, the iron powder that oversize, that is, surface is embedded in ultra-fine carbon dust is mixed with alcohol, additional ultrasonic treatment 20min,
Maintenance solution temperature is room temperature, then obtains soft ultra-fine carbon dust and surface is residual solution after ultrasound after 60 DEG C of vacuum drying
The iron powder of the ultra-fine carbon dust of hard is stayed, ultrasonic wave spin vibration sieve is further separated by superfine powder and is sieved, sieve minimum mesh number 500
Mesh retains the soft ultra-fine carbon dust of screenings, that is, second level.Step 3, oversize, that is, remained on surface hard ultra-fine carbon dust iron powder is passed through
After 150 DEG C of vacuum heat-preserving 30min, it is placed directly in liquid nitrogen and keeps the temperature 10min, then mixed with alcohol, additional ultrasonic treatment 20min,
The solution after ultrasound is obtained into the iron of the ultra-fine carbon dust of hard and the ultra-fine carbon dust of internal residual hard after 60 DEG C of vacuum drying again
Powder further separates ultrasonic wave spin vibration sieve by superfine powder and carries out screening process, and 500 mesh of sieve minimum mesh number, screenings is hard
The ultra-fine carbon dust of matter, oversize are the ultra-fine carbon dust being embedded in inside iron powder.
The knot of the 2 ultra-fine carbon dust (general designation of level-one, second level soft ultra-fine carbon dust and the ultra-fine carbon dust of hard) of gained of the present embodiment
Structure is similar with carbon fiber, and partial size is 1~3 μm.
Application Example 2
It is iron-based compound applied to ultra-fine carbon particle enhancing is prepared by the ultra-fine carbon dust inside iron powder is embedded in obtained by embodiment 2
Material, wherein the ultra-fine carbon dust being embedded in inside iron powder application when with iron powder as a whole, iron powder ultimately forms Copper substrate, and
Ultra-fine carbon dust forms reinforcement.
The ultra-fine carbon dust inside iron powder will be embedded in obtained by embodiment 2, the partial size of iron powder is 180 μm, by it in room temperature
Under be cold-pressed, pressing pressure 550MPa, dwell time 20s, the ferroalloy green compact of preparation pressurize burning under vacuum protection
Knot, in 750 DEG C of sintering 2h, then is warming up to 1100 DEG C of sintering 2h, and the heating rate of stove and rate of temperature fall be 10~15 DEG C/
Min, pressure 0.45MPa obtain ultra-fine carbonization iron particle enhancing ferroalloy.The consistency of ferroalloy is 98.5%, tensile strength
For 750MPa.
Embodiment 3
For the present embodiment 3 using commercially available carbon chopped fiber as object, the diameter of the commercially available short carbon fiber is 6 μm, length 1mm.True
Under empty condition, 700 DEG C of heat preservation 30min carry out degumming process；Then it is high that progress is added into ball-grinding machine together with electrolytic nickel powder
Energy ball milling, the partial size of electrolytic nickel powder be added are 100 μm；Electrolytic nickel powder and the volume ratio of degumming short carbon fiber are 19:1, ball milling
Revolving speed is 250r/min, and Ball-milling Time 14h, ball milling ball is stainless steel ball and sintered carbide ball, and sphere diameter is 3mm~10mm (ball
The mass ratio of ball radius 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm be 4:8:11:20:12:8:6:1), degumming staple fiber with
The quality sum of electrolytic nickel powder and the mass ratio of ball milling ball are 1:7.
After ball milling is complete, after the powder in ball grinder is collected, chooses ball milling ball, separated.Step 1, mixed powder is set
In carrying out screening process in superfine powder separation ultrasonic wave spin vibration sieve, it is soft to retain screenings, that is, level-one for 500 mesh of sieve minimum mesh number
Ultra-fine carbon dust.Step 2, the nickel powder that oversize, that is, surface is embedded in ultra-fine carbon dust is mixed with alcohol, additional ultrasonic treatment 20min,
Maintenance solution temperature is room temperature, then obtains soft ultra-fine carbon dust and surface is residual solution after ultrasound after 60 DEG C of vacuum drying
The nickel powder of the ultra-fine carbon dust of hard is stayed, ultrasonic wave spin vibration sieve is further separated by superfine powder and is sieved, sieve minimum mesh number 500
Mesh retains the soft ultra-fine carbon dust of screenings, that is, second level.Step 3, oversize, that is, remained on surface hard ultra-fine carbon dust nickel powder is passed through
After 150 DEG C of vacuum heat-preserving 30min, it is placed directly in liquid nitrogen and keeps the temperature 10min, then mixed with alcohol, additional ultrasonic treatment 20min,
The solution after ultrasound is obtained into the nickel of the ultra-fine carbon dust of hard and the ultra-fine carbon dust of internal residual hard after 60 DEG C of vacuum drying again
Powder further separates ultrasonic wave spin vibration sieve by superfine powder and carries out screening process, and 500 mesh of sieve minimum mesh number, screenings is hard
The ultra-fine carbon dust of matter, oversize are the ultra-fine carbon dust being embedded in inside nickel powder.
The knot of the 3 ultra-fine carbon dust (general designation of level-one, second level soft ultra-fine carbon dust and the ultra-fine carbon dust of hard) of gained of the present embodiment
Structure is similar with carbon fiber, and partial size is 1~3 μm.
Application Example 3
It is Ni-based compound applied to ultra-fine carbon particle enhancing is prepared by the ultra-fine carbon dust inside nickel powder is embedded in obtained by embodiment 3
Material, wherein the ultra-fine carbon dust being embedded in inside nickel powder application when with nickel powder as a whole, nickel powder ultimately forms Ni substrate, and
Ultra-fine carbon dust forms reinforcement.In following mass ratio, be embedded in the ultra-fine carbon dust inside nickel powder quality refer to ultra-fine carbon dust with
The gross mass of nickel powder.
By the resulting ultra-fine carbon dust being embedded in inside nickel powder of embodiment 3, wherein the partial size of nickel powder is 180 μm, by quality
Percentage: the ultra-fine carbon dust 96.0% being embedded in inside nickel powder, aluminium oxide 4% are mixed in V-type batch mixer, are obtained with powder is taken
Mixed powder.The partial size for wherein matching the aluminium oxide taken is 120 μm.Gained mixed powder is cold-pressed at room temperature, compacting pressure
Power is 450MPa, dwell time 20s, nickel-base composite material green compact pressure sintering under hydrogen atmosphere protection of preparation,
1000 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 10~15 DEG C/min, and pressure 0.5MPa obtains ultra-fine carbon
Grain enhancing nickel-base composite material.The consistency of nickel-base composite material is 98.2%, tensile strength 1450MPa.
Comparative example 1
1 other conditions of this comparative example are same as Example 1, be only directly using commercially available short carbon fiber as object, without appoint
What is pre-processed, and is added in ball-grinding machine and is carried out high-energy ball milling, the ball of revolving speed 250r/min, Ball-milling Time 6h, ball milling are
Stainless steel ball, sphere diameter are that (ball milling bulb diameter 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm is added in 3mm~10mm according to a certain ratio
Mass ratio be 4:8:11:20:12:8:6:1), the quality sum of degumming staple fiber and soft alloy powder and the matter of ball milling ball
Amount is frequently 1:6.Short carbon fiber is simultaneously unbroken, is sticked at ball milling tank skin, and the pattern of fiber is as shown in Figure 2 after processing.
Comparative example 2
2 other conditions of this comparative example are same as Example 1, be only degumming temperature be 1000 DEG C.It is with commercially available short carbon fiber
Object, 1000 DEG C of degumming process, is added in ball-grinding machine and carries out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 6h,
The ball of ball milling be stainless steel ball, sphere diameter be 3mm~10mm be added according to a certain ratio (ball milling bulb diameter 3mm, 4mm, 5mm, 6mm,
The mass ratio of 7mm, 8mm, 9mm are 4:8:11:20:12:8:6:1), the quality sum of degumming staple fiber and soft alloy powder with
The mass ratio ratio of ball milling ball is 1:6.Short carbon fiber is simultaneously not apparent from broken, and the pattern of fiber is as shown in Figure 3 after processing.
Comparative example 3
3 other conditions of this comparative example are same as Example 1, be only rotational speed of ball-mill be 600r/min.With commercially available short carbon fiber
For object, 700 DEG C of degumming process are added in ball-grinding machine and carry out high-energy ball milling, revolving speed 600r/min, and Ball-milling Time is
6h, the ball of ball milling are stainless steel ball, sphere diameter be 3mm~10mm be added according to a certain ratio (ball milling bulb diameter 3mm, 4mm, 5mm,
The mass ratio of 6mm, 7mm, 8mm, 9mm are 4:8:11:20:12:8:6:1), the quality of degumming staple fiber and soft alloy powder it
With with the mass ratio of ball milling ball be 1:6.Short carbon fiber is simultaneously not apparent from broken, most of to deposit at ball grinder top covers, processing
The pattern of fiber is as shown in Figure 4 afterwards.
Comparative example 4
4 other conditions of this comparative example are same as Example 1, are only that electrolytic copper powder is added without in mechanical milling process, only individually
Using commercially available short carbon fiber as object, under vacuum conditions, 700 DEG C of heat preservation 60min carry out degumming process；It adds it to later
High-energy ball milling, revolving speed 250r/min, Ball-milling Time 6h are carried out in ball-grinding machine, ball milling ball is stainless steel ball, the short fibre of degumming
Dimension is 1:6 with the quality sum of soft alloy powder and the mass ratio ratio of ball milling ball.Carbon fiber, which is agglomerated into, to stick together, unbroken.
It was found from above-mentioned comparative example and shape appearance figure 2-4；Short carbon fiber is without special carbonization treatment or carbonization treatment temperature
Height is spent, soft alloy is added without in mechanical milling process or high-energy ball milling revolving speed is too fast or too slow, or without subsequent anneal
Processing, all cannot achieve the ultra-fine carbon dust of approximate carbon fiber structural.
Comparative example 5
Other conditions are same as Example 1, and only the diameter of commercially available short carbon fiber is 7 μm, length 10mm.In vacuum condition
Under, 700 DEG C of heat preservation 60min carry out degumming process；Then it is added together with electrolytic copper powder into ball-grinding machine and carries out high energy ball
Mill, the partial size of electrolytic copper powder be added are 150 μm；The volume ratio of electrolytic copper powder and degumming short carbon fiber is 2:3, and rotational speed of ball-mill is
250r/min, Ball-milling Time 6h, ball milling ball be stainless steel ball, sphere diameter be 3mm~10mm (ball milling bulb diameter 3mm, 4mm, 5mm,
The mass ratio of 6mm, 7mm, 8mm, 9mm be 4:8:11:20:12:8:6:1), the quality sum of degumming staple fiber and electrolytic copper powder with
The mass ratio of ball milling ball is 1:6.Since short carbon fiber is too long, after leading to 6h ball milling, carbon fiber is too long, and reunion balling-up is unbroken.
Comparative example 6
Other conditions are same as Example 1, and only the diameter of commercially available short carbon fiber is 7 μm, length 1mm.Under vacuum conditions,
700 DEG C of heat preservation 60min carry out degumming process；Then it is added together with electrolytic copper powder into ball-grinding machine and carries out high-energy ball milling, institute
The partial size that electrolytic copper powder is added is 150 μm；The volume ratio of electrolytic copper powder and degumming short carbon fiber is 25:1, and rotational speed of ball-mill is
250r/min, Ball-milling Time 6h, ball milling ball be stainless steel ball, sphere diameter be 3mm~10mm (ball milling bulb diameter 3mm, 4mm, 5mm,
The mass ratio of 6mm, 7mm, 8mm, 9mm be 4:8:11:20:12:8:6:1), the quality sum of degumming staple fiber and electrolytic copper powder with
The mass ratio of ball milling ball is 1:6.Since the additional amount of electrolytic copper powder is excessively high, although fiber occurs to be crushed, separated after broken
The ultra-fine carbon dust arrived is extremely limited.After ball milling is complete, after the powder in ball grinder is collected, chooses ball milling ball, separated.Separation
Step is same as Example 1.After separation, for discovery the present embodiment since soft alloy additional amount is excessive, final gained level-one is soft
The soft ultra-fine carbon dust of ultra-fine carbon dust, second level, the ultra-fine carbon dust of hard amount be considerably less than quality obtained in embodiment, wherein big portion
The carbon dust of part is embedded in soft alloy.
By the resulting ultra-fine carbon dust being embedded in inside electrolytic copper powder of comparative example 6, the partial size of copper powder is 180 μm, by quality
Percentage is embedded in the ultra-fine carbon dust 99.0% inside electrolytic copper powder, and silicon carbide 1% is mixed in V-type batch mixer, obtained with powder is taken
To mixed powder.The partial size for wherein matching the silicon carbide taken is 200 μm.Gained mixed powder is cold-pressed at room temperature, is pressed
Pressing pressure is 450MPa, dwell time 20s, Cu-base composites green compact pressure sintering under hydrogen atmosphere protection of preparation,
In 950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 12 DEG C/min, and pressure 0.35MPa obtains copper-based composite wood
Material.The consistency of Cu-base composites is 98%, bending strength 480MPa.
Comparative example 7
Other conditions are same as Example 1, and only the diameter of commercially available short carbon fiber is 7 μm, length 1mm.Under vacuum conditions,
700 DEG C of heat preservation 60min carry out degumming process；Then it is added together with electrolytic copper powder into ball-grinding machine and carries out high-energy ball milling, institute
The partial size that electrolytic copper powder is added is 150 μm；The volume ratio of electrolytic copper powder and degumming short carbon fiber is 1:1, rotational speed of ball-mill 250r/
Min, Ball-milling Time 6h, ball milling ball be stainless steel ball, sphere diameter be 3mm~10mm (ball milling bulb diameter 3mm, 4mm, 5mm, 6mm,
The mass ratio of 7mm, 8mm, 9mm are 4:8:11:20:12:8:6:1), the quality sum and ball milling of degumming staple fiber and electrolytic copper powder
The mass ratio of ball is 1:6.
After ball milling is complete, after the powder in ball grinder is collected, chooses ball milling ball, separated.Separating step and embodiment 1
It is identical.
Since the soft alloy additional amount that this comparative example 7 is added is very few, lead to the final resulting soft ultra-fine carbon of level-one
Particle diameter distribution wideization of the soft ultra-fine carbon dust of powder, second level, the ultra-fine carbon dust of hard, and be not broken completely there are also few fibers.
By the resulting ultra-fine carbon dust being embedded in inside electrolytic copper powder of comparative example 7, the partial size of copper powder is 180 μm, by quality
Percentage is embedded in the ultra-fine carbon dust 99.0% inside electrolytic copper powder, and silicon carbide 1% is mixed in V-type batch mixer, obtained with powder is taken
To mixed powder.The partial size for wherein matching the silicon carbide taken is 200 μm.Gained mixed powder is cold-pressed at room temperature, is suppressed
Pressure is 450MPa, dwell time 20s, Cu-base composites green compact pressure sintering under hydrogen atmosphere protection of preparation,
950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 12 DEG C/min, and pressure 0.65MPa obtains copper-based composite wood
Material.The consistency of Cu-base composites is 95%, bending strength 450MPa.
Claims (10)
1. a kind of ultra-fine carbon dust, it is characterised in that: the ultra-fine carbon dust is by degumming carbon fiber under metal powder auxiliary through machine
The broken soft ultra-fine carbon dust obtained of tool power, the ultra-fine carbon dust of hard, the ultra-fine carbon dust being embedded in inside metal powder；The metal
The non-rigid alloy powder of powder.
2. a kind of ultra-fine carbon dust according to claim 1, it is characterised in that: the section of the ultra-fine carbon dust of hard is at polygon
Shape；The number of edges of the polygon is more than or equal to 4, and the partial size of the ultra-fine carbon dust of hard is 1~3 μm.
3. a kind of ultra-fine carbon dust according to claim 1, it is characterised in that: the metal powder is soft alloy powder,
The soft alloy is selected from least one of silver, aluminium, copper, titanium, iron, manganese, cobalt, nickel, chromium.
4. the method for preparing a kind of ultra-fine carbon dust as claimed in any one of claims 1 to 3, which is characterized in that including following steps
It is rapid:
By degumming short carbon fiber, soft alloy powder carry out ball milling obtain mixed powder, mixed powder separate up to soft ultra-fine carbon dust,
The ultra-fine carbon dust of hard, the ultra-fine carbon dust being embedded in inside metal powder；
The revolving speed of the ball milling is 220~350r/min；The time of ball milling >=6h；
The mass ratio of the quality sum and ball milling ball of the degumming staple fiber and soft alloy powder is 1:5~8；
The volume ratio of the soft alloy powder and degumming short carbon fiber is 2~19:1~3.
5. a kind of preparation method of ultra-fine carbon dust according to claim 4, which is characterized in that
The diameter of the degumming short carbon fiber is 6~8 μm, 1~4mm of length；
The partial size of the soft alloy is 30~250 μm.
6. a kind of preparation method of ultra-fine carbon dust according to claim 4, which is characterized in that
The revolving speed of the ball milling is 250~300r/min；The time of the ball milling is 6~14h；
The ball milling ball is selected from least one of stainless steel ball, sintered carbide ball and tungsten alloy ball；
The diameter of the ball milling ball is 3mm~10mm.
7. a kind of preparation method of ultra-fine carbon dust according to claim 4, which is characterized in that
The isolated process includes the following steps:
1) mixed powder is crossed into 400~600 meshes, obtains oversize A and screenings B, gained screenings B is the soft ultra-fine carbon of level-one
Powder；The partial size of the soft ultra-fine carbon dust of level-one is 1~3 μm；
2) step 1 gained oversize A is added in alcohol and obtains mixed liquor, be ultrasonically treated 10min~30min, mixed liquor is true
Sky is dry, obtains dry powder M, and dry powder M is crossed 400~600 meshes, obtains oversize C and screenings D, under the sieve
Object D is the soft ultra-fine carbon dust of second level；The partial size of the soft ultra-fine carbon dust of second level is 1~3 μm；
3) by step 2 gained oversize C under vacuum conditions after 150~300 DEG C of 30~60min of heat treatment, then it is placed in liquid nitrogen
Treated oversize C is added in alcohol and obtains slurries, is ultrasonically treated 10~30min, will starch by middle 5~10min of isothermal holding
After liquid vacuum drying, dry powder N is obtained, dry powder N is crossed into 400~600 meshes, obtains oversize E and screenings F, institute
Obtaining screenings F is the ultra-fine carbon dust of hard, and oversize E is the ultra-fine carbon dust being embedded in inside metal powder, described to be embedded in metal
The partial size of ultra-fine carbon dust inside powder is 1~3 μm.
8. a kind of preparation method of ultra-fine carbon dust according to claim 4, which is characterized in that the degumming short carbon fiber
The preparation method comprises the following steps: obtaining degumming in 650~800 DEG C of 20~90min of heat preservation by short carbon fiber beam under vacuum or protective atmosphere
Short carbon fiber.
9. according to a kind of described in any item preparation methods of ultra-fine carbon dust of claim 4~8, which is characterized in that will be soft super
Fine carbon powder annealing, obtains superfine graphite powder；The temperature of the annealing is 650~1000 DEG C, time of annealing is 5~
30min。
10. the application of ultra-fine carbon dust described in any one according to claim 1~3, it is characterised in that: be embedded in metal for described
Ultra-fine carbon dust inside powder, which is applied to preparation carbon particle, enhances metal-base composites.
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| CN118125859A (en) * | 2024-02-29 | 2024-06-04 | 安徽弘昌新材料股份有限公司 | Method for preparing light high-strength pore-adjustable porous carbon brick by using recycled carbon fiber |
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| CN103333473A (en) * | 2013-04-18 | 2013-10-02 | 邱献腾 | Composite material of carbon fibers or carbon fiber powder, and processing process thereof |
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| JPH10273882A (en) * | 1997-03-31 | 1998-10-13 | Toray Ind Inc | Milled carbon fiber and its production |
| CN103333473A (en) * | 2013-04-18 | 2013-10-02 | 邱献腾 | Composite material of carbon fibers or carbon fiber powder, and processing process thereof |
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| CN118125859A (en) * | 2024-02-29 | 2024-06-04 | 安徽弘昌新材料股份有限公司 | Method for preparing light high-strength pore-adjustable porous carbon brick by using recycled carbon fiber |
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