CN106673653A - Preparation method for diamond/silicon composite material - Google Patents
Preparation method for diamond/silicon composite material Download PDFInfo
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- CN106673653A CN106673653A CN201710039147.5A CN201710039147A CN106673653A CN 106673653 A CN106673653 A CN 106673653A CN 201710039147 A CN201710039147 A CN 201710039147A CN 106673653 A CN106673653 A CN 106673653A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63472—Condensation polymers of aldehydes or ketones
- C04B35/63476—Phenol-formaldehyde condensation polymers
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/428—Silicon
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
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Abstract
The invention relates to a preparation method for a diamond/silicon composite material, which belongs to the field of diamond/silicon composite materials. Under a vacuum condition, the preparation method adopts a silicon vapor phase permeation method to prepare the diamond/silicon composite material. Diamond particles, silicon powder and binder are first mixed according to appropriate proportions, wetted by adopting an organic solvent and then mixed by a mixer, so that raw mixed powder is prepared, the mixed powder is then prepressed to be shaped in a press, so that a porous preformed green is prepared, the porous preformed green is then degreased in a tubular furnace, afterwards, the degreased preformed green undergoes the vapor phase permeation of silicon vapor in a vacuum infiltration furnace, so that the porous preformed green is densified, and thereby, the diamond/silicon composite material with good heat-conducting property is obtained ultimately. The process of the preparation method is easy to operate, the efficiency is high, the density of the obtained composite material reaches more than 99 percent, the heat conductivity is 200W/(m.K) to 500W/(m.K), the thermal expansion coefficient is 1.5 to 4.5 multiplied by 10<6>, the strength and hardness of the product are high, and the industrialization of the diamond/silicon composite material can be realized.
Description
Technical field
The present invention relates to a kind of heat-conductive composite material used for electronic packaging, component is mainly made up of diamond and silicon, heat conduction
Rate is high, and thermal coefficient of expansion is small, and intensity and hardness are high, and chemical stability is good, is applicable to as the baseplate material of integrated circuit.
Background technology
Diamond/Si composite is a kind of with high heat conduction, the New Materials for Electric Packing of low heat expansion.It is true
On, this composite has received the concern of more and more researchers.Diamond/Si composite is main by diamond,
Silicon and partially carbonized silicon are constituted.Wherein diamond has thermal conductivity high, low thermal expansivity, electrical insulating property and chemistry in itself
Good stability.With composite prepared by Buddha's warrior attendant masonry heat conduction source, its excellent thermal conductivity, and using silicon as matrix, diamond/
Silicon composite can just match with silicon, arsenic, be good electronic package material, simultaneously as diamond and silicon are belonged to
Ceramic material, chemical stability is good, acid-alkali-corrosive-resisting, good weatherability, therefore, product prepared by this material can be used for various multiple
Miscellaneous environmental condition.
At present, the preparation method of Diamond/Si composite mainly has two kinds, and one kind is high temperature and high pressure method.This method
It is raw material mainly to use diamond, silicon and sintering aid, and silica flour is melted by HTHP, and then between filling diamond
Gap, so as to realize the densification of diamond and silicon, the composite of the Diamond/Si prepared by this method has very high
Compactness and thermal conductivity.The Diamond/Si composite for having research this method of display to obtain can reach 600W/ (mK),
Additionally, composite prepared by this method, physical properties have good performance, are a kind of for Electronic Packaging
Selection well, but some defects for being difficult to overcome there is also by Diamond/Si composite prepared by this method.It is first
First, in order to improve the compactness of material, this method can only be realized by way of improving pressure.Usual this pressure can reach
More than 5G, this composite for resulting in preparation has technique and equipment cost higher, it is difficult to promote open in the industrial production
Come, while the production method of this HTHP makes the shaping of material and densification process integrator, simplify processing step,
But its scope of application is restricted, there is the workpiece of the complicated shapes such as deep camber, wedge angle, effect especially for some
It is often not good, it is therefore necessary to further to be optimized.Another mode for preparing Diamond/Si composite is infiltration
Method, i.e., the porous preforming base of first pre-molding composite at a lower temperature, then passes through molten state under the high temperature conditions
Liquid infiltration fills porous preforming base, and the composite of Diamond/Si is prepared with the behavior for realizing densifying materials.Use at present
Impregnant be mainly the silicon of molten state, infiltration temperature is generally more than the fusing point (1420 DEG C) of silicon.Research display, by infiltration method
The composite of the Diamond/Si of preparation has following facility：
1>, because diamond and silicon have similar crystal structure, liquid silicon has preferable surface wettability with diamond,
Therefore liquid-phase silicone can more easily penetrate into the gap between diamond, can at lower pressures form densification very high
Degree；
2>, large scale, the product of complicated shape can be prepared.Because the forming method of prefabricated blank is many and sintered
Without pressurization in journey, in principle, the size of product is only limited by sintering furnace size, and its complex-shaped degree is molded work by it
Skill is determined；
3>, change in size is small in sample handling processes, and product is completely fine and close；
4>, product process time is short.
This liquid infiltration method, mainly uses liquid silicon, in the presence of capillary force, the side in filling prefabricated blank duct
Formula realizes densification, but in infiltration process, liquid silicon can react generation certain thickness with the carbon in cell walls unavoidably
Carborundum so that the diameter in duct diminishes, so as to hinder the further infiltration of liquid silicon, under serious conditions, the carbon of generation
SiClx can cause that duct closes, and liquid silicon is difficult to penetrate into and is filled up completely with inside duct, so as to be formed in fine and closely woven in material internal
Hole, this compactness for not only resulting in material declines, while can also influence the performances such as the intensity of material, hardness.Research display, mesh
The maximum infiltration thickness of Diamond/Si composite prepared by preceding infiltration method is no more than 5mm, this material for preparing thicker size
Material is unfavorable.
The content of the invention
The present invention prepares Diamond/Si mainly on the basis of liquid-phase infiltrating using the method for vacuum gas-phase infiltration
Composite.
A kind of preparation method of Diamond/Si composite, it is characterised in that using silicon as impregnant, in vacuum condition
Under, silica flour is heated to more than 1420 DEG C.Primary operational process of the invention is：By binding agent organic solvent heating for dissolving,
Silica flour is added thereto and stirred again, bortz powder is subsequently added into and is stirred to pasty state, mixture is then put into ball grinder
In, abrading-ball is added, stirred on batch mixer.Cleaned with organic solvent by the mixed powder after stirring, and by drying,
Broken, sieving technique, obtains evengranular mixed material.Then take appropriate mixed material to be fitted into mould, in press
Upper compacting obtains porous preforming base, and prefabricated blank is then carried out into degreasing in tube furnace, binding agent is decomposed completely, obtains degreasing
Base.Then silica flour will be loaded in the crystal vessel of infiltration in vacuum stove, the suspension of degreasing base is fixed on the top of silica flour, finally to molten
Stove evacuation is oozed, and rises high-temperature, carry out silicon vapor-gas phase infiltration.Sample furnace cooling after the completion of process of osmosis, finally takes out
Sample, obtains the Diamond/Si composite of densification, wherein bortz powder, and the percetage by weight of silica flour and binding agent is：10%
~80%, 10%~70%, 10%~40%.
Further, diamond of the present invention is monocrystalline, the broken powder of glomerocryst or diamond, particle diameter 10~
500μm.Diamond using preceding needing to be cleaned with organic solvent, to remove the impurity on surface.Additionally, in order to increase Buddha's warrior attendant
Stone and the associativity of silicon, can carry out surface corrosion to bortz powder, or necessary surface is modified, and increases the surface of diamond
Roughness.
Further, as matrix silica flour can select metallic silicon power of the purity more than 99.99%, HIGH-PURITY SILICON, or
Person is corresponding silicon alloy, such as Si-Mo, Si-Ti, Si-Tn, Si-Al, Si-Cu etc..
Further, the organic binder bond that the present invention is used includes phenolic resin, epoxy resin, polyvinyl alcohol, paraffin, height
Density polyethylene, polypropylene, stearic acid, polystyrene etc. it is therein one or more.
Further, organic solvent can select absolute ethyl alcohol or acetone.
Rotating speed 800r/min~1500r/min, 4~24h of mixing time, ratio of grinding media to material 10~20 during batch mixing:1.Drying temperature
50~120 DEG C, the mesh of screen cloth 60~3000.
Further, 35~100MPa of pressure during pre-molding, 80~150 DEG C of temperature.
Further, using inert atmosphere or vacuum conditions such as argon gas during degreasing, 2~10 DEG C/min of programming rate takes off
Then 1000~1200 DEG C of fat temperature, 1~2.5h of soaking time cools to room temperature with the furnace.
Further, capital equipment of the present invention is infiltration in vacuum stove.Vacuum during infiltration in below 15Pa,
5~10 DEG C/min of heating rate, 1420~2000 DEG C of holding temperature, 15~90min of soaking time.
Using silicon as impregnant, under vacuum, silica flour is heated to more than 1420 DEG C.Now in closed vessel
Silicon air pressure is raised rapidly, and substantial amounts of silicon steam can be penetrated into the duct of porous preforming base, and upon a drop in temperature, silicon steam can be deposited
And fill up inside duct, so as to realize the densification process of prefabricated blank.Compared to traditional liquid infiltration, the diffusion speed of silicon steam
Faster, permeability-thickness is bigger, has preferable osmotic effect especially for some fine pores, is advantageously implemented the complete of material for degree
It is fine and close.The present invention is that on the basis of many experiments, raw material composition and technological parameter to gas-phase permeation are optimized design,
The quick densifying of product can be in the short period of time realized, is conducive to industrialized production application.In the mistake of gas-phase permeation
Cheng Zhong, with the rising of temperature, silica flour gradually melts and discharges silicon steam, and under vacuum condition, silicon steam expands everywhere in container
Dissipate.Substantial amounts of silicon steam enters in the hole of degreasing blank, and gradually penetrates into the interconnected pore of deep inside.True
Empty condition, the silicon vapour concentration in closed vessel is high, and diffusion is fast, and the micro gap in base substrate can also be filled by it.Then these
Silicon steam can be adsorbed onto in cell walls, and when temperature begins to decline in duct, silicon steam is gradually deposited, and then temperature continues
Decline, silicon steam forms liquid phase before this, finally condensation forms silicon crystal, so as to fill up the hole of blank, realizes porous degreasing base
The densification completely of body, accordingly, it can be said that the densification process of degreasing blank is silicon steam " evaporation-infiltration-deposition-condensation "
Process.
The beneficial effects of the present invention are, by shaping separated with densification process, can a sub-percolation prepare Various Complex shape
The product of shape, technological operation is simple, efficiency high.Meanwhile, composite obtained by the method for the present invention, consistency reach 99% with
On, thermal conductivity is 200~500W/ (mK), and thermal coefficient of expansion is 1.5~4.5 × 10-6, the intensity hardness of product is high, is conducive to
Realize the industrialization of Diamond/Si composite.
Specific embodiment
Example 1,
The phenolic resin of 0.351g is mixed and heated with the absolute ethyl alcohol of 5ml, is stirred, be completely dissolved phenolic resin.
50 μm of silica flours of 0.403g are added in mixed liquor, are stirred, be eventually adding 2.5g200 μm of single crystal diamond stone flour, stirred
To pasty state, then mixture is put into ball grinder, adds abrading-ball, batch mixing 10 hours on batch mixer, batch mixer rotating speed 800r/
min.Batch mixing is completed, and uses washes of absolute alcohol ball grinder, and is dried in 60 DEG C of baking oven, then with the screen cloth of 1000 mesh to mixed
Compound is sieved, and obtains the mixed powder of uniform particle sizes.Then mixed powder is fitted into the mould of Φ 30mm, is heated to
120 DEG C, and suppressed on the forcing press of 45MPa, obtain the porous preforming base of composite.By prefabricated blank argon gas atmosphere pipe
Ungrease treatment, 1100 DEG C of skimming temp, programming rate 5 DEG C/min, soaking time 90min are carried out in formula stove.Then vacuum is melted
Silica flour is inserted in the crystal vessel for oozing stove, will be fixed at the 5mm of silica flour top by the prefabricated blank of degreasing, then crystal vessel is close
Envelope, then to infiltration stove evacuation.When vacuum at lopa when, start to warm up.5 DEG C/min of heating rate, when temperature reaches
After 1550 DEG C, 45min is incubated, then sample cools to room temperature with the furnace.Open in infiltration stove, take out sample, clean up, obtain
Fine and close Diamond/Si composite.
Example 2
Phenolic resin and acetone soln are mixed, and heating is completely dissolved it, then by silica flour and 50 μm of diamonds,
200 μm of diamond mixing, and stir to pasty state.Wherein phenolic resin, silica flour, 50 μm of diamonds, 200 μm of weight of diamond hundred
Fraction is respectively 15%, 20%, 15%, 50%.Then mixture is put into ball grinder, on the batch mixer of 1000r/min
Batch mixing 5 hours.Batch mixing is completed, and ball grinder is cleaned with acetone, and the mixture that will be obtained is dried in 80 DEG C of baking ovens, then with 1000
Purpose screen cloth is sieved.Then mixture powder is fitted into the mould of 10mm × 40mm, mould is heated to 120 DEG C, plus
Pressure 60MPa, is fixed the porous preforming base of shape.Porous preforming base is carried out into degreasing in vacuum tube furnace, wherein being incubated
1000 DEG C of temperature, soaking time 90min, 5 DEG C/min of programming rate.Then the prefabricated blank of degreasing is put in and has loaded the true of silica flour
Empty infiltration stove, wherein prefabricated blank are placed at the 8mm of silica flour top.Then seal, vacuumize.When vacuum reaches below 15Pa,
Start to warm up, 5 DEG C/min of heating rate.After temperature reaches 1700 DEG C, 30min, then sample furnace cooling are incubated.Open true
Empty infiltration stove, takes out sample, after cleaning, obtains Diamond/Si composite.
Example 3
Polypropylene is mixed with absolute ethyl alcohol, and heating dissolves it, then by 50 μm of diamonds, 50 μm of purity of particle diameter
99.99% HIGH-PURITY SILICON is added in mixed liquor, and heating stirring is to pasty state, the wherein weight percent of polypropylene, diamond, silica flour
Than being 15%, 60%, 25%,.Then mixture is put into ball grinder, abrading-ball is added, in the batch mixer of rotating speed 800r/min
On carry out batch mixing.Batch mixing terminates, and uses washes of absolute alcohol ball grinder, and the mixture that will be obtained to be dried in 100 DEG C of baking ovens, then
It is finely divided with the screen cloth of 1000 mesh.Then the mixing batch mixing after subdivision is fitted into the mould of Φ 30mm, in 120 DEG C of 50MPa
Pressure under carry out pre-molding, obtain porous preforming base.Prefabricated blank is put into the tube furnace of argon gas atmosphere carries out degreasing, takes off
1000 DEG C of fat temperature, degreasing time 90min, 5 DEG C/min of heating rate.Degreasing is completed, and will load silica flour in infiltration in vacuum stove, will
Prefabricated blank suspension is fixed on directly over silica flour at 10mm, is then sealed infiltration in vacuum stove, and vacuumize.When vacuum is less than
During 15Pa, start to warm up, 10 DEG C/min of heating rate, final infiltration temperature be set to 1550 DEG C, 1600 DEG C, 1650 DEG C,
1700 DEG C, 1750 DEG C, soaking time 45min.Insulation terminates, sample furnace cooling.Infiltration in vacuum stove is opened, sample is taken out, clearly
After washing, Diamond/Si composite is obtained.Constituent analysis is carried out to the sample under different infiltrating temperatures respectively, it is found that work as temperature
Degree is higher than 1700 DEG C, and diamond occurs obvious graphitization.
Claims (10)
1. a kind of preparation method of Diamond/Si composite, it is characterised in that using silica flour as impregnant, in vacuum condition
Under, silica flour is heated to more than 1420 DEG C；
Specific operation process is：By binding agent organic solvent heating for dissolving, then silica flour is added thereto and stirred, then
Add bortz powder to stir to pasty state, then mixture is put into ball grinder, add abrading-ball, stirred on batch mixer；
Cleaned with organic solvent by the mixed powder after stirring, and by drying, broken, sieving technique, obtain evengranular
Mixed material；Then take appropriate mixed material to be fitted into mould, compacting obtains porous preforming base on press, then will be prefabricated
Base carries out degreasing in tube furnace, binding agent is decomposed completely, obtains degreasing base；Then by the crystal vessel of infiltration in vacuum stove
Load silica flour, the suspension of degreasing base is fixed on the top of silica flour, finally to infiltration stove evacuation, and rise high-temperature, carry out silicon steaming
Vapour gas-phase permeation；Sample furnace cooling after the completion of process of osmosis, finally takes out sample, obtains the Diamond/Si composite wood of densification
Expect, wherein bortz powder, the percetage by weight of silica flour and binding agent is：10%~80%, 10%~70%, 10%~40%.
2. as claimed in claim 1 a kind of preparation method of Diamond/Si composite, it is characterised in that the diamond for being used
It is monocrystalline, glomerocryst or the broken powder of diamond, 10~500 μm of particle diameter；Diamond is using preceding needing to be entered with organic solvent
Row cleaning, to remove the impurity on surface.
3. as claimed in claim 2 a kind of preparation method of Diamond/Si composite, it is characterised in that bortz powder is carried out
Surface corrosion, or necessary surface is modified, increases the surface roughness of diamond.
4. as claimed in claim 1 a kind of preparation method of Diamond/Si composite, it is characterised in that as the silica flour of matrix
Metallic silicon power from purity more than 99.99%, HIGH-PURITY SILICON, or corresponding silicon alloy.
5. as claimed in claim 1 a kind of preparation method of Diamond/Si composite, it is characterised in that the organic adhesive of use
Agent includes phenolic resin, epoxy resin, polyvinyl alcohol, paraffin, high density polyethylene (HDPE), polypropylene, stearic acid, polystyrene wherein
One or more.
6. as claimed in claim 1 a kind of preparation method of Diamond/Si composite, it is characterised in that organic solvent select nothing
Water-ethanol or acetone.
7. as claimed in claim 1 a kind of preparation method of Diamond/Si composite, it is characterised in that rotating speed during batch mixing
800r/min~1500r/min, 4~24h of mixing time, ratio of grinding media to material 10~20:1；50~120 DEG C of drying temperature, screen cloth 60~
3000 mesh.
8. as claimed in claim 1 a kind of preparation method of Diamond/Si composite, it is characterised in that pressure during pre-molding
35~100MPa, 80~150 DEG C of temperature.
9. as claimed in claim 1 a kind of preparation method of Diamond/Si composite, it is characterised in that during degreasing use argon gas
Or vacuum condition, 2~10 DEG C/min of programming rate, 1000~1200 DEG C of skimming temp, soaking time 1~2.5h, Ran Housui
Stove is cooled to room temperature.
10. as claimed in claim 1 a kind of preparation method of Diamond/Si composite, it is characterised in that the equipment for using for
Infiltration in vacuum stove；Vacuum during infiltration in below 15Pa, 5~10 DEG C/min of heating rate, 1420~2000 DEG C of holding temperature,
15~90min of soaking time.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108257880A (en) * | 2018-01-03 | 2018-07-06 | 北京科技大学 | A kind of infiltration in vacuum method prepares diamond/Si（Al）The process of composite material |
| CN108941541A (en) * | 2018-07-25 | 2018-12-07 | 芜湖昌菱金刚石工具有限公司 | A kind of method that diamond surface forms high-temperature stable coating |
| CN110304628A (en) * | 2019-08-12 | 2019-10-08 | 南昌航空大学 | A method of controllable nano silica is prepared in diamond surface |
| CN110698202A (en) * | 2019-11-08 | 2020-01-17 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide composite material and preparation method and application thereof |
| CN113199410A (en) * | 2021-05-28 | 2021-08-03 | 郑州磨料磨具磨削研究所有限公司 | Preparation method and application of composite material for grinding wheel |
| CN113309512A (en) * | 2021-05-25 | 2021-08-27 | 吉林大学 | Erosion-resistant corrosion-resistant hard alloy mud pulse generator rotor and preparation method thereof |
| CN113416075A (en) * | 2021-07-13 | 2021-09-21 | 华侨大学 | Method for preparing Diamond/SiC composite material |
| CN113735583A (en) * | 2021-10-27 | 2021-12-03 | 河南联合精密材料股份有限公司 | Novel diamond/silicon carbide composite ceramic and preparation method thereof |
| CN114874025A (en) * | 2022-03-28 | 2022-08-09 | 广州德百顺蓝钻科技有限公司 | Diamond water filtering ring and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108257880A (en) * | 2018-01-03 | 2018-07-06 | 北京科技大学 | A kind of infiltration in vacuum method prepares diamond/Si（Al）The process of composite material |
| CN108257880B (en) * | 2018-01-03 | 2020-09-11 | 北京科技大学 | Process method for preparing diamond/Si (Al) composite material by vacuum infiltration method |
| CN108941541A (en) * | 2018-07-25 | 2018-12-07 | 芜湖昌菱金刚石工具有限公司 | A kind of method that diamond surface forms high-temperature stable coating |
| CN110304628A (en) * | 2019-08-12 | 2019-10-08 | 南昌航空大学 | A method of controllable nano silica is prepared in diamond surface |
| CN110698202A (en) * | 2019-11-08 | 2020-01-17 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide composite material and preparation method and application thereof |
| CN110698202B (en) * | 2019-11-08 | 2022-04-05 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide composite material and preparation method and application thereof |
| CN113309512A (en) * | 2021-05-25 | 2021-08-27 | 吉林大学 | Erosion-resistant corrosion-resistant hard alloy mud pulse generator rotor and preparation method thereof |
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| CN113416075A (en) * | 2021-07-13 | 2021-09-21 | 华侨大学 | Method for preparing Diamond/SiC composite material |
| CN113416075B (en) * | 2021-07-13 | 2022-09-30 | 华侨大学 | Method for preparing Diamond/SiC composite material |
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