CN105347799B - A kind of preparation method of big particle diameter Diamond/SiC composites - Google Patents
A kind of preparation method of big particle diameter Diamond/SiC composites Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of big particle diameter Diamond/SiC composites, Diamond/SiC composites are made in the method combined using the big particle diameter diamond precast body of one-shot forming with CVI techniques.Using the method increase the particle diameter and volume content of diamond in composite, so as to effectively raise the thermal conductivity of composite.So that thermal conductivity combines composite raising about 30% prepared by CVI methods than curtain coating.Moreover, this method simple production process, controllable, available for industrialized production.
Description
Technical field
The invention belongs to the preparation method of Diamond/SiC composites, and in particular to a kind of big particle diameter Diamond/SiC
The preparation method of composite, is the composite wood that the diamond doped SiC of big particle diameter is prepared using chemical vapor infiltration (CVI)
Material.
Background technology
Diamond/SiC composites have high rigidity, high-wearing feature, low-density, high heat conductance, low-thermal-expansion system because of it
The advantages of several, good high-temperature stability and be widely applied to PDC high-abrasive materials, resistance to compression bottom felt, petroleum machinery drill bit, reflection
Among mirror substrate and electronic package material.Among these due to highly thermally conductive, low-thermal-expansion that Diamond/SiC composites have
Property and the characteristic such as low-density allow it as forth generation electronic package material, so as to adapt to current high performance chipses and extensive
And use and high integration, high packaging density and the senior engineer's working frequency pair of electronic device chip of super large-scale integration
The requirement of encapsulating material.
Preparing the main technique of Diamond/SiC composites at present mainly has：HTHP sintering (HPHT), reaction are molten
Body infiltration gas-phase silicon (RMI), HIP sintering (HIP), precursor synthesis method conversion method (PIP) and discharge plasma sintering
(SPS) etc..But or these methods are requirement and the degree of danger height to equipment, it is difficult to large-sized Diamond/ is made
SiC sheet materials.It is to have residual silicon in obtained sample so that the mechanical properties decrease of product.In addition, due to top
The preparation temperature of method is universal higher, and this causes diamond easily to occur graphitization, have a strong impact on composite mechanical property and
Thermophysical property.
The problem of in order to solve mentioned above, document " Yongsheng Liu and Chenghao Hu
Microstructure and properties of diamond/SiC composites prepared by tape-
casting and chemical vapor infiltration process[J].J.Eur.Ceram.Soc.,34,3489-
Curtain coating is employed in 3498 (2014) " and patent No. ZL201310739082.7 first and combines chemical vapor infiltration (CVI)
Diamond/SiC composites have been made.The diamond slurry that this method requirement configures different-grain diameter (7~27 μm) first is entered
Row curtain coating experiment, is placed in CVI cvd furnaces after then the substrate being cast is dried and deposits SiC matrix, obtain Diamond/SiC
Thin slice, thin slice is taken out and is cast and deposits repeatedly on its surface.Finally, the diamond/silicon carbide for having obtained thickness about 2mm is combined
Material sample.
Because chemical vapor infiltration reaction condition is gentleer, and deposit SiC be it is generated in-situ, avoiding problems
Diamond graphitization and the problem of residual silicon in composite.Preparation-obtained Diamond/SiC/ composites are Buddha's warrior attendant
Stone and carborundum two-phase, without other impurities, diamond is evenly distributed and is well combined with matrix diamond in the composite.This
Outside, industrialized production can be achieved as a kind of technique for the comparative maturity for preparing ceramic matric composite in CVI.
But in curtain coating combines CVI methods, due to the limitation of the tape casting in itself, the particle diameter of the diadust used
Can not be too big, which limits the raising of the intrinsic thermal conductivity of diamond, so as to limit Diamond/SiC heat conductivities
Raising so that the thermal conductivity highest of the composite of preparation only has about 110W/ (mk)
The content of the invention
The technical problem to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of big particle diameter Diamond/SiC composites
Preparation method, solve curtain coating prepares diamond particle diameter in Diamond/SiC composites with reference to CVI can not too big technology hardly possible
Topic.
Technical scheme
A kind of preparation method of big particle diameter Diamond/SiC composites, it is characterised in that step is as follows：
Step 1：By the anti-settling increasing of the diamond powder of 56%~66% mass fraction, 0.35%~1.38% mass fraction
Thick dose, the solvent mixing ball of the polyvinyl butyral resin of 3.5%~4.2% mass fraction and 30.3%~38.3% mass fraction
Slurry is obtained after mill；The solvent is the absolute ethyl alcohol of 1: 1 mass ratio and the mixed solvent of butanone；The quality of each component is total
With for absolutely；
Step 2：The slurry mixed is poured into mould, after it is spontaneously dried under air ambient, is made after the demoulding
The diamond precast body that thickness is about 2-3mm；The inner surface brushing releasing agent of the mould；
Step 3：Diamond precast body is used after graphite fixture, chemical vapor infiltration poke CVI stoves is put into and carries out chemical gas
Mutually infiltration prepares Diamond/SiC composites；After SiC shells occur in Diamond/SiC composite material surfaces, by it
The SiC shells on surface proceed deposition after polishing off, until the density of Diamond/SiC composites reaches about 3.1g/
cm3。
The ball milling of the step 1 is：Ball milling cylinder speed is 50-300r/min, and the time is 5-15h.
The step 3 CVI methods generation SiC matrix technique be：Using trichloromethyl silane MTS as precursor, hydrogen
As carrier gas, argon gas is as diluent gas, and its flow rate ratio is 1:5~50:2~20, total gas pressure is 0.5~5kPa, depositing temperature
For 873~1773K.
The particle diameter of the diamond powder is 50~500um.
Beneficial effect
The preparation method of a kind of big particle diameter Diamond/SiC composites proposed by the present invention, using the big grain of one-shot forming
The method that footpath diamond precast body is combined with CVI techniques, is made Diamond/SiC composites.It is multiple using the method increase
The particle diameter and volume content of diamond in condensation material, so as to effectively raise the thermal conductivity of composite.So that thermal conductivity compared with
Curtain coating combination CVI methods prepare composite improve about 30%.Moreover, this method simple production process, controllable, can
For industrialized production.
Brief description of the drawings
Fig. 1：The schematic flow sheet of the inventive method
Fig. 2：The fracture apperance figure of Diamond/SiC composites prepared by the inventive method
Fig. 3：The present invention uses the thermal conductivity figure of the composite of different diamond particle diameters
Embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment one
Step 1. by mass percentage, by 62.3% 50um bortz powder, 4.2% polyvinyl butyral resin,
0.3% anti-settling thickener, (ethanol and butanone are according to mass ratio 1 for 33.2% solvent:1 addition) mixing after carry out ball milling, ball
Consume time as 10h, ball milling cylinder speed is 120r/min.
Floor space is uniformly brushed one layer of silicone oil by step 2. in advance for the inner surface of 55 × 55 mould, then by foregoing ball
The slurry of milled takes out, and uniformly pours among mould.Make after it is completely dried in atmosphere, to carry out the de- of diamond precast body
Mould, can obtain the diamond precast body that thickness is about 2mm.
Diamond preform deposition SiC matrix is obtained Diamond/SiC composites by step 3.：By obtained diamond
Precast body carries out chemical vapor infiltration deposition SiC matrix, and carrier gas, argon are used as by the use of MTS (CH3SiCl3) as precursor, hydrogen
Gas is as diluent gas, and its flow rate ratio is 1:40:40, the wherein flow rate of argon gas is 350mL/min, and total gas pressure is 5000Pa, is sunk
Accumulated temperature degree is 1273K.
Step 4. can influence reacting gas to enter in material after SiC shells occur in Diamond/SiC composite material surfaces
Portion influences the densification of material, now needs to proceed deposition after the SiC shells of composite material surface are polished off.Finally
It is about the thick Diamond/SiC composites of 2mm to thickness, density is 3.03g/cm3, open pore rate is 8.8%.
Embodiment two
Step 1. by mass percentage, by 57.4% 104um bortz powder, 3.8% polyvinyl butyral resin,
0.5% anti-settling thickener, (ethanol and butanone are according to mass ratio 1 for 38.3% solvent:1 addition) mixing after carry out ball milling, ball
Consume time as 10h, ball milling cylinder speed is 120r/min.
Floor space is uniformly brushed one layer of silicone oil by step 2. in advance for the inner surface of 55 × 55 mould, then by foregoing ball
The slurry of milled takes out, and uniformly pours among mould.Make after it is completely dried in atmosphere, to carry out the de- of diamond precast body
Mould, can obtain the diamond precast body that thickness is about 2mm.
Diamond preform deposition SiC matrix is obtained Diamond/SiC composites by step 3.：By obtained diamond
Precast body carries out chemical vapor infiltration deposition SiC matrix, and carrier gas, argon are used as by the use of MTS (CH3SiCl3) as precursor, hydrogen
Gas is as diluent gas, and its flow rate ratio is 1:40:40, the wherein flow rate of argon gas is 350mL/min, and total gas pressure is 5000Pa, is sunk
Accumulated temperature degree is 1273K.
Step 4. can influence reacting gas to enter in material after SiC shells occur in Diamond/SiC composite material surfaces
Portion influences the densification of material, now needs to proceed deposition after the SiC shells of composite material surface are polished off.Finally
It is about the thick Diamond/SiC composites of 2mm to thickness, density is 3.04g/cm3, and open pore rate is 7.6%.
Embodiment three
Step 1. by mass percentage, by 61.5% 250um bortz powder, 4.2% polyvinyl butyral resin,
0.5% anti-settling thickener, (ethanol and butanone are according to mass ratio 1 for 33.8% solvent:1 addition) mixing after carry out ball milling, ball
Consume time as 10h, ball milling cylinder speed is 120r/min.
Floor space is uniformly brushed one layer of silicone oil by step 2. in advance for the inner surface of 55 × 55 mould, then by foregoing ball
The slurry of milled takes out, and uniformly pours among mould.Make after it is completely dried in atmosphere, to carry out the de- of diamond precast body
Mould, can obtain the diamond precast body that thickness is about 2.5mm.
Diamond preform deposition SiC matrix is obtained Diamond/SiC composites by step 3.：By obtained diamond
Precast body carries out chemical vapor infiltration deposition SiC matrix, and carrier gas, argon are used as by the use of MTS (CH3SiCl3) as precursor, hydrogen
Gas is as diluent gas, and its flow rate ratio is 1:40:40, the wherein flow rate of argon gas is 350mL/min, and total gas pressure is 5000Pa, is sunk
Accumulated temperature degree is 1273K.
Step 4. can influence reacting gas to enter in material after SiC shells occur in Diamond/SiC composite material surfaces
Portion influences the densification of material, now needs to proceed deposition after the SiC shells of composite material surface are polished off.Finally
It is about the thick Diamond/SiC composites of 2.5mm to thickness, density is 3.17g/cm3, open pore rate is 3.1%.
Example IV
Step 1. by mass percentage, by 64.9% 350um bortz powder, 3.93% polyvinyl butyral resin,
0.87% anti-settling thickener, (ethanol and butanone are according to mass ratio 1 for 30.3% solvent:1 addition) mixing after carry out ball milling, ball
Consume time as 10h, ball milling cylinder speed is 120r/min.
Floor space is uniformly brushed one layer of silicone oil by step 2. in advance for the inner surface of 55 × 55 mould, then by foregoing ball
The slurry of milled takes out, and uniformly pours among mould.Make after it is completely dried in atmosphere, to carry out the de- of diamond precast body
Mould, can obtain the diamond precast body that thickness is about 2.5mm.
Diamond preform deposition SiC matrix is obtained Diamond/SiC composites by step 3.：By obtained diamond
Precast body carries out chemical vapor infiltration deposition SiC matrix, and carrier gas, argon are used as by the use of MTS (CH3SiCl3) as precursor, hydrogen
Gas is as diluent gas, and its flow rate ratio is 1:40:40, the wherein flow rate of argon gas is 350mL/min, and total gas pressure is 5000Pa, is sunk
Accumulated temperature degree is 1273K.
Step 4. can influence reacting gas to enter in material after SiC shells occur in Diamond/SiC composite material surfaces
Portion influences the densification of material, now needs to proceed deposition after the SiC shells of composite material surface are polished off.Finally
It is about the thick Diamond/SiC composites of 2.5mm to thickness, density is 3.14g/cm3, open pore rate is 5.6%.
Embodiment five
Step 1. by mass percentage, by 60.6% 500um bortz powder, 3.5% polyvinyl butyral resin,
1.3% anti-settling thickener, (ethanol and butanone are according to mass ratio 1 for 34.6% solvent：1 addition) mixing after carry out ball milling, ball
Consume time as 10h, ball milling cylinder speed is 120r/min.
Floor space is uniformly brushed one layer of silicone oil by step 2. in advance for the inner surface of 55 × 55 mould, then by foregoing ball
The slurry of milled takes out, and uniformly pours among mould.Make after it is completely dried in atmosphere, to carry out the de- of diamond precast body
Mould, can obtain the diamond precast body that thickness is about 2.5mm.
Diamond preform deposition SiC matrix is obtained Diamond/SiC composites by step 3.：By obtained diamond
Precast body carries out chemical vapor infiltration deposition SiC matrix, and carrier gas, argon are used as by the use of MTS (CH3SiCl3) as precursor, hydrogen
Gas is as diluent gas, and its flow rate ratio is 1:40:40, the wherein flow rate of argon gas is 350mL/min, and total gas pressure is 5000Pa, is sunk
Accumulated temperature degree is 1273K.
Step 4. can influence reacting gas to enter in material after SiC shells occur in Diamond/SiC composite material surfaces
Portion influences the densification of material, now needs to proceed deposition after the SiC shells of composite material surface are polished off.Finally
It is about the thick Diamond/SiC composites of 2.5mm to thickness, density is 3.18g/cm3, open pore rate is 3.9%.
Claims (3)
1. a kind of preparation method of big particle diameter Diamond/SiC composites, it is characterised in that step is as follows：
Step 1：By the anti-settling thickening of the diamond powder of 56%~66% mass fraction, 0.35%~1.38% mass fraction
The solvent mixing and ball milling of agent, the polyvinyl butyral resin of 3.5%~4.2% mass fraction and 30.3%~38.3% mass fraction
After obtain slurry；The solvent is the absolute ethyl alcohol of 1: 1 mass ratio and the mixed solvent of butanone；The quality summation of each component is hundred
/ hundred；The particle diameter of the diamond powder is 50~500 μm；
Step 2：The slurry mixed is poured into mould, after it is spontaneously dried under air ambient, thickness is made after the demoulding
For 2-3mm diamond precast body；The inner surface brushing releasing agent of the mould；
Step 3：Diamond precast body is used after graphite fixture, chemical vapor infiltration poke CVI stoves is put into and carries out chemical vapor infiltration
Prepare Diamond/SiC composites thoroughly；After SiC shells occur in Diamond/SiC composite material surfaces, by its surface
SiC shells polish off after proceed deposition, until the density of Diamond/SiC composites reaches 3.1g/cm3。
2. the preparation method of big particle diameter Diamond/SiC composites according to claim 1, it is characterised in that：The step
Rapid 1 ball milling is：Ball milling cylinder speed is 50-300r/min, and the time is 5-15h.
3. the preparation method of big particle diameter Diamond/SiC composites according to claim 1, it is characterised in that：The step
Rapid 3 CVI methods generation SiC matrix technique be：Using trichloromethyl silane MTS as precursor, hydrogen is made as carrier gas, argon gas
For diluent gas, its flow rate ratio is 1:5~50:2~20, total gas pressure is 0.5~5kPa, and depositing temperature is 873~1773K.
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| CN105777172A (en) * | 2016-03-30 | 2016-07-20 | 西北工业大学 | Method for preparing Diamond/SiC composite material by combining thermally compression molding with chemical vapor infiltration (CVI) |
| CN109704798A (en) * | 2019-01-09 | 2019-05-03 | 西北工业大学 | The method that vacuum impregnation association reaction melt infiltration RMI prepares C/SiC-Diamond composite material |
| CN111484330A (en) * | 2020-04-13 | 2020-08-04 | 北京科技大学广州新材料研究院 | Diamond-enhanced silicon carbide substrate, preparation method thereof and electronic product |
| CN114315354B (en) * | 2021-12-29 | 2023-02-07 | 武汉理工大学 | Diamond-B 4 Two-step sintering method of C-SiC three-phase composite ceramic |
| CN116969764A (en) * | 2023-07-05 | 2023-10-31 | 西安鑫垚陶瓷复合材料股份有限公司 | Method for preparing Diamond/SiC composite material by combining hot die pressing with CVI |
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| CN103724014B (en) * | 2013-12-26 | 2015-03-04 | 西北工业大学 | Preparation method of diamond doped silicon carbide (SiC) ceramics with high heat conductivity |
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