CN106830984A - A kind of method for preparing high-volume fractional silicon-carbide ceramics enhancing silicon composite - Google Patents
A kind of method for preparing high-volume fractional silicon-carbide ceramics enhancing silicon composite Download PDFInfo
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- CN106830984A CN106830984A CN201710224818.5A CN201710224818A CN106830984A CN 106830984 A CN106830984 A CN 106830984A CN 201710224818 A CN201710224818 A CN 201710224818A CN 106830984 A CN106830984 A CN 106830984A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 70
- 239000000919 ceramic Substances 0.000 title claims abstract description 66
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 39
- 239000010703 silicon Substances 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000008595 infiltration Effects 0.000 claims abstract description 26
- 238000001764 infiltration Methods 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000005453 pelletization Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000000084 colloidal system Substances 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 238000009826 distribution Methods 0.000 claims abstract description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 1
- 230000003179 granulation Effects 0.000 abstract description 4
- 238000005469 granulation Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000007493 shaping process Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000009715 pressure infiltration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- ZBZHVBPVQIHFJN-UHFFFAOYSA-N trimethylalumane Chemical compound C[Al](C)C.C[Al](C)C ZBZHVBPVQIHFJN-UHFFFAOYSA-N 0.000 description 1
- 238000004018 waxing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a kind of method for preparing high-volume fractional silicon-carbide ceramics enhancing silicon composite, according to the silicon carbide ceramics particle of research of grade-suit theory selection different-grain diameter distribution, compound is made by proportioning, water, cetyl trimethylammonium bromide, sodium cellulose glycolate and urea are mixed, heat while stirring, then will mix and be granulated with compound after colloid natural cooling, and pelletizing is put into be sieved in baking oven take, pressed compact will be carried out using powder hydraulic press；The base substrate that will be pressed is sintered in being fitted into Muffle furnace, obtains silicon carbide ceramics；It is fitted into infiltration furnace and is infiltrated.The present invention passes sequentially through batch mixing, granulation, shaping, sintering and is made the carborundum porous ceramics of high-volume fractional, again silicon carbide ceramics enhancing silicon composite is ultimately formed by infiltrating silicon, wherein the volume fraction of carborundum porous ceramics is 80%~95%, its thermal coefficient of expansion will be reduced much compared to simple silicon ceramics, and intensity will be improved much compared to simple silicon.
Description
Technical field
The invention belongs to technical field of composite preparation, and in particular to one kind prepares high-volume fractional by grain composition
Aluminium carbide ceramics prepare the preparation method of high-volume fractional silicon-carbide ceramics enhancing silicon composite by infiltrating silicon again.
Background technology
Silicon ceramics respectively have its feature with silicon carbide ceramics, and the former has, and thermal coefficient of expansion is low, density is low, easy processing etc. is excellent
Gesture, the latter has the features such as thermal conductivity is high, intensity is high, elastic modelling quantity is high, wearability is good, therefore both performance characteristics are combined
Get up, the SiC reinforcement silicon based composite material of excellent combination property can be prepared.
Prior art mixes by by carborundum powder and silica flour, adds additive to be molded under low pressure, through drying, de-waxing and
Sintering is made the ceramics preparative type that silicon mixes with carborundum, and the ceramics preparative type that the method is made is cellular, in addition carborundum
The totality of silicon point can only achieve 40~80%.
The content of the invention
The technical problems to be solved by the invention are for above-mentioned deficiency of the prior art, there is provided a kind of volume high
Fraction silicon carbide ceramics strengthens the preparation method of silicon composite, and the method is prepared for the carbon of high-volume fractional by grain composition
SiClx ceramics, its volume fraction may be up to 90%, then silicon carbide ceramics enhancing silicon composite is obtained by Pressure Infiltration silicon.
The present invention uses following technical scheme：
A kind of method for preparing high-volume fractional silicon-carbide ceramics enhancing silicon composite, comprises the following steps：
S1, the silicon carbide ceramics particle according to research of grade-suit theory selection different-grain diameter distribution, pouring into batch mixer by proportioning is carried out
Mixing, 1~40h of mixing time obtains compound；
S2, Jiang Shui, cetyl trimethylammonium bromide, sodium cellulose glycolate and urea are mixed and heated stirring, treat
Fully dissolving after continue stir 1~10h be made colloid, naturally cool to less than 40 DEG C it is standby；
The colloid that S3, the compound that step S1 is obtained and step S2 are obtained is 1 according to mass ratio：1 ratio mixing, enters
, then be put into pelletizing in baking oven by row granulation, 40~60 DEG C of 1~6h of baking, and when humidity reaches 3~20%, sieve takes 100
The pelletizing of~200 mesh；
S4, the pelletizing for loading step S3 preparations, pressed compact is carried out using powder hydraulic press；
S5, the base substrate that will be pressed are sintered in being fitted into Muffle furnace, obtain silicon carbide ceramics；
S6, by step S5 prepare silicon carbide ceramics is fitted into infiltration furnace, be incubated 30~60min, it is to be dissolved after, infiltrate 40
~100min, closes intake valve opening gas bleeder valve and starts to lose heart, and stalk heater switch is then shut off, when pressure tank in operation cabinet
It is 0, loses heart when lower pressure tank is 0 and terminate, in-furnace temperature to be infiltrated is down to 50 DEG C, closes infiltration furnace power switch, opens infiltration
Stove top case, infiltration terminates.
Preferably, in step S1, the silicon carbide ceramics particle include 2~3 μm of particle diameter distribution, 5~8 μm, 15~20um,
20~25um, carborundum.
Preferably, described 2~3 μm, 5~8 μm, the carborundum of 15-20um, 20-25um is according to 5:2:1:1 mass ratio falls
Enter batch mixer to be stirred.
Preferably, the volume fraction of the silicon carbide ceramics particle is 80%~95%.
Preferably, in step S2, the water, cetyl trimethylammonium bromide, sodium cellulose glycolate and urea
Mass ratio is 10：2：1：1.
Preferably, in step S4, it is 5~10MPa, 15~30min of dwell time to set liquid maximum pressure.
Preferably, in step S5, the curve of sintering is as follows：
With the heating rate of 3 DEG C/min by base substrate from room temperature to 800 DEG C, 150min is incubated, with the intensification of 1 DEG C/min
Temperature is continuously heating to 1600 DEG C by speed, is incubated 300min, and temperature is risen into 2200 DEG C with the heating rate of 1 DEG C/min, is protected
Warm 120min, then cools to less than 40 DEG C with the furnace and takes out burned silicon carbide ceramics.
Preferably, in step S6, infiltration furnace pressure be 1.5MPa, vacuum be 0~0.80MPa, the dwell time be 30~
120min。
Compared with prior art, the present invention at least has the advantages that：
The present invention prepares silicon carbide ceramics enhancing silicon composite using infiltration silicon, and burning is mixed with silica flour compared to carborundum powder
Knot carborundum silicon ceramics, the volume fraction of ceramics is greatly improved, and can reach 90%, and the volume fraction of simple carborundum can in addition
To reach 90%~95%, and this kind of silicon carbide ceramics strengthens the performance synthesis of silicon composite simple silicon carbide ceramics and silicon
Ceramic performance advantage, can prepare the SiC reinforcement silicon based composite material of excellent combination property.
The present invention can strengthen silicon carbide ceramics the property of silicon composite by adjusting the volume fraction of silicon carbide ceramics
Energy (density, thermal conductivity, thermal coefficient of expansion, intensity, elastic modelling quantity, processability etc.) is designed, to meet different field to this
Plant demand and the application of material.
In sum, the present invention passes sequentially through batch mixing, granulation, shaping, sinters and be made the silicon carbide porous of high-volume fractional
Ceramics, then ultimately form silicon carbide ceramics enhancing silicon composite, the wherein volume integral of carborundum porous ceramics by infiltrating silicon
80%~95%, its thermal coefficient of expansion will be reduced much number compared to simple silicon ceramics, and intensity will be improved much compared to simple silicon.
Below by embodiment, technical scheme is described in further detail.
Specific embodiment
The invention provides a kind of method for preparing high-volume fractional silicon-carbide ceramics enhancing silicon composite, its feature exists
In：Comprise the following steps：
S1, the silicon carbide ceramics particle according to research of grade-suit theory selection different-grain diameter distribution, pouring into batch mixer by proportioning is carried out
Mixing, 2~20h of mixing time obtains compound；
Wherein, the silicon carbide ceramics particle include 2~3 μm of particle diameter distribution, 5~8 μm, 15~20um, 20~25um
Carborundum.According to 5:2:1:1 mass ratio pours into batch mixer and is stirred.
S2, Jiang Shui, cetyl trimethylammonium bromide, sodium cellulose glycolate and urea mixing, mass ratio are respectively
10：2：1：1 heat while stirring all should, fully dissolving after continue stir 1~10h, then by colloid naturally cool to 40 DEG C with
Under standby
The colloid that S3, the compound that step S1 is obtained and step S2 are obtained is 1 according to mass ratio：1 ratio mixing, enters
, then be put into pelletizing in baking oven by row granulation, 40~60 DEG C of 1~6h of baking, and when humidity reaches 3%~20%, sieve takes
The pelletizing of 100~200 mesh；
S4, the pelletizing for loading step S3 preparations, pressed compact is carried out using powder hydraulic press；
Wherein, it is 5~10MPa, 15~30min of dwell time to set liquid maximum pressure.
S5, the base substrate that will be pressed are sintered in being fitted into Muffle furnace, obtain silicon carbide ceramics；
Wherein, the curve of sintering is as follows：
With the heating rate of 3 DEG C/min by base substrate from room temperature to 800 DEG C, 150min is incubated, with the intensification of 1 DEG C/min
Temperature is continuously heating to 1600 DEG C by speed, is incubated 300min, and temperature is risen into 2200 DEG C with the heating rate of 1 DEG C/min, is protected
Warm 120min, then cools to less than 40 DEG C with the furnace and takes out burned silicon carbide ceramics.
S6, by step S5 prepare silicon carbide ceramics is fitted into infiltration furnace, be incubated 30~60min, it is to be dissolved after, infiltrate 40
~100min, closes intake valve opening gas bleeder valve and starts to lose heart, and stalk heater switch is then shut off, when pressure tank in operation cabinet
It is 0, loses heart when lower pressure tank is 0 and terminate, in-furnace temperature to be infiltrated is down to 50 DEG C, closes infiltration furnace power switch, opens infiltration
Stove top case, infiltration terminates.
Wherein, infiltration furnace pressure is 1.5MPa, and vacuum is 0~0.80MPa, and the dwell time is 30~120min.
Embodiment 1
(1) be 2~3 μm by particle diameter distribution, 5~8 μm, 15~20um, the carborundum of 20~25um.According to 5:2:1:1
Mass ratio pours into batch mixer after weighing 10kg, stirs 10h, obtains well mixed silicon carbide ceramics powder；
(2) water, cetyl trimethylammonium bromide, sodium cellulose glycolate and urea are mixed, mass ratio is respectively
10：2：1：1 heat while stirring all should, fully dissolving after continue stir 1~10h, then by colloid naturally cool to 40 DEG C with
Under it is standby；
(3) organic gel obtained by the silicon carbide ceramics powder and 10kg steps (2) obtained by 10kg steps (1) is weighed to mix simultaneously
Granulated, then pelletizing is put into baking oven, when humidity reaches 7%, finishing screen is taken 100 mesh between 200 mesh
Pelletizing.
(4) pressed compact is carried out using powder hydraulic press.It is 5~10MPa to set liquid maximum pressure, the dwell time 15~
30min, loads 500g pelletizings, and starting motor carries out pressed compact, obtains silicon carbide ceramic body.
(5) base substrate that will be pressed is fitted into Muffle furnace, is sintered according to following sintering curre：
Sintering curre is：
With the heating rate of 3 DEG C/min by base substrate from room temperature to 800 DEG C, 150min is incubated, with the intensification of 1 DEG C/min
Temperature is continuously heating to 1600 DEG C by speed, is incubated 300min, and temperature is risen into 2200 DEG C with the heating rate of 1 DEG C/min, is protected
Warm 120min, then cools to less than 40 DEG C with the furnace and takes out burned silicon carbide ceramics.
(6) infiltrate
Silicon carbide ceramics is fitted into infiltration furnace, it is 1.5MPa to set infiltration furnace pressure, and vacuum is -0.80MPa, pressurize
Time is 30~60min.Heating polysilicon is incubated 30min to 1450~1500 DEG C, treats that it all dissolves, and then opens air inlet
Valve, infiltration furnace power switch and stalk heater switch start infiltration.Infiltration 40min, closes intake valve opening gas bleeder valve and starts
Lose heart, close stalk heater switch immediately afterwards, when pressure tank is 0 in operation cabinet, loses heart when lower pressure tank is 0 and terminate, treat
Infiltration in-furnace temperature is down to 50 DEG C, closes infiltration furnace power switch, opens infiltration stove top case, and infiltration terminates.
The density for using density instrument to measure the silicon carbide ceramics enhancing silicon composite that embodiment 1 is obtained is 2.60g/
cm3；
The silicon carbide ceramics obtained using RDJ-201 laser conductometers measurement embodiment 1 strengthens the thermal conductivity of silicon composite
Rate is 120W/ (M-K) (sample size is Φ 12.3 × 7)；
The silicon carbide ceramics obtained using NETZSCH DIL402C mechanical levers instrument measurement embodiment 1 strengthens aluminium composite wood
Expect that the thermal coefficient of expansion at 25 DEG C is 3.2759E-06/K (sample size is 3mm × 4mm × 25mm).
The silicon carbide ceramics of embodiment 1 enhancing aluminium composite wood is measured to obtain using WDW-100 multisensor electronic universal testers
The bending strength of material is 210MPa (sample sizes：3mm×4mm×50mm).
Above content is only explanation technological thought of the invention, it is impossible to limit protection scope of the present invention with this, every to press
According to technological thought proposed by the present invention, any change done on the basis of technical scheme each falls within claims of the present invention
Protection domain within.
Claims (8)
1. it is a kind of to prepare the method that high-volume fractional silicon-carbide ceramics strengthen silicon composite, it is characterised in that including following step
Suddenly：
S1, the silicon carbide ceramics particle according to research of grade-suit theory selection different-grain diameter distribution, pour into batch mixer and are mixed by proportioning,
1~40h of mixing time, obtains compound；
S2, Jiang Shui, cetyl trimethylammonium bromide, sodium cellulose glycolate and urea are mixed and heated stirring, treat fully
After dissolving continue stir 1~10h be made colloid, naturally cool to less than 40 DEG C it is standby；
The colloid that S3, the compound that step S1 is obtained and step S2 are obtained is 1 according to mass ratio：1 ratio mixing, is made
, then be put into pelletizing in baking oven by grain, 40~60 DEG C of 1~6h of baking, and when humidity reaches 3~20%, sieve takes 100~
The pelletizing of 200 mesh；
S4, the pelletizing for loading step S3 preparations, pressed compact is carried out using powder hydraulic press；
S5, the base substrate that will be pressed are sintered in being fitted into Muffle furnace, obtain silicon carbide ceramics；
S6, by step S5 prepare silicon carbide ceramics is fitted into infiltration furnace, be incubated 30~60min, it is to be dissolved after, infiltrate 40~
100min, closes intake valve opening gas bleeder valve and starts to lose heart, and stalk heater switch is then shut off, when pressure tank is in operation cabinet
0, lose heart when lower pressure tank is 0 and terminate, in-furnace temperature to be infiltrated is down to 50 DEG C, closes infiltration furnace power switch, opens infiltration furnace
Upper lid, infiltration terminates.
2. it is according to claim 1 it is a kind of prepare high-volume fractional silicon-carbide ceramics enhancing silicon composite method, its
It is characterised by：In step S1, the silicon carbide ceramics particle includes 2~3 μm of particle diameter distribution, 5~8 μm, 15-20um, 20-
25um, carborundum.
3. it is according to claim 2 it is a kind of prepare high-volume fractional silicon-carbide ceramics enhancing silicon composite method, its
Be characterised by, described 2~3 μm, 5~8 μm, 15~20um, the carborundum of 20~25um is according to 5:2:1:1 mass ratio pours into mixed
Material machine is stirred.
4. it is according to claim 3 it is a kind of prepare high-volume fractional silicon-carbide ceramics enhancing silicon composite method, its
It is characterised by：The volume fraction of the silicon carbide ceramics particle is 80%~95%.
5. it is according to claim 1 it is a kind of prepare high-volume fractional silicon-carbide ceramics enhancing silicon composite method, its
It is characterised by：In step S2, the mass ratio of the water, cetyl trimethylammonium bromide, sodium cellulose glycolate and urea
It is 10：2：1：1.
6. it is according to claim 1 it is a kind of prepare high-volume fractional silicon-carbide ceramics enhancing silicon composite method, its
It is characterised by：In step S4, it is 5~10MPa, 15~30min of dwell time to set liquid maximum pressure.
7. it is according to claim 1 it is a kind of prepare high-volume fractional silicon-carbide ceramics enhancing silicon composite method, its
It is characterised by, in step S5, the curve of sintering is as follows：
With the heating rate of 3 DEG C/min by base substrate from room temperature to 800 DEG C, 150min is incubated, with the heating rate of 1 DEG C/min
Temperature is continuously heating to 1600 DEG C, 300min is incubated, temperature is risen to by 2200 DEG C, insulation with the heating rate of 1 DEG C/min
120min, then cools to less than 40 DEG C with the furnace and takes out burned silicon carbide ceramics.
8. it is according to claim 1 it is a kind of prepare high-volume fractional silicon-carbide ceramics enhancing silicon composite method, its
It is characterised by：In step S6, infiltration furnace pressure is 1.5MPa, and vacuum is 0~0.80MPa, and the dwell time is 30~120min.
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| CN113097153A (en) * | 2021-03-31 | 2021-07-09 | 珠海亿特立新材料有限公司 | Preparation method of aluminum silicon carbide heat sink substrate and aluminum silicon carbide heat sink substrate |
| CN116425548A (en) * | 2023-04-10 | 2023-07-14 | 中国科学院上海硅酸盐研究所 | Binder Jet Printing Silicon Carbide Ceramic Composite Material Based on Particle Grading Powder and Its Preparation Method |
| CN117802361A (en) * | 2023-12-29 | 2024-04-02 | 浙江吉成新材股份有限公司 | Ceramic reinforced aluminum-based composite material and preparation method thereof |
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