CN106830984B - Method for preparing high volume fraction silicon carbide ceramic reinforced silicon composite material - Google Patents
Method for preparing high volume fraction silicon carbide ceramic reinforced silicon composite material Download PDFInfo
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- CN106830984B CN106830984B CN201710224818.5A CN201710224818A CN106830984B CN 106830984 B CN106830984 B CN 106830984B CN 201710224818 A CN201710224818 A CN 201710224818A CN 106830984 B CN106830984 B CN 106830984B
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 71
- 239000000919 ceramic Substances 0.000 title claims abstract description 67
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 33
- 239000010703 silicon Substances 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 230000008595 infiltration Effects 0.000 claims abstract description 26
- 238000001764 infiltration Methods 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000000084 colloidal system Substances 0.000 claims abstract description 8
- 238000009826 distribution Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims 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 description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 6
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 abstract description 5
- 238000011068 loading method Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 abstract 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009715 pressure infiltration Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a high volume fraction silicon carbide ceramic reinforced silicon composite material, which comprises the steps of selecting silicon carbide ceramic particles with different particle size distributions according to a grading theory, preparing a mixture according to a proportion, mixing water, cetyl trimethyl ammonium bromide, sodium hydroxymethyl cellulose and urea while heating and stirring, naturally cooling a colloid, mixing with the mixture, granulating, putting granulated powder into a drying oven for sieving, and pressing by using a powder hydraulic press; putting the pressed blank into a muffle furnace for sintering to obtain silicon carbide ceramic; and (4) loading the mixture into an infiltration furnace for infiltration. The invention prepares the silicon carbide porous ceramic with high volume fraction through mixing, granulating, molding and sintering, and finally forms the silicon carbide ceramic reinforced silicon composite material through silicon impregnation, wherein the volume fraction of the silicon carbide porous ceramic is 80-95%, the thermal expansion coefficient of the silicon carbide porous ceramic is greatly reduced compared with that of the single pure silicon ceramic, and the strength of the silicon carbide porous ceramic is greatly improved compared with that of the single pure silicon.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a preparation method for preparing a high volume fraction aluminum carbide ceramic reinforced silicon composite material by grain composition and then impregnating silicon.
Background
The silicon ceramic and the silicon carbide ceramic have the characteristics that the former has the advantages of low thermal expansion coefficient, low density, easy processing and the like, and the latter has the characteristics of high thermal conductivity, high strength, high elastic modulus, good wear resistance and the like, so that the silicon carbide reinforced silicon-based composite material with excellent comprehensive performance can be prepared by combining the performance characteristics of the silicon ceramic and the silicon carbide ceramic.
In the prior art, silicon carbide powder and silicon powder are mixed, an additive is added to the mixture to be formed under low pressure, and the mixture is dried, de-waxed and sintered to prepare a prefabricated ceramic mould with silicon and silicon carbide mixed, wherein the prefabricated ceramic mould prepared by the method is porous, and the total content of silicon carbide can only reach 40-80%.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a silicon carbide ceramic reinforced silicon composite material with high volume fraction, aiming at the defects in the prior art, the method prepares the silicon carbide ceramic with high volume fraction which can reach 90 percent through grain composition, and then prepares the silicon carbide ceramic reinforced silicon composite material by pressure infiltration of silicon.
The invention adopts the following technical scheme:
a method for preparing a high volume fraction silicon carbide ceramic reinforced silicon composite material comprises the following steps:
s1, selecting silicon carbide ceramic particles with different particle size distributions according to a grading theory, pouring the silicon carbide ceramic particles into a mixer according to the proportion, and mixing for 1-40 h to obtain a mixture;
s2, mixing water, cetyl trimethyl ammonium bromide, sodium carboxymethyl cellulose and urea, heating and stirring, continuing stirring for 1-10 hours after the materials are fully dissolved to prepare colloid, and naturally cooling to below 40 ℃ for later use;
s3, mixing the mixture obtained in the step S1 with the colloid obtained in the step S2 according to the mass ratio of 1:1, granulating, then putting the granulated powder into a drying oven, baking for 1-6 hours at 40-60 ℃, and screening 100-200 meshes of granulated powder when the dry humidity reaches 3-20%;
s4, filling the granulated powder prepared in the step S3, and pressing the granulated powder into a compact by using a powder hydraulic press;
s5, putting the pressed blank into a muffle furnace for sintering to obtain silicon carbide ceramic;
and S6, putting the silicon carbide ceramic prepared in the step S5 into an infiltration furnace, preserving heat for 30-60 min, infiltrating for 40-100 min after the silicon carbide ceramic is dissolved, closing an air inlet valve, opening an air release valve to release air, then closing a heating switch of a liquid lifting pipe, stopping releasing air when the pressure of an upper tank of an operation cabinet is 0 and the pressure of a lower tank is 0, cooling the temperature in the infiltration furnace to 50 ℃, closing a power switch of the infiltration furnace, opening an upper cover of the infiltration furnace, and finishing infiltration.
Preferably, in step S1, the silicon carbide ceramic particles include silicon carbide with a particle size distribution of 2-3 μm, 5-8 μm, 15-20um, 20-25 um.
Preferably, the silicon carbide with the particle size of 2-3 microns, 5-8 microns, 15-20 microns and 20-25 microns is poured into a mixer according to the mass ratio of 5:2:1:1 and stirred.
Preferably, the volume fraction of the silicon carbide ceramic particles is 80-95%.
Preferably, in step S2, the mass ratio of the water, the cetyl trimethyl ammonium bromide, the sodium carboxymethyl cellulose and the urea is 10: 2:1: 1.
preferably, in step S4, the maximum liquid pressure is set to be 5-10 MPa, and the pressure maintaining time is set to be 15-30 min.
Preferably, in step S5, the sintering curve is as follows:
heating the blank body from room temperature to 800 ℃ at the heating rate of 3 ℃/min, preserving heat for 150min, continuously heating the blank body to 1600 ℃ at the heating rate of 1 ℃/min, preserving heat for 300min, heating the blank body to 2200 ℃ at the heating rate of 1 ℃/min, preserving heat for 120min, and then cooling the blank body along with the furnace to below 40 ℃ to take out the fired silicon carbide ceramic.
Preferably, in step S6, the pressure of the infiltration furnace is 1.5MPa, the vacuum degree is 0 to 0.80MPa, and the pressure maintaining time is 30 to 120 min.
Compared with the prior art, the invention has at least the following beneficial effects:
compared with the silicon carbide ceramic sintered by mixing silicon carbide powder and silicon powder, the volume fraction of the ceramic is greatly improved and can reach 90 percent, in addition, the volume fraction of pure silicon carbide can reach 90 to 95 percent, and the performance of the silicon carbide ceramic reinforced silicon composite material integrates the advantages of the pure silicon carbide ceramic and the silicon ceramic, so that the silicon carbide ceramic reinforced silicon-based composite material with excellent comprehensive performance can be prepared.
The invention can design the performance (density, thermal conductivity, thermal expansion coefficient, strength, elastic modulus, processability and the like) of the silicon carbide ceramic reinforced silicon composite material by adjusting the volume fraction of the silicon carbide ceramic so as to meet the requirements and applications of the material in different fields.
In conclusion, the invention prepares the silicon carbide porous ceramic with high volume fraction through mixing, granulating, molding and sintering, and finally forms the silicon carbide ceramic reinforced silicon composite material through silicon impregnation, wherein the volume fraction of the silicon carbide porous ceramic is 80-95%, the thermal expansion coefficient of the silicon carbide porous ceramic is greatly reduced compared with that of the single pure silicon ceramic, and the strength of the silicon carbide porous ceramic is greatly improved compared with that of the single pure silicon.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The invention provides a method for preparing a silicon carbide ceramic reinforced silicon composite material with high volume fraction, which is characterized by comprising the following steps: the method comprises the following steps:
s1, selecting silicon carbide ceramic particles with different particle size distributions according to a grading theory, pouring the silicon carbide ceramic particles into a mixer according to the proportion, and mixing for 2-20 hours to obtain a mixture;
wherein, the silicon carbide ceramic particles comprise silicon carbide with the particle size distribution of 2-3 mu m, 5-8 mu m, 15-20um and 20-25 um. Pouring the mixture into a mixer according to the mass ratio of 5:2:1:1, and stirring.
S2, mixing water, cetyl trimethyl ammonium bromide, sodium carboxymethyl cellulose and urea, wherein the mass ratio is 10: 2:1: heating while stirring, continuously stirring for 1-10 h after fully dissolving, and naturally cooling the colloid to below 40 ℃ for later use.
S3, mixing the mixture obtained in the step S1 with the colloid obtained in the step S2 according to the mass ratio of 1:1, granulating, then putting the granulated powder into a drying oven, baking for 1-6 hours at 40-60 ℃, and screening 100-200 meshes of granulated powder when the dry humidity reaches 3-20%;
s4, filling the granulated powder prepared in the step S3, and pressing the granulated powder into a compact by using a powder hydraulic press;
wherein the maximum pressure of the liquid is set to be 5-10 MPa, and the pressure maintaining time is 15-30 min.
S5, putting the pressed blank into a muffle furnace for sintering to obtain silicon carbide ceramic;
wherein, the sintering curve is as follows:
heating the blank body from room temperature to 800 ℃ at the heating rate of 3 ℃/min, preserving heat for 150min, continuously heating the blank body to 1600 ℃ at the heating rate of 1 ℃/min, preserving heat for 300min, heating the blank body to 2200 ℃ at the heating rate of 1 ℃/min, preserving heat for 120min, and then cooling the blank body along with the furnace to below 40 ℃ to take out the fired silicon carbide ceramic.
And S6, putting the silicon carbide ceramic prepared in the step S5 into an infiltration furnace, preserving heat for 30-60 min, infiltrating for 40-100 min after the silicon carbide ceramic is dissolved, closing an air inlet valve, opening an air release valve to release air, then closing a heating switch of a liquid lifting pipe, stopping releasing air when the pressure of an upper tank of an operation cabinet is 0 and the pressure of a lower tank is 0, cooling the temperature in the infiltration furnace to 50 ℃, closing a power switch of the infiltration furnace, opening an upper cover of the infiltration furnace, and finishing infiltration.
Wherein the pressure of the infiltration furnace is 1.5MPa, the vacuum degree is 0-0.80 MPa, and the pressure maintaining time is 30-120 min.
Example 1
(1) Silicon carbide with particle size distribution of 2-3 μm, 5-8 μm, 15-20um, 20-25um is used. Weighing 10kg of the raw materials according to the mass ratio of 5:2:1:1, pouring the raw materials into a mixer, and stirring for 10 hours to obtain uniformly mixed silicon carbide ceramic powder;
(2) mixing water, cetyl trimethyl ammonium bromide, sodium carboxymethylcellulose and urea according to the mass ratio of 10: 2:1:1, heating while stirring, continuously stirring for 1-10 h after fully dissolving, and naturally cooling the colloid to below 40 ℃ for later use;
(3) and (3) weighing 10kg of the silicon carbide ceramic powder obtained in the step (1) and 10kg of the organic glue obtained in the step (2), mixing and granulating, then putting the granulated powder into a drying oven, and finally screening the granulated powder of 100 meshes to 200 meshes when the drying humidity reaches 7%.
(4) And pressing the blank by using a powder hydraulic press. Setting the maximum pressure of the liquid to be 5-10 MPa, maintaining the pressure for 15-30 min, filling 500g of granulation powder, and starting a motor to perform compaction to obtain the silicon carbide ceramic blank.
(5) And (3) putting the pressed green body into a muffle furnace, and sintering according to the following sintering curve:
the sintering curve is:
heating the blank body from room temperature to 800 ℃ at the heating rate of 3 ℃/min, preserving heat for 150min, continuously heating the blank body to 1600 ℃ at the heating rate of 1 ℃/min, preserving heat for 300min, heating the blank body to 2200 ℃ at the heating rate of 1 ℃/min, preserving heat for 120min, and then cooling the blank body along with the furnace to below 40 ℃ to take out the fired silicon carbide ceramic.
(6) Impregnation with water
And (3) loading the silicon carbide ceramic into an infiltration furnace, setting the pressure of the infiltration furnace to be 1.5MPa, setting the vacuum degree to be-0.80 MPa, and keeping the pressure for 30-60 min. Heating the polysilicon to 1450-1500 ℃, preserving heat for 30min, opening an air inlet valve, an impregnation furnace power switch and a lift tube heating switch to start impregnation after the polysilicon is completely dissolved. And (3) infiltrating for 40min, closing an air inlet valve, opening an air release valve to begin air release, immediately closing a heating switch of a lift pipe, stopping air release when the pressure of an upper tank of an operation cabinet is 0 and the pressure of a lower tank is 0, stopping air release when the temperature in the infiltration furnace is reduced to 50 ℃, closing a power switch of the infiltration furnace, opening an upper cover of the infiltration furnace, and stopping infiltration.
The density of the silicon carbide ceramic-reinforced silicon composite material obtained in example 1 was measured by a density instrument to be 2.60g/cm3；
The thermal conductivity of the silicon carbide ceramic reinforced silicon composite material obtained in example 1 was measured by using an RDJ-201 laser thermal conductivity meter to be 120W/(M-K) (sample size is Φ 12.3 × 7);
the silicon carbide ceramic-reinforced silicon composite material obtained in example 1 was measured to have a thermal expansion coefficient of 3.2759E-06/K (sample size of 3 mm. times.4 mm. times.25 mm) at 25 ℃ by using a NETZSCH DIL402C mechanical lever meter.
The bending strength of the silicon carbide ceramic-reinforced silicon composite material of example 1 was measured to be 210MPa (sample size: 3 mm. times.4 mm. times.50 mm) using a WDW-100 multisensor electronic universal tester.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (4)
1. A method for preparing a high volume fraction silicon carbide ceramic reinforced silicon composite material is characterized by comprising the following steps:
s1, selecting silicon carbide ceramic particles with different particle size distributions according to a grading theory, pouring the silicon carbide ceramic particles into a mixer according to a ratio, mixing for 1-40 hours to obtain a mixture, wherein the silicon carbide ceramic particles comprise silicon carbide with particle size distributions of 2-3 microns, 5-8 microns, 15-20 microns and 20-25 microns, and the silicon carbide with particle sizes of 2-3 microns, 5-8 microns, 15-20 microns and 20-25 microns is poured into the mixer according to a mass ratio of 5:2:1:1 and stirred;
s2, mixing water, cetyl trimethyl ammonium bromide, sodium carboxymethyl cellulose and urea, heating and stirring, continuing stirring for 1-10 hours after the materials are fully dissolved to prepare colloid, and naturally cooling to below 40 ℃ for later use;
s3, mixing the mixture obtained in the step S1 with the colloid obtained in the step S2 according to the mass ratio of 1:1, granulating, then putting the granulated powder into a drying oven, baking for 1-6 hours at 40-60 ℃, and screening 100-200 meshes of granulated powder when the dry humidity reaches 3-20%;
s4, filling the granulated powder prepared in the step S3, and pressing the granulated powder into a compact by using a powder hydraulic press;
s5, putting the pressed blank into a muffle furnace for sintering to obtain silicon carbide ceramic;
s6, the silicon carbide ceramic prepared in the step S5 is filled into an infiltration furnace, the pressure of the infiltration furnace is 1.5MPa, the vacuum degree is 0-0.80 MPa, the pressure maintaining time is 30-120 min, the polycrystalline silicon is heated to 1450-1500 ℃, the temperature is kept for 30-60 min, after the polycrystalline silicon is dissolved, infiltration is performed for 40-100 min, an air inlet valve is closed, an air release valve is opened to release air, then a heating switch of a liquid lifting pipe is closed, when the pressure of an upper tank of an operation cabinet is 0, the air release is finished when the pressure of a lower tank is 0, the temperature in the infiltration furnace is reduced to 50 ℃, a power switch of the infiltration furnace is closed, an upper cover of the infiltration.
2. The method of claim 1, wherein the high volume fraction silicon carbide ceramic reinforced silicon composite material comprises: in step S2, the mass ratio of the water, the cetyl trimethyl ammonium bromide, the sodium carboxymethyl cellulose, and the urea is 10: 2:1: 1.
3. the method of claim 1, wherein the high volume fraction silicon carbide ceramic reinforced silicon composite material comprises: in step S4, the maximum pressure of the liquid is set to be 5-10 MPa, and the pressure maintaining time is set to be 15-30 min.
4. The method of claim 1, wherein in step S5, the sintering curve is as follows:
heating the blank body from room temperature to 800 ℃ at the heating rate of 3 ℃/min, preserving heat for 150min, continuously heating the blank body to 1600 ℃ at the heating rate of 1 ℃/min, preserving heat for 300min, heating the blank body to 2200 ℃ at the heating rate of 1 ℃/min, preserving heat for 120min, and then cooling the blank body along with the furnace to below 40 ℃ to take out the fired silicon carbide ceramic.
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