CN104692778A - Al2O3/SiC composite material containing mullite reinforcing phases and method for preparing Al2O3/SiC composite material containing mullite reinforcing phases - Google Patents

Al2O3/SiC composite material containing mullite reinforcing phases and method for preparing Al2O3/SiC composite material containing mullite reinforcing phases Download PDF

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CN104692778A
CN104692778A CN201510055397.9A CN201510055397A CN104692778A CN 104692778 A CN104692778 A CN 104692778A CN 201510055397 A CN201510055397 A CN 201510055397A CN 104692778 A CN104692778 A CN 104692778A
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sic
composite material
mullite
ceramic matrix
wild phase
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张锐
张帆
范冰冰
邵刚
管可可
宋勃震
梁芃
王海龙
陈德良
卢红霞
许红亮
解亚军
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Zhengzhou University
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Zhengzhou University
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Abstract

The invention discloses an Al2O3/SiC composite material containing mullite reinforcing phases and a method for preparing the Al2O3/SiC composite material containing the mullite reinforcing phases, belonging to the technical field of inorganic nonmetal materials. The Al2O3/SiC composite material is prepared from Al2O3 and SiC particles coated with SiO2, wherein the surface of the SiC particles is coated with SiO2, so that Al2O3 is directed to the surface of the surface of the SiC particles to react with SiO2 to produce mulluite which bridges SiO2 particles and Al2O3, and consequently the toughness of the composite material is improved. According to the method for preparing the Al2O3/SiC composite material containing the mullite reinforcing phases, sintering is carried out in a way of microwave heating, and SiC particles in the composite material absorb microwave heat to achieve the internal self heating of the material, so that the heat is radiated from inside to outside to promote mullite produced by the reaction between Al2O3 and SiO2 to directionally grow from inside to outside so as to bridge the SiO2 particles and Al2O3, and the toughness of the composite material is improved.

Description

A kind of Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material and preparation method thereof
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, be specifically related to a kind of Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material and preparation method thereof.
Background technology
Mullite is Al 2o 3, SiO 2a kind of compound at high temperature formed, still very stable 1800 DEG C time, 1810 DEG C are decomposed into corundum and liquid phase, mullite has features such as expanding evenly, thermal shock resistance is fabulous, load softening point is high, high temperature creep value is little, hardness is large, resistance to chemical corrosion is good, be counted as a kind of high temperature ceramic material of great potential, but its ambient temperature mechanical properties is low to be made it apply to be restricted, usually and other materials compound improve the mechanical property of material.
Aluminum oxide and silicon carbide are also the high temperature ceramic material of being used widely, SiC particles reinforced alumina matrix composite, improve the shortcoming that the sintering temperature of single-phase alumina-ceramic is high, there is excellent mechanical property, there is the advantages such as hardness is high, physical strength is high, wear resistance is good, high-temperature oxidation resistance is strong, chemical stability is good, electrical insulation capability is good, good biocompatibility.Prior art is in SiC particles reinforced alumina-based material preparation process, and SiC is at high temperature oxidized and generates SiO 2, SiO 2with Al 2o 3at high temperature reaction generates mullite, and mullite crystal whisker connects SiC and Al 2o 3particle, plays bridge joint effect, thus toughening ceramic, but adopt the SiO that the method SiC oxidation generates 2amount is few, and the mullite of generation is few mutually, and the composite material toughness of preparation is low.
Summary of the invention
In order to overcome the defect of prior art, an object of the present invention is the Al containing mullite wild phase providing a kind of toughness high 2o 3/ SiC ceramic matrix composite material.
Meanwhile, the present invention is also to provide a kind of Al containing mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, improves the toughness of matrix material.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material, makes primarily of following raw material: SiO 2coated SiC particle, Al 2o 3; Wherein Al 2o 3be 1 ~ 4:1 with the volume ratio of SiC; SiC and SiO 2volume ratio be 1 ~ 10:1.
The particle diameter of described SiC particle is 5 ~ 15 μm.
Described SiO 2coated SiC particle is amorphous Si O 2coated SiC particle.
The above-mentioned Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material, Al 2o 3with SiO 2generate mullite wild phase, this mullite wild phase bridge joint Al 2o 3particle and SiC particle.
The composition of described mullite wild phase is Al 2o 3and SiO 2, Al 2o 3and SiO 2mol ratio be 3:2.
The above-mentioned Al containing mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, comprises following operation steps:
(1) by SiO 2coated SiC particle and Al 2o 3after mixed grinding, compression molding, obtained sheet-like composite;
(2) sheet-like composite microwave heating sintering step (1) prepared, obtains the described Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
In step (1) after grinding, after crossing 120 mesh sieve 6 times, compression molding.
In step (1) after compression molding, under 90 ~ 110MPa pressure after isostatic cool pressing, obtain described sheet-like composite.
Sheet-like composite described in step (1) is diameter is 30mm, and thickness is the slice of cylinder mixture of 2 ~ 4mm.
Microwave heating described in step (2) is sintered to and is heated to 1300 ~ 1600 DEG C, and insulation 30 ~ 120min, air cooling is to room temperature.
The detailed process of the sintering of microwave heating described in step (2) is: first with the ramp to 600 DEG C of 10 ~ 15 DEG C/min, then with ramp to 1300 ~ 1600 DEG C of 15 ~ 20 DEG C/min, and insulation 30 ~ 120min, air cooling is to room temperature.
Described SiO 2the preparation method of coated SiC particle is comprise following operation steps:
A: by α-SiC Granular composite and aqueous ethanolic solution, regulates PH=2 ~ 3, obtains SiC dispersion liquid;
Add tetraethoxy, heated and stirred in b: the step a SiC dispersion liquid prepared, regulate PH=8 ~ 9, stir to obtain plural gel;
C: namely obtain described SiO after the plural gel drying and grinding prepared by step b 2coated SiC particle.
Citric acid is adopted to regulate PH=2 ~ 3 in step a.
In step b, heated and stirred is stir 4h at 30 DEG C of temperature.
Ammoniacal liquor is adopted to regulate PH=8 ~ 9 in step b.
Drying described in step b is 80 DEG C of dry 2h.
Described Al 2o 3preparation method be: by Al (OH) 3namely described Al is obtained at 1100 ~ 1300 DEG C of temperature lower calcination 5 ~ 30min 2o 3.
The present invention is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, with SiO 2coated SiC particle and Al 2o 3for raw material is made, compare traditional only with SiC and Al 2o 3the matrix material that raw material is made, due to SiO 2direct introducing add the mullite of generation, improve the toughness of matrix material; In addition, SiC particle surface parcel SiO 2make Al 2o 3be oriented in SiC particle surface and SiO 2reaction generates mullite, the mullite bridge joint SiO of generation 2particle and Al 2o 3, improve the toughness of matrix material.
The present invention is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, adopts the mode of microwave heating to sinter.Al 2o 3lattice is compact, and fusing point is high, recrystallize ability, is difficult to sintering, adopts the mode of microwave heating sintering, reduces the activation energy of matrix material, thus reduce the sintering temperature of matrix material, shorten sintering time, and Al 2o 3crystal grain has little time to grow up under the effect of microwave, crystal grain thinning; In addition, under the effect of microwave heating, the SiC particulate absorbent microwave heat in matrix material, realizes material internal conducting self-heating, heat is from inside to outside spread, and promotes Al 2o 3with SiO 2the mullite oriented growth from inside to outside that reaction generates, bridge joint SiO 2particle and Al 2o 3, and then improve the toughness of matrix material.
Further, sintering process of the present invention is warming up to required temperature with the temperature rise rate that segmentation is different, and the mode of air cooling cooling after insulation, further shorten sintering time, improve the toughness of matrix material.
Accompanying drawing explanation
Fig. 1 is the Al containing mullite wild phase prepared by embodiment 1 2o 3the XRD figure of/SiC ceramic matrix composite material;
Fig. 2 is the Al containing mullite wild phase prepared by embodiment 1 2o 3the SEM figure of/SiC ceramic matrix composite material;
Fig. 3 is the Al containing mullite wild phase prepared by embodiment 2 2o 3the XRD figure of/SiC ceramic matrix composite material;
Fig. 4 is the Al containing mullite wild phase prepared by embodiment 2 2o 3the SEM figure of/SiC ceramic matrix composite material;
Fig. 5 is the Al containing mullite wild phase prepared by embodiment 3 2o 3the XRD figure of/SiC ceramic matrix composite material;
Fig. 6 is the Al containing mullite wild phase prepared by embodiment 3 2o 3the SEM figure of/SiC ceramic matrix composite material;
Fig. 7 is the Al containing mullite wild phase prepared by embodiment 4 2o 3the XRD figure of/SiC ceramic matrix composite material;
Fig. 8 is the Al containing mullite wild phase prepared by embodiment 4 2o 3the SEM figure of/SiC ceramic matrix composite material;
Fig. 9 is the Al containing mullite wild phase prepared by embodiment 5 2o 3the XRD figure of/SiC ceramic matrix composite material;
Figure 10 is the Al containing mullite wild phase prepared by embodiment 5 2o 3the SEM figure of/SiC ceramic matrix composite material;
Figure 11 is the Al containing mullite wild phase prepared by comparative example 1 2o 3the XRD figure of/SiC ceramic matrix composite material;
Figure 12 is the Al containing mullite wild phase prepared by comparative example 1 2o 3the SEM figure of/SiC ceramic matrix composite material;
Figure 13 is the Al containing mullite wild phase prepared by comparative example 2 2o 3the XRD figure of/SiC ceramic matrix composite material;
Figure 14 is the Al containing mullite wild phase prepared by comparative example 2 2o 3the SEM figure of/SiC ceramic matrix composite material;
Figure 15 is the Al containing mullite wild phase prepared by comparative example 3 2o 3the XRD figure of/SiC ceramic matrix composite material;
Figure 16 is the Al containing mullite wild phase prepared by comparative example 3 2o 3the SEM figure of/SiC ceramic matrix composite material.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1
The present embodiment is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, by SiO 2coated SiC particle, Al 2o 3for raw material is made, wherein Al 2o 3be 1:1 with the volume ratio of SiC; SiO 2the particle diameter being 5:1, SiC particle with the volume ratio of SiC is 10 μm.
The present embodiment is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, concrete operation step is:
(1) raw materials:
A: preparation SiO 2coated SiC particle:
1) getting α-SiC particle 32.1g is scattered in aqueous ethanolic solution, adds citric acid and regulates PH=2, obtain SiC dispersion liquid;
2) getting tetraethoxy 16.7ml adds in SiC dispersion liquid prepared by step (1), and 30 DEG C are stirred 4h, then drips ammoniacal liquor and regulate PH=8, stirs to obtain plural gel;
3) plural gel prepared by step (2) is ground after forced air drying 2h under 80 DEG C of conditions, obtain SiO 2coated SiC particle;
B: preparation Al 2o 3:
1) Al (OH) is got 330min is calcined, obtained Al at 1100 DEG C 2o 3;
(2) matrix material is prepared:
1) according to Al 2o 3be the SiO that 1:1 takes step (1) and prepares with the volume ratio of SiC 2coated SiC particle and Al 2o 3, by SiO 2coated SiC particle and Al 2o 3mix, grinding, cross 120 sieve 6 times, 10MPa tableting under pressure is shaping, obtained sheet-like composite after 100MPa isostatic cool pressing;
2) by step 1) sheet-like composite prepared is placed in boosting attemperator, attemperator being inserted frequency is heat in the multimode cavity microwave oven of 2.45GHz, open microwave source, regulate microwave input power, be warming up to 600 DEG C with 10 DEG C/min speed, regulate microwave input power again, with the ramp to 1500 DEG C of 15 DEG C/min, detection of reflected power simultaneously, insulation 30min, control is chilled to room temperature, obtains the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
Fig. 1 is the XRD figure of the present embodiment matrix material, occurs mullite phase as seen from the figure in the present embodiment matrix material, and the volume content of mullite phase accounts for 30 ~ 35% of cumulative volume;
Fig. 2 is the SEM figure of the present embodiment matrix material, occurs a large amount of mullite crystal whisker as seen from the figure in the present embodiment matrix material.
Embodiment 2
The present embodiment is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, by SiO 2coated SiC particle, Al 2o 3for raw material is made, wherein Al 2o 3be 1:1 with the volume ratio of SiC; SiO 2the particle diameter being 10:1, SiC particle with the volume ratio of SiC is 10 μm.
The present embodiment is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, concrete operation step is:
(1) raw materials:
A: preparation SiO 2coated SiC particle:
1) getting α-SiC particle 31.2g is scattered in aqueous ethanolic solution, adds citric acid and regulates PH=3, obtain SiC dispersion liquid;
2) getting tetraethoxy 8.4ml adds in SiC dispersion liquid prepared by step (1), and 30 DEG C are stirred 4h, then drips ammoniacal liquor and regulate PH=9, stirs to obtain plural gel;
3) plural gel prepared by step (2) is ground after forced air drying 2h under 80 DEG C of conditions, obtain SiO 2coated SiC particle;
B: preparation Al 2o 3:
1) Al (OH) is got 35min is calcined, obtained Al at 1300 DEG C 2o 3;
(2) matrix material is prepared:
1) according to Al 2o 3be the SiO that 1:1 takes step (1) and prepares with the volume ratio of SiC 2coated SiC particle and Al 2o 3, by SiO 2coated SiC particle and Al 2o 3mix, grinding, cross 120 sieve 6 times, 10MPa tableting under pressure is shaping, obtained sheet-like composite after 110MPa isostatic cool pressing;
2) by step 1) sheet-like composite prepared is placed in boosting attemperator, attemperator being inserted frequency is heat in the multimode cavity microwave oven of 2.45GHz, open microwave source, regulate microwave input power, be warming up to 600 DEG C with 15 DEG C/min speed, regulate microwave input power again, with the ramp to 1450 DEG C of 18 DEG C/min, detection of reflected power simultaneously, insulation 90min, control is chilled to room temperature, obtains the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
Fig. 3 is the XRD figure of the present embodiment matrix material, occurs mullite phase as seen from the figure in the present embodiment matrix material, and the volume content of mullite phase accounts for 20 ~ 25% of cumulative volume;
Fig. 4 is the SEM figure of the present embodiment matrix material, mullite crystal whisker bridge joint SiC and Al in the present embodiment matrix material as seen from the figure 2o 3particle.
Embodiment 3
The present embodiment is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, by SiO 2coated SiC particle, Al 2o 3for raw material is made, wherein Al 2o 3be 7:3 with the volume ratio of SiC; SiO 2the particle diameter being 3:1, SiC particle with the volume ratio of SiC is 10 μm.
The present embodiment is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, concrete operation step is:
(1) raw materials:
A: preparation SiO 2coated SiC particle:
1) getting α-SiC particle 9.63g is scattered in aqueous ethanolic solution, adds citric acid and regulates PH=2, obtain SiC dispersion liquid;
2) getting tetraethoxy 8.4ml adds in SiC dispersion liquid prepared by step (1), and 30 DEG C are stirred 4h, then drips ammoniacal liquor and regulate PH=9, stirs to obtain plural gel;
3) plural gel prepared by step (2) is ground after forced air drying 2h under 80 DEG C of conditions, obtain SiO 2coated SiC particle;
B: preparation Al 2o 3:
1) Al (OH) is got 315min is calcined, obtained Al at 1200 DEG C 2o 3;
(2) matrix material is prepared:
1) according to Al 2o 3be the SiO that 7:3 takes step (1) and prepares with the volume ratio of SiC 2coated SiC particle and Al 2o 3, by SiO 2coated SiC particle and Al 2o 3mix, grinding, cross 120 sieve 6 times, 10MPa tableting under pressure is shaping, obtained sheet-like composite after 90MPa isostatic cool pressing;
2) by step 1) sheet-like composite prepared is placed in boosting attemperator, attemperator being inserted frequency is heat in the multimode cavity microwave oven of 2.45GHz, open microwave source, regulate microwave input power, be warming up to 600 DEG C with 12 DEG C/min speed, regulate microwave input power again, with the ramp to 1600 DEG C of 20 DEG C/min, detection of reflected power simultaneously, insulation 30min, control is chilled to room temperature, obtains the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
Fig. 5 is the XRD figure of the present embodiment matrix material, occurs mullite phase as seen from the figure in the present embodiment matrix material, and the volume content of mullite accounts for 20 ~ 25% of cumulative volume;
Fig. 6 is the SEM figure of the present embodiment matrix material, and in the present embodiment matrix material, mullite crystal whisker is elongated as seen from the figure, starts to extend.
Embodiment 4
The present embodiment is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, by SiO 2coated SiC particle, Al 2o 3for raw material is made, wherein Al 2o 3be 4:1 with the volume ratio of SiC; SiC and SiO 2volume ratio be the particle diameter of 1:1, SiC particle be 5 μm.
The present embodiment is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, concrete operation step is:
(1) raw materials:
A: preparation SiO 2coated SiC particle:
1) getting α-SiC particle 6.42g is scattered in aqueous ethanolic solution, adds citric acid and regulates PH=2, obtain SiC dispersion liquid;
2) getting tetraethoxy 16.8ml adds in SiC dispersion liquid prepared by step (1), and 30 DEG C are stirred 4h, then drips ammoniacal liquor and regulate PH=9, stirs to obtain plural gel;
3) plural gel prepared by step (2) is ground after forced air drying 2h under 80 DEG C of conditions, obtain SiO 2coated SiC particle;
B: preparation Al 2o 3:
1) Al (OH) is got 315min is calcined, obtained Al at 1200 DEG C 2o 3;
(2) matrix material is prepared:
1) according to Al 2o 3be the SiO that 4:1 takes step (1) and prepares with the volume ratio of SiC 2coated SiC particle and Al 2o 3, by SiO 2coated SiC particle and Al 2o 3mix, grinding, cross 120 sieve 6 times, 10MPa tableting under pressure is shaping, obtained sheet-like composite after 100MPa isostatic cool pressing;
2) by step 1) sheet-like composite prepared is placed in boosting attemperator, attemperator being inserted frequency is heat in the multimode cavity microwave oven of 2.45GHz, open microwave source, regulate microwave input power, be warming up to 600 DEG C with 10 DEG C of speed, regulate microwave input power again, with the ramp to 1350 DEG C of 20 DEG C/min, detection of reflected power simultaneously, insulation 60min, control is chilled to room temperature, obtains the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
Fig. 7 is the XRD figure of the present embodiment matrix material, occurs mullite phase as seen from the figure in the present embodiment matrix material, and the volume content of mullite accounts for 5 ~ 10% of total composite volume.
Fig. 8 is the SEM figure of the present embodiment matrix material, occurs a small amount of mullite crystal whisker as seen from the figure in the present embodiment matrix material.
Embodiment 5
The present embodiment is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, by SiO 2coated SiC particle, Al 2o 3for raw material is made, wherein Al 2o 3be 4:1 with the volume ratio of SiC; SiC and SiO 2volume ratio be the particle diameter of 2:1, SiC particle be 15 μm.
The present embodiment is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, concrete operation step is:
(1) raw materials:
A: preparation SiO 2coated SiC particle:
1) getting-SiC particle 9.63g is scattered in aqueous ethanolic solution, adds citric acid and regulates PH=2, obtain SiC dispersion liquid;
2) getting tetraethoxy 12.6ml adds in SiC dispersion liquid prepared by step (1), and 30 DEG C are stirred 4h, then drips ammoniacal liquor and regulate PH=9, stirs to obtain plural gel;
3) plural gel prepared by step (2) is ground after forced air drying 2h under 80 DEG C of conditions, obtain SiO 2coated SiC particle;
B: preparation Al 2o 3:
1) Al (OH) is got 315min is calcined, obtained Al at 1200 DEG C 2o 3;
(2) matrix material is prepared:
1) according to Al 2o 3be the SiO that 4:1 takes step (1) and prepares with the volume ratio of SiC 2coated SiC particle and Al 2o 3, by SiO 2coated SiC particle and Al 2o 3mix, grinding, cross 120 sieve 6 times, 10MPa tableting under pressure is shaping, obtained sheet-like composite after 100MPa isostatic cool pressing;
2) by step 1) sheet-like composite prepared is placed in boosting attemperator, attemperator being inserted frequency is heat in the multimode cavity microwave oven of 2.45GHz, open microwave source, regulate microwave input power, be warming up to 600 DEG C with 14 DEG C of speed, regulate microwave input power again, with the ramp to 1450 DEG C of 18 DEG C/min, detection of reflected power simultaneously, insulation 120min, control is chilled to room temperature, obtains the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
Fig. 9 is the XRD figure of the present embodiment matrix material, occurs mullite phase as seen from the figure in the present embodiment matrix material, and the volume content of mullite accounts for 30 ~ 35% of total composite volume.
Figure 10 is the SEM figure of the present embodiment matrix material, and in the present embodiment matrix material, mullite crystal whisker is grown up as seen from the figure, becomes connection strong between particle.
Comparative example 1
This comparative example is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, by SiC and Al 2o 3for raw material is made, wherein Al 2o 3the particle diameter being 1:1, SiC particle with the volume ratio of SiC is 10 μm.
The present embodiment is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, concrete operation step is:
(1) raw materials:
A: preparation Al 2o 3:
Get Al (OH) 35min is calcined, obtained Al at 1300 DEG C 2o 3;
(2) matrix material is prepared:
1) according to Al 2o 3be 1:1 with the volume ratio of SiC, take Al prepared by SiC particle and step (1) 2o 3, by SiC particle and Al 2o 3mix, grinding, cross 120 sieve 6 times, 10MPa tableting under pressure is shaping, obtained sheet-like composite after 100MPa isostatic cool pressing;
2) by step 1) sheet-like composite prepared is placed in boosting attemperator, attemperator being inserted frequency is heat in the multimode cavity microwave oven of 2.45GHz, open microwave source, regulate microwave input power, be warming up to 600 DEG C with 10 DEG C/min speed, regulate microwave input power again, with the ramp to 1500 DEG C of 15 DEG C/min, detection of reflected power simultaneously, insulation 30min, control is chilled to room temperature, obtains the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
Figure 11 is the XRD figure of the present embodiment matrix material, as seen from the figure Al in the present embodiment matrix material 2o 3occupy an leading position, occurred SiO 2phase, this be surface of SiC be oxidized to SiO 2, the mullite now generated is few, to such an extent as to can't detect.
Figure 12 is the SEM figure of the present embodiment matrix material, and in the present embodiment matrix material, major part is SiC and Al as seen from the figure 2o 3particle, there is the SiO of a small amount of melting in the oxidation of SiC grain edges 2.
Comparative example 2
The present embodiment is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, by SiO 2, SiC particle, Al 2o 3for raw material is made, wherein Al 2o 3be 1:1 with the volume ratio of SiC; SiC and SiO 2volume ratio be the particle diameter of 5:1, SiC particle be 10 μm.
The present embodiment is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, concrete operation step is:
(1) raw materials:
A: preparation Al 2o 3:
1) Al (OH) is got 35min is calcined, obtained Al at 1300 DEG C 2o 3;
(2) matrix material is prepared:
1) according to Al 2o 3be 1:1, SiC and SiO with the volume ratio of SiC 2volume ratio be 5:1, take SiC particle, SiO 2al prepared by particle and step (1) 2o 3, by SiC, SiO 2and Al 2o 3particle mixes, grinding, and cross 120 sieve 6 times, 10MPa tableting under pressure is shaping, obtained sheet-like composite after 100MPa isostatic cool pressing;
2) by step 1) sheet-like composite prepared is placed in boosting attemperator, attemperator being inserted frequency is heat in the multimode cavity microwave oven of 2.45GHz, open microwave source, regulate microwave input power, be warming up to 600 DEG C with 10 DEG C/min speed, regulate microwave input power again, with the ramp to 1500 DEG C of 15 DEG C/min, detection of reflected power simultaneously, insulation 30min, control is chilled to room temperature, obtains the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
Figure 13 is the XRD figure of the present embodiment matrix material, occurs mullite phase as seen from the figure in the present embodiment matrix material, and the volume content of mullite phase approximately account for 5 ~ 10% of cumulative volume.
Figure 14 is the SEM figure of the present embodiment matrix material, occurs a small amount of mullite crystal whisker bridge joint as seen from the figure in the present embodiment matrix material.
Comparative example 3
The present embodiment is containing the Al of mullite wild phase 2o 3/ SiC ceramic matrix composite material, by SiO 2coated SiC particle, Al 2o 3for raw material is made, wherein Al 2o 3be 1:1 with the volume ratio of SiC; SiC and SiO 2volume ratio be the particle diameter of 5:1, SiC particle be 10 μm.
The present embodiment is containing the Al of mullite wild phase 2o 3the preparation method of/SiC ceramic matrix composite material, concrete operation step is:
(1) raw materials:
A: preparation SiO 2coated SiC particle:
1) getting α-SiC particle 32.1g is scattered in aqueous ethanolic solution, adds citric acid and regulates PH=3, obtain SiC dispersion liquid;
2) getting tetraethoxy 16.7ml adds in SiC dispersion liquid prepared by step (1), and 30 DEG C are stirred 4h, then drips ammoniacal liquor and regulate PH=8, stirs to obtain plural gel;
3) plural gel prepared by step (2) is ground after forced air drying 2h under 80 DEG C of conditions, obtain SiO 2coated SiC particle;
B: preparation Al 2o 3:
1) Al (OH) is got 35min is calcined, obtained Al at 1300 DEG C 2o 3;
(2) matrix material is prepared:
1) according to Al 2o 3be the SiO that 1:1 takes step (1) and prepares with the volume ratio of SiC 2coated SiC particle and Al 2o 3, by SiO 2coated SiC particle and Al 2o 3mix, grinding, cross 120 sieve 6 times, 10MPa tableting under pressure is shaping, obtained sheet-like composite after 100MPa isostatic cool pressing;
2) by step 1) sheet-like composite prepared is placed in the conventional chamber type electric resistance furnace of tungsten, carry out normal sintering, 600 DEG C are warming up to 10 DEG C/min speed, regulate temperature rise rate again, with the ramp to 1500 DEG C of 15 DEG C/min, insulation 30min, control is chilled to room temperature, obtains the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
Figure 15 is the XRD figure of the present embodiment matrix material, occurs mullite phase as seen from the figure in the present embodiment matrix material, and the volume content of mullite phase account for 10 ~ 15% of cumulative volume.
Figure 16 is the SEM figure of the present embodiment matrix material, occurs mullite crystal whisker as seen from the figure in the present embodiment matrix material.
Test example
Al containing mullite wild phase prepared by testing example 1 ~ 3 and comparative example 1 ~ 3 2o 3the toughness of/SiC ceramic matrix composite material
Testing method: adopt monolateral otch amount method (SENB) to measure the toughness SENB of matrix material
Test result is as shown in table 1
Al containing mullite wild phase prepared by table 1 embodiment 1 ~ 3 and comparative example 1 ~ 3 2o 3the Toughness comparison of/SiC ceramic matrix composite material
Numbering Fracture toughness property (Mpa m 1/2)
Embodiment 1 5.6±0.1
Embodiment 2 4.5±0.1
Embodiment 3 3.8±0.2
Comparative example 1 2.6±0.2
Comparative example 2 2.4±0.1
Comparative example 3 3.2±0.2

Claims (10)

1. the Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material, is characterized in that, makes: SiO primarily of following raw material 2coated SiC particle, Al 2o 3; Wherein Al 2o 3be 1 ~ 4:1 with the volume ratio of SiC; SiC and SiO 2volume ratio be 1 ~ 10:1.
2. the Al containing mullite wild phase as claimed in claim 1 2o 3/ SiC ceramic matrix composite material, is characterized in that, the particle diameter of described SiC particle is 5 ~ 15 μm.
3. one kind contains the Al of mullite wild phase as claimed in claim 1 2o 3the preparation method of/SiC ceramic matrix composite material, is characterized in that, comprises following operation steps:
(1) by SiO 2coated SiC particle and Al 2o 3after powder mixed grinding, compression molding, obtained sheet-like composite;
(2) sheet-like composite microwave heating sintering step (1) prepared, obtains the described Al containing mullite wild phase 2o 3/ SiC ceramic matrix composite material.
4. the Al containing mullite wild phase as claimed in claim 3 2o 3the preparation method of/SiC ceramic matrix composite material, is characterized in that, microwave heating described in step (2) is sintered to and is heated to 1300 ~ 1600 DEG C, and insulation 30 ~ 120min, air cooling is to room temperature.
5. the Al containing mullite wild phase as claimed in claim 3 2o 3the preparation method of/SiC ceramic matrix composite material, it is characterized in that, the detailed process of the sintering of microwave heating described in step (2) is: first with the ramp to 600 DEG C of 10 ~ 15 DEG C/min, then with ramp to 1300 ~ 1600 DEG C of 15 ~ 20 DEG C/min, insulation 30 ~ 120min, air cooling is to room temperature.
6. the Al containing mullite wild phase as claimed in claim 3 2o 3the preparation method of/SiC ceramic matrix composite material, is characterized in that, described SiO 2the preparation method of coated SiC particle is comprise following operation steps:
A: by α-SiC Granular composite in aqueous ethanolic solution, regulates PH=2 ~ 3, obtains SiC dispersion liquid;
Add tetraethoxy, heated and stirred in b: the step a SiC dispersion liquid prepared, regulate PH=8 ~ 9, stir to obtain plural gel;
C: namely obtain described SiO after the plural gel drying and grinding prepared by step b 2coated SiC particle.
7. the Al containing mullite wild phase as claimed in claim 6 2o 3the preparation method of/SiC ceramic matrix composite material, is characterized in that, in step b, heated and stirred is stir 4h at 30 DEG C of temperature.
8. the Al containing mullite wild phase as claimed in claim 6 2o 3the preparation method of/SiC ceramic matrix composite material, is characterized in that, the drying described in step b is 80 DEG C of dry 2h.
9. the Al containing mullite wild phase as claimed in claim 3 2o 3the preparation method of/SiC ceramic matrix composite material, is characterized in that, described Al 2o 3preparation method be: by Al (OH) 3namely described Al is obtained at 1100 ~ 1300 DEG C of temperature lower calcination 5 ~ 30min 2o 3.
10. the Al containing mullite wild phase as claimed in claim 3 2o 3the preparation method of/SiC ceramic matrix composite material, is characterized in that, in step (1) after compression molding, under 90 ~ 110MPa pressure, isostatic cool pressing obtains described sheet-like composite.
CN201510055397.9A 2015-02-03 2015-02-03 Al2O3/SiC composite material containing mullite reinforcing phases and method for preparing Al2O3/SiC composite material containing mullite reinforcing phases Pending CN104692778A (en)

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CN108002850A (en) * 2016-10-28 2018-05-08 河南智联寰宇知识产权运营有限公司 Refractory brick containing spodumene and preparation method thereof
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CN108002849A (en) * 2016-10-28 2018-05-08 河南智联寰宇知识产权运营有限公司 Refractory brick containing magnesia and preparation method thereof
CN108101520A (en) * 2017-12-23 2018-06-01 深圳万佳互动科技有限公司 Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof
CN109422528A (en) * 2017-09-05 2019-03-05 张家港市五湖新材料技术开发有限公司 A kind of preparation method of aluminum oxide-silicon carbide high-temperature ceramic materials
CN112062573A (en) * 2020-09-11 2020-12-11 郑州大学 Sheet SiC-SiO2 composite material and preparation method thereof
CN113185268A (en) * 2021-04-29 2021-07-30 湖南大学 Preparation method of alumina ceramic material and alumina ceramic substrate
CN115231926A (en) * 2022-07-20 2022-10-25 洛阳理工学院 Method for preparing mullite-silicon carbide-combined ceramic by microwaves

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108002850A (en) * 2016-10-28 2018-05-08 河南智联寰宇知识产权运营有限公司 Refractory brick containing spodumene and preparation method thereof
CN108002851A (en) * 2016-10-28 2018-05-08 河南智联寰宇知识产权运营有限公司 Refractory brick containing mullite and preparation method thereof
CN108002849A (en) * 2016-10-28 2018-05-08 河南智联寰宇知识产权运营有限公司 Refractory brick containing magnesia and preparation method thereof
CN109422528A (en) * 2017-09-05 2019-03-05 张家港市五湖新材料技术开发有限公司 A kind of preparation method of aluminum oxide-silicon carbide high-temperature ceramic materials
CN108101520A (en) * 2017-12-23 2018-06-01 深圳万佳互动科技有限公司 Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof
CN112062573A (en) * 2020-09-11 2020-12-11 郑州大学 Sheet SiC-SiO2 composite material and preparation method thereof
CN113185268A (en) * 2021-04-29 2021-07-30 湖南大学 Preparation method of alumina ceramic material and alumina ceramic substrate
CN113185268B (en) * 2021-04-29 2022-04-22 湖南大学 Preparation method of alumina ceramic material and alumina ceramic substrate
CN115231926A (en) * 2022-07-20 2022-10-25 洛阳理工学院 Method for preparing mullite-silicon carbide-combined ceramic by microwaves
CN115231926B (en) * 2022-07-20 2023-10-27 洛阳理工学院 Method for preparing mullite combined silicon carbide ceramic by microwaves

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