CN115838281A - Composite ceramic material with low thermal expansion coefficient and preparation method thereof - Google Patents
Composite ceramic material with low thermal expansion coefficient and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 57
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 239000011812 mixed powder Substances 0.000 claims abstract description 33
- 239000011268 mixed slurry Substances 0.000 claims abstract description 29
- 238000011065 in-situ storage Methods 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 16
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000465 moulding Methods 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000004677 Nylon Substances 0.000 claims description 9
- 229920001778 nylon Polymers 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910052878 cordierite Inorganic materials 0.000 abstract description 43
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 abstract description 43
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 abstract description 43
- 239000012071 phase Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 description 37
- 230000004888 barrier function Effects 0.000 description 33
- 239000011248 coating agent Substances 0.000 description 21
- 238000000576 coating method Methods 0.000 description 21
- 230000007613 environmental effect Effects 0.000 description 18
- 239000011153 ceramic matrix composite Substances 0.000 description 14
- 229910001220 stainless steel Inorganic materials 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000003825 pressing Methods 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- -1 rare earth silicates Chemical class 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000008646 thermal stress Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/60—Efficient propulsion technologies, e.g. for aircraft
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Abstract
The invention discloses a composite ceramic material with low thermal expansion coefficient and a preparation method thereof, wherein the preparation method comprises the following steps: adding MgO and Al 2 O 3 、SiO 2 And ZrO 2 Mixing the four raw material powders according to a proportion to obtain mixed powder A; dispersing the mixed powder A into a ball milling medium to form mixed slurry, and carrying out wet ball milling on the mixed slurry to obtain ball-milled slurry; drying and sieving the ball-milled slurry to obtain mixed powder B; tabletting and molding the mixed powder B by using a press machine to obtain a block raw material; and putting the block raw material into a high-temperature furnace for in-situ solid-phase reaction to obtain the low-thermal expansion coefficient composite ceramic material generated by the in-situ reaction. The cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient is directly prepared by adopting oxide powder as a raw material through an in-situ solid-phase reaction method, has low density and uniform two-phase distribution, and is thermally expanded with a SiC composite material matrixProximity and low thermal conductivity.
Description
Technical Field
The invention relates to the technical field of thermal barrier/environmental barrier coating materials, in particular to a composite ceramic material with a low thermal expansion coefficient and a preparation method thereof.
Background
In recent years, with the development of aircraft engines towards high flow ratio, high thrust-weight ratio and high inlet temperature, hot end parts of engines are exposed to increasingly severe and complex service environments. With SiC f The ceramic matrix composite represented by the/SiC has the advantages of light weight, high strength, high toughness, high temperature resistance and the like, and is an ideal material for hot end parts of future aircraft engines. The thermal barrier/environmental barrier coating material (T/EBC) is a layer of ceramic coating material sprayed on the surface of a hot end part of an aeroengine, has the function of protecting a SiCf/SiC part from being corroded by external high-temperature fuel gas in the service process, and has the performance characteristics of high temperature resistance, corrosion resistance and thermal expansion matching with a matrix.
In view of the importance of thermal/environmental barrier coating materials in the protection of aircraft engines, many researchers in countries around the world have been working on the development of thermal/environmental barrier coating materials. To date, the most advanced thermal/environmental barrier coating material is rare earth silicates (RE) 2 SiO 5 And RE 2 Si 2 O 7 ) It has the advantages of high temperature resistance, corrosion resistance and low thermal conductivity. However, the rare earth silicate thermal barrier/environmental barrier coating material has the problem of poor thermal expansion matching with the SiCf/SiC ceramic matrix composite material. The reason is that the SiCf/SiC ceramic matrix composite material has low thermal expansion coefficient which is 3-5 multiplied by 10 at 1200 DEG C -6 The thermal expansion coefficient of the rare earth silicate thermal barrier/environmental barrier coating material is generally 6 x 10 -6 More than K. Because the thermal expansion coefficient of the rare earth silicate thermal barrier/environmental barrier coating material is different from that of the SiCf/SiC ceramic matrix composite material, huge thermal stress can be generated at the interface of the coating and the matrix in the service process, so that the coating material is cracked and fails. Therefore, it is an important problem to be solved urgently to reduce the thermal expansion coefficient of the thermal barrier/environmental barrier coating material and develop a novel thermal barrier/environmental barrier coating material with good thermal expansion matching with the SiCf/SiC ceramic matrix composite material.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides a composite ceramic material with a low thermal expansion coefficient and a preparation method thereof, so as to solve the above problems in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, a method for preparing a composite ceramic material with a low thermal expansion coefficient is provided, which comprises the following steps:
(1) Mixing MgO and Al 2 O 3 、SiO 2 And ZrO 2 Mixing the four raw material powders according to a certain proportion to obtain mixed powder A;
(2) Dispersing the mixed powder A in the step (1) into a ball milling medium to form mixed slurry, and carrying out wet ball milling on the mixed slurry to obtain ball-milled slurry;
(3) Drying and sieving the ball-milled slurry in the step (2) to obtain mixed powder B;
(4) Tabletting and molding the mixed powder B in the step (3) by using a press machine to obtain a block raw material;
(5) And (4) putting the block raw material in the step (4) into a high-temperature furnace to perform in-situ solid-phase reaction to obtain the low-thermal expansion coefficient cordierite/zirconium silicate composite ceramic material generated by the in-situ reaction.
Aiming at the bottleneck problems that the existing rare earth silicate thermal barrier/environmental barrier coating material has poor thermal expansion matching property with a SiCf/SiC ceramic matrix composite substrate, is easy to crack and cannot meet the service requirement of an extreme gas environment, the invention provides a new generation thermal barrier/environmental barrier coating material which uses a cordierite material with a low expansion coefficient as a new generation thermal barrier/environmental barrier coating material, and further adjusts the thermal expansion coefficient of ceramic by compounding with zirconium silicate with high thermal expansion so as to ensure that the thermal expansion coefficient of ceramic is matched with the SiCf/SiC ceramic matrix composite material in a thermal expansion way, so that the thermal barrier/environmental barrier coating material is a novel thermal barrier/environmental barrier coating material with a low thermal expansion coefficient and good thermal expansion matching property with the SiCf/SiC ceramic matrix composite material. The cordierite/zirconium silicate composite ceramic material is prepared by adopting an in-situ high-temperature solid-phase reaction method with simple process and low cost. The prepared cordierite/zirconium silicate composite ceramic material has the advantages of uniform component distribution and good thermal expansion matching with the SiCf/SiC ceramic matrix composite material, can provide long-term effective protection for the SiC/SiC ceramic matrix composite material matrix as a coating material, and has good application prospect in the field of thermal barrier/environmental barrier coating materials.
Preferably, the molar ratio of the four raw materials in the step (1) is MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 =（1～2）:（1～4）：（1～6）：（0.01～1）。
Specifically, the composite ceramic material with low thermal expansion coefficient is prepared from MgO and Al 2 O 3 、SiO 2 And ZrO 2 Or mineral containing the four substances is prepared by taking the raw materials as raw materials; the molar ratio of the four raw materials is MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 =（1～2）:（1～4）：（1～6）：（0.01～1）。
Preferably, the MgO and Al in the step (1) 2 O 3 、SiO 2 And ZrO 2 The grain diameters of the four raw materials are all 20-2000 nm.
Preferably, the ball milling medium in the step (2) is absolute ethyl alcohol or deionized water, the ball-milled grinding balls are agate balls or zirconia balls, and the ball milling tank is made of nylon or agate; the rotation speed of the ball milling is 200-500 r/min, and the ball milling time is 5-40 h.
Preferably, the solid content in the mixed slurry in the step (2) is 20-80%.
Preferably, the drying in the step (3) is drying for 12 to 36 hours in an oven at a temperature of between 80 and 150 ℃; the number of the sieved meshes is 200-500 meshes.
Preferably, the pressure of the press in the step (4) is 100-300 MPa, and the dwell time is 5-10 min. Specifically, the die used for tabletting is a round stainless steel die, and the phi of the block raw material is 8-30 mm.
Preferably, the reaction atmosphere of the in-situ solid-phase reaction in the step (5) is air, the reaction temperature is 1000-1400 ℃, and the reaction time is 10-30 h.
In a second aspect of the present invention, the low thermal expansion coefficient is obtained by the production method of the first aspectThe grain size of the composite ceramic material with low thermal expansion coefficient is 0.1-10 mu m, the porosity is 0-15 percent, and the thermal expansion coefficient is (2.5-4) multiplied by 10 -6 /℃。
In summary, compared with the prior art, the invention has the advantages that:
1. the cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient is directly prepared by adopting oxide powder as a raw material through an in-situ solid-phase reaction method. The preparation method has the advantages of simple process, low cost and low requirement on equipment, and is convenient for large-scale popularization and application.
2. The cordierite/zirconium silicate composite ceramic material has the advantages of low density, uniform two-phase distribution, thermal expansion close to that of a SiC composite material substrate and low thermal conductivity, has small thermal stress when being used as a thermal barrier/environmental barrier coating material, and is not easy to crack.
Drawings
FIG. 1 is an X-ray diffraction pattern of a cordierite/zirconium silicate composite ceramic material having a low coefficient of thermal expansion prepared in example 1 of the present invention.
FIG. 2 is a micro-topography of a low coefficient of thermal expansion cordierite/zirconium silicate composite ceramic material prepared in example 1 of the present invention.
FIG. 3 is a graph showing the distribution of the grain size of the cordierite/zirconium silicate composite ceramic material having a low coefficient of thermal expansion prepared in example 2 of the present invention.
FIG. 4 is a graph showing the thermal expansion coefficient of a cordierite/zirconium silicate composite ceramic material having a low thermal expansion coefficient prepared in example 3 of the present invention.
FIG. 5 is a graph showing the thermal expansion coefficient of a cordierite/zirconium silicate composite ceramic material having a low thermal expansion coefficient prepared in example 4 of the present invention.
Detailed Description
The present invention is further described below.
Example 1
The embodiment provides a cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient and a preparation method thereof, and the preparation method comprises the following steps:
（1）according to MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 The molar ratios of = 2.
(2) And dispersing the mixed powder into an absolute ethyl alcohol solution to form mixed slurry, wherein the solid content of the mixed slurry is controlled to be 20%. Pouring the mixed slurry into a nylon ball milling tank, and adding agate grinding balls; and sealing the ball milling tank, and then putting the ball milling tank into a ball mill for ball milling, wherein the rotating speed of the ball mill is 300 revolutions per minute, and the ball milling time is 30 hours.
(3) And (3) putting the ground paste into an oven for drying at 100 ℃ for 24 h. And (4) sieving the dried powder with a 300-mesh sieve to obtain uniformly mixed dry mixed powder B.
(4) And (3) putting the dried mixed powder B into a stainless steel die of a press, and maintaining the pressure at 100MPa for 10 min to obtain a green block raw material with the size phi of 8 mm.
(5) Putting the green block raw material obtained by dry pressing into a muffle furnace for in-situ solid-phase reaction, heating to 1400 ℃ in air atmosphere, preserving heat for 10h, and naturally cooling to obtain the cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient generated by in-situ reaction.
The X-ray diffraction pattern of the obtained cordierite/zirconium silicate composite ceramic material with the low thermal expansion coefficient is shown in figure 1, and as can be seen from figure 1, the phase of the prepared cordierite/zirconium silicate composite ceramic material with the low thermal expansion coefficient is a cordierite/zirconium silicate dual-phase.
Example 2
The embodiment provides a cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient and a preparation method thereof, and the preparation method comprises the following steps:
(1) According to MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 The molar ratios of = 2.
(2) And dispersing the mixed powder into an absolute ethyl alcohol solution to form mixed slurry, wherein the solid content of the mixed slurry is controlled to be 20%. Pouring the mixed slurry into a nylon ball milling tank, and adding agate grinding balls; and sealing the ball milling tank, and then putting the ball milling tank into a ball mill for ball milling, wherein the rotating speed of the ball mill is 400 r/min, and the ball milling time is 20h.
(3) And (3) putting the slurry subjected to ball milling into an oven for drying at the drying temperature of 110 ℃ for 20 hours. And (4) sieving the dried powder with a 300-mesh sieve to obtain uniformly mixed dry mixed powder B.
(4) And (3) putting the dried mixed powder B into a stainless steel die of a press, and maintaining the pressure at 100MPa for 10 min to obtain a green block raw material with the size phi of 20 mm.
(5) And (3) putting the green body block raw material obtained by dry pressing into a muffle furnace for in-situ solid-phase reaction, heating to 1300 ℃ in the air atmosphere, preserving the heat for 15 hours, and naturally cooling to obtain the cordierite/zirconium silicate composite ceramic material with the low thermal expansion coefficient generated by the in-situ reaction.
The micro-topography of the obtained low-thermal expansion coefficient cordierite/zirconium silicate composite ceramic material is shown in fig. 2, and as can be seen from fig. 2, the prepared low-thermal expansion coefficient cordierite/zirconium silicate composite ceramic material has uniform distribution of cordierite and zirconium silicate; in FIG. 2, the dark color is a cordierite phase and the white color is a zirconium silicate phase.
Example 3
The embodiment provides a cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient and a preparation method thereof, and the preparation method comprises the following steps:
(1) According to the weight ratio of MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 The molar ratios of = 2.
(2) And dispersing the mixed powder into an absolute ethyl alcohol solution to form mixed slurry, wherein the solid content of the mixed slurry is controlled to be 20%. Pouring the mixed slurry into a nylon ball milling tank, and adding agate grinding balls; and sealing the ball milling tank, and then putting the ball milling tank into a ball mill for ball milling, wherein the rotating speed of the ball mill is 450 revolutions per minute, and the ball milling time is 15 hours.
(3) And (3) putting the ground paste subjected to ball milling into an oven for drying at the drying temperature of 120 ℃ for 20 hours. And (4) sieving the dried powder with a 300-mesh sieve to obtain uniformly mixed dry mixed powder B.
(4) And (3) putting the dried mixed powder B into a stainless steel die of a press, and maintaining the pressure for 10 min at the pressure of 100MPa to obtain a green block raw material with the size phi of 20 mm.
(5) Putting the green block raw material obtained by dry pressing into a muffle furnace for in-situ solid-phase reaction, heating to 1200 ℃ in air atmosphere, preserving heat for 20 hours, and naturally cooling to obtain the cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient generated by in-situ reaction.
The distribution of the grain size of the obtained cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient is shown in fig. 3, and it can be seen from fig. 3 that the grain size of the prepared cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient is distributed in the range of 0.2 to 2.0 μm.
Example 4
The embodiment provides a cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient and a preparation method thereof, and the preparation method comprises the following steps:
(1) According to MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 The molar ratios of = 2.
(2) And dispersing the mixed powder into an absolute ethyl alcohol solution to form mixed slurry, wherein the solid content of the mixed slurry is controlled to be 20%. Pouring the mixed slurry into an agate ball milling tank, and putting zirconia grinding balls into the tank; and sealing the ball milling tank, and then putting the ball milling tank into a ball mill for ball milling, wherein the rotating speed of the ball mill is 500 revolutions per minute, and the ball milling time is 10 hours.
(3) And (3) putting the slurry subjected to ball milling into an oven for drying at the temperature of 130 ℃ for 18h. And (3) sieving the dried powder with a 300-mesh sieve to obtain uniformly mixed dry mixed powder B.
(4) And (3) putting the dried mixed powder B into a stainless steel die of a press, and maintaining the pressure at 150 MPa for 8 min to obtain a green block raw material with the size phi of 30 mm.
(5) Putting the green block raw material obtained by dry pressing into a muffle furnace for in-situ solid-phase reaction, heating to 1150 ℃ in air atmosphere, preserving heat for 24 hours, and naturally cooling to obtain the cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient generated by in-situ reaction.
The thermal expansion coefficient curve of the obtained cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient is shown in FIG. 4, and as can be seen from FIG. 4, the thermal expansion coefficient of the prepared cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient is 3.3 multiplied by 10 within the range of 200-1200 DEG C -6 The temperature per DEG C is well matched with the thermal expansion of the SiCf/SiC ceramic matrix composite material. The density of the composite ceramic measured by an Archimedes drainage method is 99%, and the porosity is 1%.
Example 5
The embodiment provides a cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient and a preparation method thereof, and the preparation method comprises the following steps:
(1) According to MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 The molar ratios of = 2.
(2) And dispersing the mixed powder into an absolute ethyl alcohol solution to form mixed slurry, wherein the solid content of the mixed slurry is controlled to be 20%. Pouring the mixed slurry into an agate ball milling tank, and putting zirconia grinding balls into the tank; and sealing the ball milling tank, and then putting the ball milling tank into a ball mill for ball milling, wherein the rotating speed of the ball mill is 200 revolutions per minute, and the ball milling time is 10 hours.
(3) And (3) putting the ground paste subjected to ball milling into an oven for drying at the drying temperature of 80 ℃ for 18h. And (4) sieving the dried powder with a 300-mesh sieve to obtain uniformly mixed dry mixed powder B.
(4) And (3) putting the dried mixed powder B into a stainless steel die of a press, and maintaining the pressure at 150 MPa for 8 min to obtain a green block raw material with the size phi of 30 mm.
(5) Putting the green block raw material obtained by dry pressing into a muffle furnace for in-situ solid-phase reaction, heating to 1100 ℃ in air atmosphere, preserving heat for 28h, and naturally cooling to obtain the cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient generated by in-situ reaction.
The thermal expansion coefficient curve of the obtained cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient is shown in FIG. 5, and as can be seen from FIG. 5,the prepared cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient has the thermal expansion coefficient of 3.4 multiplied by 10 within the temperature range of 200-1200 DEG C -6 The temperature per DEG C is good in thermal expansion matching with the SiCf/SiC ceramic matrix composite material. The density of the composite ceramic measured by an Archimedes drainage method is 90%, and the porosity is 10%.
Example 6
The embodiment provides a cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient and a preparation method thereof, and the preparation method comprises the following steps:
(1) According to MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 The molar ratios of =1.
(2) And dispersing the mixed powder into deionized water to form mixed slurry, wherein the solid content of the mixed slurry is controlled to be 80%. Pouring the mixed slurry into a nylon ball milling tank, and putting agate balls into the nylon ball milling tank for milling; and sealing the ball milling tank, and then putting the ball milling tank into a ball mill for ball milling, wherein the rotating speed of the ball mill is 500 revolutions per minute, and the ball milling time is 40 hours.
(3) And (3) putting the ground paste into an oven for drying at the drying temperature of 150 ℃ for 36h. And (3) sieving the dried powder with a 500-mesh sieve to obtain uniformly mixed dry mixed powder B.
(4) And (3) putting the dried mixed powder B into a stainless steel die of a press, and maintaining the pressure at 100MPa for 5 min to obtain a green block raw material with the size phi of 30 mm.
(5) Putting the green block raw material obtained by dry pressing into a muffle furnace for in-situ solid-phase reaction, heating to 1000 ℃ in air atmosphere, preserving heat for 10 hours, and naturally cooling to obtain the cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient generated by in-situ reaction.
The thermal expansion coefficient of the prepared cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient is 2.0 multiplied by 10 within the range of 200-1200 DEG C -6 The temperature per DEG C is well matched with the thermal expansion of the SiCf/SiC ceramic matrix composite material.
Example 7
The embodiment provides a cordierite/zirconium silicate composite ceramic material with a low thermal expansion coefficient and a preparation method thereof, and the preparation method comprises the following steps:
(1) According to the weight ratio of MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 1.5.
(2) And dispersing the mixed powder into deionized water to form mixed slurry, wherein the solid content of the mixed slurry is controlled to be 50%. Pouring the mixed slurry into a nylon ball milling tank, and putting agate balls into the nylon ball milling tank for milling; and sealing the ball milling tank, and then putting the ball milling tank into a ball mill for ball milling, wherein the rotating speed of the ball mill is 350 r/min, and the ball milling time is 5h.
(3) And (3) putting the ground paste subjected to ball milling into an oven for drying at the drying temperature of 80 ℃ for 12h. And (3) sieving the dried powder with a 200-mesh sieve to obtain uniformly mixed dry mixed powder B.
(4) And (3) putting the dried mixed powder B into a stainless steel die of a press, and maintaining the pressure at 300MPa for 10 min to obtain a green block raw material with the size phi of 30 mm.
(5) Putting the green block raw material obtained by dry pressing into a muffle furnace for in-situ solid-phase reaction, heating to 1000 ℃ in air atmosphere, preserving heat for 30h, and naturally cooling to obtain the cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient generated by in-situ reaction.
The thermal expansion coefficient of the prepared cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient is 4.0 multiplied by 10 within the range of 200-1200 DEG C -6 The temperature per DEG C is well matched with the thermal expansion of the SiCf/SiC ceramic matrix composite material.
In conclusion, the cordierite/zirconium silicate composite ceramic material with the low thermal expansion coefficient is directly prepared by adopting the oxide powder as the raw material through an in-situ solid-phase reaction method. The prepared cordierite/zirconium silicate composite ceramic material with low thermal expansion coefficient has the advantages of low density, uniform two-phase distribution, thermal expansion close to that of a SiC composite material matrix and low thermal conductivity, and has the advantages of small thermal stress and difficult cracking when being used as a thermal barrier/environmental barrier coating material. The prepared composite ceramic material with low thermal expansion coefficient and the crystal of the composite ceramic material with low thermal expansion coefficientThe grain size is 0.1-10 μm, the porosity is 0-15%, and the thermal expansion coefficient is (2.5-4) × 10 -6 /℃。
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that those skilled in the art may make variations, modifications, substitutions and alterations within the scope of the present invention without departing from the spirit and scope of the present invention.
Claims (9)
1. The preparation method of the composite ceramic material with low thermal expansion coefficient is characterized by comprising the following steps:
(1) Adding MgO and Al 2 O 3 、SiO 2 And ZrO 2 Mixing the four raw material powders according to a certain proportion to obtain mixed powder A;
(2) Dispersing the mixed powder A in the step (1) into a ball milling medium to form mixed slurry, and carrying out wet ball milling on the mixed slurry to obtain ball-milled slurry;
(3) Drying and sieving the ball-milled slurry in the step (2) to obtain mixed powder B;
(4) Tabletting and molding the mixed powder B in the step (3) by using a press machine to obtain a block raw material;
(5) And (4) putting the block raw material in the step (4) into a high-temperature furnace for in-situ solid-phase reaction to obtain the low-thermal expansion coefficient composite ceramic material generated by the in-situ reaction.
2. The method for preparing a composite ceramic material with a low thermal expansion coefficient according to claim 1, wherein the molar ratio of the four raw materials in step (1) is MgO: al (Al) 2 O 3 ：SiO 2 ：ZrO 2 =（1～2）:（1～4）：（1～6）：（0.01～1）。
3. The method for preparing a composite ceramic material with a low coefficient of thermal expansion according to claim 1, wherein the MgO and Al are used in the step (1) 2 O 3 、SiO 2 And ZrO 2 The grain diameters of the four raw materials are all 20-2000 nm.
4. The preparation method of the composite ceramic material with the low thermal expansion coefficient according to claim 1, wherein in the step (2), the ball milling medium is absolute ethyl alcohol or deionized water, the ball milling grinding balls are agate balls or zirconia balls, and the ball milling tank is made of nylon or agate; the rotation speed of the ball milling is 200-500 r/min, and the ball milling time is 5-40 h.
5. The method of claim 1 wherein the solid content of the mixed slurry in step (2) is 20-80%.
6. The method for preparing the composite ceramic material with low thermal expansion coefficient according to claim 1, wherein the drying in the step (3) is drying in an oven at a temperature of 80-150 ℃ for 12-36 h; the number of the sieved meshes is 200-500 meshes.
7. The method for preparing a composite ceramic material with a low thermal expansion coefficient according to claim 1, wherein the pressure of the press in the step (4) is 100 to 300MPa, and the dwell time is 5 to 10 min.
8. The method for preparing the composite ceramic material with low thermal expansion coefficient according to claim 1, wherein the reaction atmosphere of the in-situ solid-phase reaction in the step (5) is air, the reaction temperature is 1000-1400 ℃, and the reaction time is 10-30 h.
9. A composite ceramic material having a low coefficient of thermal expansion, which is obtained by the production method as set forth in any one of claims 1 to 8, characterized in that the grain size of the composite ceramic material having a low coefficient of thermal expansion is 0.1 to 10 μm, the porosity is 0 to 15%, and the coefficient of thermal expansion is (2.5 to 4). Times.10 -6 /℃。
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| CN1277173A (en) * | 2000-07-13 | 2000-12-20 | 胡勇波 | Honeycomb ceramic as one kind of high-performance composite material |
| FR2991677A1 (en) * | 2012-06-08 | 2013-12-13 | Bosch Gmbh Robert | METHOD OF MAKING SENSOR SUPPORT AND SUPPORT AND SENSOR OBTAINED |
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