CN115974540A - Rare earth doped cordierite ceramic material and preparation method thereof - Google Patents
Rare earth doped cordierite ceramic material and preparation method thereof Download PDFInfo
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- 229910052878 cordierite Inorganic materials 0.000 title claims abstract description 75
- 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 title claims abstract description 75
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 73
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 48
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims description 40
- 239000011812 mixed powder Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003801 milling Methods 0.000 claims description 8
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 22
- 239000011248 coating agent Substances 0.000 description 15
- 238000000576 coating method Methods 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 230000004888 barrier function Effects 0.000 description 14
- 230000007613 environmental effect Effects 0.000 description 9
- 239000011153 ceramic matrix composite Substances 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 7
- 239000010935 stainless steel Substances 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- -1 rare earth silicate Chemical class 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
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- 229920001778 nylon Polymers 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention discloses a rare earth-doped cordierite ceramic material and a preparation method thereof, wherein the chemical expression of the rare earth-doped cordierite ceramic material is (Mg) 1‑x RE x ) 2 Al 4 Si 5 O 18+x Wherein x is more than or equal to 0 and less than or equal to 0.5, RE is one of Y, yb, lu, tm and Er; the grain size of the rare earth doped cordierite ceramic material is 0.2-8 mu m, the porosity is 0-10%, the high-temperature thermal conductivity is not higher than 1.5W/(m.K), and the thermal expansion coefficient is (2.0-5.0) multiplied by 10 ‑6 and/K. The preparation method is prepared by a solid-phase reaction method. The rare earth doped cordierite ceramic material prepared by the invention has wide component range and flexible and adjustable thermal conductivity and thermal expansion coefficient, and the thermal conductivity and the thermal expansion coefficient can be adjusted by changing the doping amount of rare earth elements. The rare earth doped cordierite ceramic material is preparedThe solid phase reaction method has the advantages of low raw material cost, simple process and low equipment requirement.
Description
Technical Field
The invention relates to the technical field of environmental barrier coating ceramic materials, in particular to a rare earth doped cordierite ceramic material and a preparation method thereof.
Background
SiC f The SiC ceramic matrix composite has the advantages of light weight, high strength, high toughness and high temperature resistance, and has important application in hot end parts of aircraft engines. However, siC f the/SiC ceramic matrix composite material is easy to corrode and degrade in the high-temperature combustion environment of an aircraft engine. An effective way to solve this problem is in SiC f And the surface of the/SiC ceramic matrix composite substrate is sprayed with an environmental barrier coating material (EBC), so that the SiCf/SiC component is protected from being corroded by external high-temperature fuel gas in the service process. Typically, environmental barrier coating materials (EBC) are required to have high temperature resistance, corrosion resistance, thermal expansion matching to the substrate, and low thermal conductivity.
To date, the most widely studied and applied environmental barrier coating material is the rare earth silicate material system (RE) 2 SiO 5 And RE 2 Si 2 O 7 ) It has the performances of high temperature resistance, corrosion resistance and low thermal conductivity. However, the thermal expansion coefficient of rare earth silicates is generally high, typically 6X 10 -6 More than K; the SiCf/SiC ceramic matrix composite material has a low thermal expansion coefficient which is 3-5 multiplied by 10 at 1200 DEG C -6 and/K. Therefore, the thermal expansion matching of the rare earth silicate environmental barrier coating material and the SiCf/SiC ceramic matrix composite material is generally poor. This results in the environmental barrier coating material developing a great thermal stress at the interface of the coating and the substrate during service, which leads to cracking failure of the coating material. Therefore, the development of a novel environmental barrier coating material with low thermal expansion coefficient and low thermal conductivity is an important problem to be solved urgently.
Disclosure of Invention
In order to solve the technical problems, the invention provides a rare earth doped cordierite ceramic material and a preparation method thereof, and aims to develop a novel environmental barrier coating material with low thermal conductivity and low thermal expansion coefficient.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided a rare earth-doped cordierite ceramic material having a chemical formula of (Mg) 1-x RE x ) 2 Al 4 Si 5 O 18+x Wherein x is more than or equal to 0 and less than or equal to 0.5, RE is one of Y, yb, lu, tm and Er.
Preferably, the grain size of the rare earth doped cordierite ceramic material is 0.2-8 mu m, the porosity is 0-10%, the high-temperature thermal conductivity is not higher than 1.5W/(m.K), and the thermal expansion coefficient is (2.0-5.0) multiplied by 10 -6 and/K. The use temperature of the rare earth doped cordierite ceramic material is between normal temperature and 1400 ℃.
Aiming at the bottleneck problems that the rare earth silicate environment barrier coating material in the prior art is poor in thermal expansion matching property with a SiCf/SiC ceramic matrix composite substrate, easy to crack and incapable of meeting the service requirement of an extreme gas environment, the invention provides a new generation of environment barrier coating material by using a cordierite material with a low expansion coefficient. Based on the characteristics of low thermal expansion coefficient and low thermal conductivity of cordierite, the thermal expansion coefficient and the thermal conductivity of the ceramic are further adjusted by doping rare earth elements, so that the ceramic is matched with the SiCf/SiC ceramic matrix composite in thermal expansion, and has the advantage of low thermal conductivity.
In a second aspect of the present invention, there is provided a method for preparing a rare earth-doped cordierite ceramic material, comprising the steps of:
(1) Mixing MgO and Al 2 O 3 、SiO 2 Mixing the powder and the rare earth oxide powder according to a ratio to obtain mixed powder A;
(2) Putting the mixed powder A in the step (1) into a ball milling tank, adding a ball milling medium and milling balls, and carrying out wet ball milling to obtain slurry;
(3) Drying and sieving the slurry obtained in the step (2) to obtain mixed powder B;
(4) Tabletting the mixed powder B in the step (3) by using a tabletting machine to obtain a block raw material;
(5) And (4) heating the block raw material in the step (4) in a muffle furnace to enable the block raw material to generate a solid phase reaction and generate the rare earth doped cordierite ceramic material.
Preferably, the MgO and Al in the step (1) 2 O 3 、SiO 2 The particle diameters of the powder and the rare earth oxide powder are less than or equal to 2 mu m; the molar ratio of four raw materials is MgO: al (Al) 2 O 3 ：SiO 2 : rare earth oxide = (1 to 2): 2:5: (0.1-1).
Preferably, the rare earth oxide is Y 2 O 3 、Yb 2 O 3 、Lu 2 O 3 、Tm 2 O 3 And Er 2 O 3 One kind of (1).
Preferably, the rotation speed of the ball milling in the step (2) is 300-600 r/min, and the ball milling time is 10-30 h. The ball milling medium is deionized water or absolute ethyl alcohol, the milling balls are agate balls or zirconia balls, the ball milling tank is made of nylon or agate, and the ball milling mode is planetary wheel ball milling.
Preferably, the solid content of the slurry in the step (2) is 10-60%.
Preferably, the drying in the step (3) is drying for 12-24 h at 80-120 ℃ in air atmosphere; the number of the sieved meshes is 300-600 meshes.
Preferably, the pressure of the tablet press in the step (4) is 100-300 MPa, and the pressure maintaining time is 1-10 min; the die used for tabletting forming is a stainless steel die.
Preferably, the solid phase reaction in the step (5) is carried out at 1000-1500 ℃ for 15-20 h under an air atmosphere.
The rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient is prepared by adopting a high-temperature solid-phase reaction method with simple process and low cost. The prepared rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient has uniform components, adjustable thermal expansion coefficient and low thermal conductivity, can be used as a high-temperature environment barrier coating material, and has good application prospect in the field of environment barrier coating materials.
In summary, compared with the prior art, the invention has the advantages that:
1、the thermal conductivity and the thermal expansion coefficient of the cordierite ceramic are improved for the first time in a rare earth doping mode, the rare earth doped cordierite ceramic material is obtained by a solid phase reaction method, the ceramic material has the advantages of high purity, low thermal conductivity and low thermal expansion coefficient, the high-temperature thermal conductivity is not higher than 1.5W/(m.K), and the thermal expansion coefficient is (2.0-5.0) multiplied by 10 -6 /K。
2. The rare earth doped cordierite ceramic material prepared by the invention has wide component range and flexible and adjustable thermal conductivity and thermal expansion coefficient, and the thermal conductivity and the thermal expansion coefficient can be adjusted by changing the doping amount of rare earth elements.
3. The solid phase reaction method adopted by the invention for preparing the rare earth doped cordierite ceramic material has the advantages of low raw material cost, simple process and low requirement on equipment. The method adopts oxide powder with low cost as a raw material, directly obtains the rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient through high-temperature solid phase reaction, belongs to a one-step method for preparing the ceramic material, and does not need to carry out secondary sintering on the ceramic. The method can be used for quickly preparing the rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient.
Drawings
FIG. 1 is an X-ray diffraction pattern of a low thermal conductivity, low coefficient of thermal expansion rare earth-doped cordierite ceramic material prepared in accordance with example 1 of the present invention.
FIG. 2 is a microstructure diagram of a low thermal conductivity, low coefficient of thermal expansion rare earth-doped cordierite ceramic material prepared in example 1 of the present invention.
FIG. 3 is a graph of the high temperature thermal conductivity of a low thermal conductivity, low coefficient of thermal expansion rare earth doped cordierite ceramic material prepared in accordance with example 2 of the present invention.
FIG. 4 is a graph of the coefficient of thermal expansion of a low thermal conductivity, low coefficient of thermal expansion rare earth doped cordierite ceramic material prepared in example 3 of the present invention.
FIG. 5 is a graph of the high temperature thermal conductivity of a low thermal conductivity, low coefficient of thermal expansion rare earth doped cordierite ceramic material prepared in example 3 of the present invention.
FIG. 6 is a graph of the grain size distribution of a low thermal conductivity, low coefficient of thermal expansion rare earth doped cordierite ceramic material prepared in accordance with example 4 of the present invention.
Detailed Description
The present invention is further described below.
Example 1
The embodiment provides a preparation method of a rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient, which comprises the following steps:
(1) MgO and Al with the grain diameter less than or equal to 2 mu m 2 O 3 、SiO 2 And Y 2 O 3 Raw material powders were mixed in a molar ratio of 1;
(2) Placing the mixed powder A into an agate ball mill, adding agate grinding balls, and adding absolute ethyl alcohol according to the proportion of 15-20% of solid content; sealing the ball milling tank, and putting the ball milling tank into a planetary ball mill with the rotating speed of 300 r/min for wet ball milling for 30 h to obtain ball-milled slurry;
(3) Putting the ball-milled slurry into a drying oven, drying for 20 hours at 100 ℃ in the air atmosphere, and sieving with a 300-mesh sieve to obtain mixed powder B;
(4) Putting the mixed powder B into a stainless steel mold of a tablet press, and maintaining the pressure at 200 MPa for 6 min to obtain a block raw material;
(5) Heating the block raw material in a muffle furnace, and carrying out solid phase reaction for 18h at 1400 ℃ in an air environment to obtain the rare earth-doped cordierite ceramic material with the grain size of 0.2-8 mu m and the porosity of 5 percent and low thermal conductivity and thermal expansion coefficient, wherein the chemical expression of the rare earth-doped cordierite ceramic material is (Mg) 1-x Y x ) 2 Al 4 Si 5 O 18+x Wherein x =0.5
The X-ray diffraction pattern of the prepared rare earth-doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient is shown in figure 1. As can be seen from FIG. 1, the prepared rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient keeps the same crystal structure as cordierite, and has no impurity phase, which indicates that the rare earth element Y is successfully dissolved into the crystal structure of cordierite.
The microstructure photograph of the prepared rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient is shown in figure 2. As can be seen from FIG. 2, the prepared rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient has a similar micro-morphology to cordierite.
Example 2
The embodiment provides a preparation method of a rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient, which comprises the following steps:
(1) MgO and Al with the grain diameter less than or equal to 2 mu m 2 O 3 、SiO 2 And Yb 2 O 3 The raw material powders were mixed in a molar ratio of 1.5;
(2) Putting the mixed powder A into an agate ball milling tank, adding agate milling balls, and adding absolute ethyl alcohol according to the proportion of 10-15% of solid content; sealing the ball milling tank, and putting the ball milling tank into a planetary ball mill with the rotating speed of 350 r/min for wet ball milling for 28 h to obtain ball-milled slurry;
(3) Putting the ball-milled slurry into a drying oven, drying for 20 hours at 100 ℃ in the air atmosphere, and sieving with a 300-mesh sieve to obtain mixed powder B;
(4) Putting the mixed powder B into a stainless steel mold of a tablet press, and maintaining the pressure at 200 MPa for 6 min to obtain a block raw material;
(5) Heating the block raw material in a muffle furnace, and carrying out solid phase reaction for 18h at 1400 ℃ in an air environment to obtain the rare earth-doped cordierite ceramic material with the grain size of 0.2-8 mu m and the porosity of 2%, wherein the chemical expression of the rare earth-doped cordierite ceramic material is (Mg) 1-x Yb x ) 2 Al 4 Si 5 O 18+x Wherein x =0.3.
The high temperature thermal conductivity profile of the prepared low thermal conductivity, low coefficient of thermal expansion rare earth doped cordierite ceramic material is shown in fig. 3. As can be seen from FIG. 1, the thermal conductivity of the prepared rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient is only 1.15W/(m.K) at 900 ℃, which indicates that the ceramic has the characteristic of low thermal conductivity.
Example 3
The embodiment provides a preparation method of a rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient, which comprises the following steps:
(1) MgO and Al with the grain diameter less than or equal to 2 mu m 2 O 3 、SiO 2 And Lu 2 O 3 Raw material powders were mixed in a molar ratio of 1.6;
(2) Putting the mixed powder A into an agate ball milling tank, adding agate milling balls, and adding absolute ethyl alcohol according to the proportion of 20-30% of solid content; sealing the ball milling tank, and putting the ball milling tank into a planetary ball mill with the rotating speed of 400 r/min for wet ball milling for 25 h to obtain ball-milled slurry;
(3) Placing the ball-milled slurry into a drying oven, drying for 15 hours at 110 ℃ in an air atmosphere, and then sieving with a 300-mesh sieve to obtain mixed powder B;
(4) Putting the mixed powder B into a stainless steel mold of a tablet press, and maintaining the pressure at 250 MPa for 5 min to obtain a block raw material;
(5) Heating the block raw material in a muffle furnace, and carrying out solid phase reaction for 10h at 1500 ℃ in an air environment to obtain the rare earth-doped cordierite ceramic material with the grain size of 0.2-8 mu m and the porosity of 10 percent, wherein the chemical expression of the rare earth-doped cordierite ceramic material is (Mg) 1-x Lu x ) 2 Al 4 Si 5 O 18+x Wherein x =0.1.
The thermal expansion coefficient curve of the prepared rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient is shown in figure 4. As can be seen from FIG. 4, the prepared rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient has a thermal expansion coefficient of 2.7 x 10 < -6 >/DEG C in the range of 200-1200 ℃, and has good thermal expansion matching with the SiCf/SiC ceramic matrix composite material.
The high temperature thermal conductivity profile of the prepared low thermal conductivity, low coefficient of thermal expansion rare earth doped cordierite ceramic material is shown in fig. 5. As can be seen from FIG. 5, the thermal conductivity of the prepared rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient is 1.17W/(m.K) at 900 ℃, which indicates that the ceramic has the characteristic of low thermal conductivity.
Example 4
The embodiment provides a preparation method of a rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient, which comprises the following steps:
(1) MgO and Al with the grain diameter less than or equal to 2 mu m 2 O 3 、SiO 2 And Er 2 O 3 Raw material powders were mixed in a molar ratio of 1.7;
(2) Putting the mixed powder A into an agate ball milling tank, adding agate milling balls, and adding absolute ethyl alcohol according to the proportion of 30-40% of solid content; sealing the ball milling tank, putting the ball milling tank into a planet wheel ball mill with the rotating speed of 450 revolutions/min, and performing wet ball milling for 20 hours to obtain slurry after ball milling;
(3) Putting the ball-milled slurry into a drying oven, drying for 16 h at 120 ℃ in an air atmosphere, and then sieving with a 300-mesh sieve to obtain mixed powder B;
(4) Putting the mixed powder B into a stainless steel mold of a tablet press, and maintaining the pressure at 280 MPa for 4 min to obtain a block raw material;
(5) Heating the block raw material in a muffle furnace, and performing solid phase reaction at 1300 deg.C for 15h in air environment to obtain the product with crystal grain size of 0.5-5 μm (as shown in FIG. 6), porosity of 8%, high temperature thermal conductivity of 1.23W/(m.K), and thermal expansion coefficient of 2.0 × 10 -6 The rare earth-doped cordierite ceramic material has low thermal conductivity and low thermal expansion coefficient of/K, and the chemical expression of the rare earth-doped cordierite ceramic material is (Mg) 1-x Lu x ) 2 Al 4 Si 5 O 18+x Wherein x =0.2.
Example 5
The embodiment provides a preparation method of a rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient, which comprises the following steps:
(1) MgO and Al with the grain diameter less than or equal to 2 mu m 2 O 3 、SiO 2 And Tm 2 O 3 Raw material powders were mixed in a molar ratio of 1.8;
(2) Putting the mixed powder A into an agate ball milling tank, adding agate milling balls, and adding absolute ethyl alcohol according to the proportion of 40-50% of solid content; sealing the ball milling tank, and putting the ball milling tank into a planet wheel ball mill with the rotating speed of 500 revolutions/min for wet ball milling for 18 hours to obtain ball-milled slurry;
(3) Putting the ball-milled slurry into a drying oven, drying for 15h at 130 ℃ in an air atmosphere, and then sieving with a 450-mesh sieve to obtain mixed powder B;
(4) Putting the mixed powder B into a stainless steel mold of a tablet press, and maintaining the pressure at 300 MPa for 1min to obtain a block raw material;
(5) Heating the block raw material in a muffle furnace, and carrying out solid-phase reaction at 1200 ℃ for 20h in an air environment to obtain the material with the grain size of 0.2-8 mu m, the porosity of 0%, the high-temperature thermal conductivity of 1.4W/(m.K), the thermal expansion coefficient of 2.0 multiplied by 10 -6 The rare earth-doped cordierite ceramic material has low thermal conductivity and low thermal expansion coefficient of/K, and the chemical expression of the rare earth-doped cordierite ceramic material is (Mg) 1-x Tm x ) 2 Al 4 Si 5 O 18+x Wherein x =0.
Example 6
The embodiment provides a preparation method of a rare earth doped cordierite ceramic material with low thermal conductivity and low thermal expansion coefficient, which comprises the following steps:
(1) MgO and Al with the grain diameter less than or equal to 2 mu m 2 O 3 、SiO 2 And Y 2 O 3 Raw material powders were mixed in a molar ratio of 2;
(2) Putting the mixed powder A into an agate ball milling tank, adding agate milling balls, and adding absolute ethyl alcohol according to the proportion of 50-60% of solid content; sealing the ball milling tank, and putting the ball milling tank into a planetary ball mill with the rotating speed of 600 revolutions/min for wet ball milling for 10 hours to obtain slurry after ball milling;
(3) Placing the ball-milled slurry into a drying oven, drying for 12 hours at 80 ℃ in an air atmosphere, and then sieving with a 600-mesh sieve to obtain mixed powder B;
(4) Putting the mixed powder B into a stainless steel mold of a tablet press, and maintaining the pressure at 100 MPa for 10min to obtain a block raw material;
(5) Mixing the block raw materialHeating in a muffle furnace, and carrying out solid-phase reaction at 1000 ℃ for 15h in an air environment to obtain the product with the grain size of 0.2-8 mu m, the porosity of 10%, the high-temperature thermal conductivity of 1.1W/(m.K), the thermal expansion coefficient of 3.5 multiplied by 10 -6 The rare earth-doped cordierite ceramic material has low thermal conductivity and low thermal expansion coefficient of the/K, and the chemical expression of the rare earth-doped cordierite ceramic material is (Mg) 1-x Y x ) 2 Al 4 Si 5 O 18+x Wherein x =0.1.
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 has the grain size of 0.1-10 mu m, the porosity of 0-15 percent and the thermal expansion coefficient of (2.5-4) multiplied by 10 -6 /℃。
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean 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 is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (10)
1. The rare earth-doped cordierite ceramic material is characterized in that the chemical expression of the rare earth-doped cordierite ceramic material is (Mg) 1-x RE x ) 2 Al 4 Si 5 O 18+x Wherein x is more than or equal to 0 and less than or equal to 0.5, RE is one of Y, yb, lu, tm and Er.
2. The rare earth-doped cordierite ceramic material of claim 1 having a grain size of 0.2 to 8 μm, a porosity of 0 to 10%, a high temperature thermal conductivity of not more than 1.5W/(m-K), and a coefficient of thermal expansion of (2.0 to 5.0) x 10 -6 /K。
3. A method of producing a rare earth doped cordierite ceramic material according to any of claims 1 to 2, comprising the steps of:
(1) Adding MgO and Al 2 O 3 、SiO 2 Mixing the powder and the rare earth oxide powder according to a ratio to obtain mixed powder A;
(2) Putting the mixed powder A in the step (1) into a ball milling tank, adding a ball milling medium and milling balls, and carrying out wet ball milling to obtain slurry;
(3) Drying and sieving the slurry obtained in the step (2) to obtain mixed powder B;
(4) Putting the mixed powder B in the step (3) into a tablet press to be tabletted and molded to obtain a block raw material;
(5) And (5) heating the block raw material in the step (4) in a muffle furnace to enable the block raw material to carry out solid phase reaction and generate the rare earth doped cordierite ceramic material.
4. The method of producing a rare earth-doped cordierite ceramic material of claim 3, wherein in step (1), mgO, al 2 O 3 、SiO 2 Particle size of the powder and the rare earth oxide powderLess than or equal to 2 mu m; the molar ratio of four raw materials is MgO: al (Al) 2 O 3 ：SiO 2 : rare earth oxide = (1-2): 2:5: (0.1-1).
5. The method of making a rare earth doped cordierite ceramic material of claim 4 wherein the rare earth oxide is Y 2 O 3 、Yb 2 O 3 、Lu 2 O 3 、Tm 2 O 3 And Er 2 O 3 One kind of (1).
6. The method of preparing a rare earth-doped cordierite ceramic material of claim 3, wherein the ball milling media in step (2) is deionized water or absolute ethanol; the rotation speed of the ball milling is 300-600 r/min, and the ball milling time is 10-30 h.
7. The method of producing a rare earth-doped cordierite ceramic material of claim 3, wherein the slurry in step (2) has a solid content of 10 to 60%.
8. The method for preparing a rare earth-doped cordierite ceramic material according to claim 3, wherein the drying in the step (3) is drying at 80-120 ℃ for 12-24 hours in an air atmosphere; the number of the sieved meshes is 300-600 meshes.
9. The method for preparing a rare earth-doped cordierite ceramic material according to claim 3, wherein the tablet press in the step (4) has a pressure of 100 to 300 MPa and a dwell time of 1 to 10 min.
10. The method of preparing a rare earth-doped cordierite ceramic material according to claim 3, wherein the solid phase reaction in the step (5) is carried out at 1000 to 1500 ℃ for 15 to 20 hours in an air atmosphere.
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0202107A2 (en) * | 1985-05-14 | 1986-11-20 | Ngk Insulators, Ltd. | Low expansion ceramics and method of producing the same |
| GB9003789D0 (en) * | 1989-02-25 | 1990-04-18 | Zeiss Stiftung | Process for producing dense-sintered cordierite bodies |
| JPH11130520A (en) * | 1997-10-24 | 1999-05-18 | Kyocera Corp | Low thermally expandable ceramic and its production |
| CN1358689A (en) * | 2001-12-29 | 2002-07-17 | 史志铭 | Iolite based composite ceramic material |
| WO2009070341A1 (en) * | 2007-11-30 | 2009-06-04 | Corning Incorporated | High thermal conductivity cordierite glass-ceramic materials |
| CN103025679A (en) * | 2010-10-21 | 2013-04-03 | 黑崎播磨株式会社 | Cordierite sintered body |
| US20130095994A1 (en) * | 2011-10-14 | 2013-04-18 | Asahi Glass Company, Limited | Oxide ceramics sintered compact and method of manufacturing the same |
| CN103755332A (en) * | 2013-12-30 | 2014-04-30 | 内蒙古工业大学 | Method for preparing cordierite ceramics from desert aeolian sand |
| CN103803957A (en) * | 2014-03-12 | 2014-05-21 | 哈尔滨工业大学 | Cordierite ceramic material with ultralow coefficient of thermal expansion and preparation method thereof |
| US20210094885A1 (en) * | 2019-09-30 | 2021-04-01 | Corning Incorporated | Reduced anisotropy aluminum titanate-cordierite ceramic bodies, batch mixtures including spherical alumina, and methods of manufacturing ceramic bodies therefrom |
| CN114349502A (en) * | 2022-03-21 | 2022-04-15 | 中国人民解放军国防科技大学 | Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof |
| CN115159973A (en) * | 2022-08-04 | 2022-10-11 | 中国兵器工业第五二研究所烟台分所有限责任公司 | Method for regulating and controlling thermal expansion performance of cordierite-based low-thermal expansion ceramic |
-
2022
- 2022-12-03 CN CN202211544151.4A patent/CN115974540B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0202107A2 (en) * | 1985-05-14 | 1986-11-20 | Ngk Insulators, Ltd. | Low expansion ceramics and method of producing the same |
| GB9003789D0 (en) * | 1989-02-25 | 1990-04-18 | Zeiss Stiftung | Process for producing dense-sintered cordierite bodies |
| JPH11130520A (en) * | 1997-10-24 | 1999-05-18 | Kyocera Corp | Low thermally expandable ceramic and its production |
| CN1358689A (en) * | 2001-12-29 | 2002-07-17 | 史志铭 | Iolite based composite ceramic material |
| WO2009070341A1 (en) * | 2007-11-30 | 2009-06-04 | Corning Incorporated | High thermal conductivity cordierite glass-ceramic materials |
| CN103025679A (en) * | 2010-10-21 | 2013-04-03 | 黑崎播磨株式会社 | Cordierite sintered body |
| US20130095994A1 (en) * | 2011-10-14 | 2013-04-18 | Asahi Glass Company, Limited | Oxide ceramics sintered compact and method of manufacturing the same |
| CN103755332A (en) * | 2013-12-30 | 2014-04-30 | 内蒙古工业大学 | Method for preparing cordierite ceramics from desert aeolian sand |
| CN103803957A (en) * | 2014-03-12 | 2014-05-21 | 哈尔滨工业大学 | Cordierite ceramic material with ultralow coefficient of thermal expansion and preparation method thereof |
| US20210094885A1 (en) * | 2019-09-30 | 2021-04-01 | Corning Incorporated | Reduced anisotropy aluminum titanate-cordierite ceramic bodies, batch mixtures including spherical alumina, and methods of manufacturing ceramic bodies therefrom |
| CN114349502A (en) * | 2022-03-21 | 2022-04-15 | 中国人民解放军国防科技大学 | Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof |
| CN115159973A (en) * | 2022-08-04 | 2022-10-11 | 中国兵器工业第五二研究所烟台分所有限责任公司 | Method for regulating and controlling thermal expansion performance of cordierite-based low-thermal expansion ceramic |
Non-Patent Citations (1)
| Title |
|---|
| 曹振: ""利用石英砂合成堇青石陶瓷的相变及性能"", 《中国优秀硕士学位论文全文数据库 (工程科技Ⅰ辑)》, pages 015 - 765 * |
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