CN117185820A - MoAlB ceramic powder with controllable granularity and preparation method thereof - Google Patents
MoAlB ceramic powder with controllable granularity and preparation method thereof Download PDFInfo
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- CN117185820A CN117185820A CN202311194652.9A CN202311194652A CN117185820A CN 117185820 A CN117185820 A CN 117185820A CN 202311194652 A CN202311194652 A CN 202311194652A CN 117185820 A CN117185820 A CN 117185820A
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- 239000000843 powder Substances 0.000 title claims abstract description 57
- 239000000919 ceramic Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 35
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 20
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 15
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000002386 leaching Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 15
- 239000007795 chemical reaction product Substances 0.000 abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- LGLOITKZTDVGOE-UHFFFAOYSA-N boranylidynemolybdenum Chemical compound [Mo]#B LGLOITKZTDVGOE-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Abstract
The application provides a particle size-controllable MoAlB ceramic powder and a preparation method thereof, comprising the following steps: s1: mixing boron carbide and molybdenum powder according to stoichiometric ratio of chemical reaction to obtain a uniformly mixed first raw material; s2: mixing the first raw material with aluminum powder according to a preset proportion to obtain a uniformly mixed second raw material; s3: pressing the second raw material on a tablet press to obtain a raw material green body; s4: roasting the raw material green body in a high-temperature furnace under the protection of inert atmosphere; s5: and leaching, filtering, rinsing and drying the roasted product to obtain the MoAlB ceramic powder with controllable granularity. The application takes boron carbide powder, molybdenum powder and aluminum powder as raw materials, and the reaction is carried out for 2 to 8 hours at the high temperature of 1200 ℃ to 1600 ℃, and the reaction product is leached, filtered, rinsed and dried to obtain the MoAlB ceramic powder with controllable product granularity.
Description
[ field of technology ]
The application relates to the technical field of inorganic chemistry, in particular to MoAlB ceramic powder with controllable granularity and a preparation method thereof.
[ background Art ]
MoAlB is used as MAB phase (nanometer layered ternary transition metal boride, wherein M is transition metal element, A is aluminum element or zinc element, B is boron element), the unit cell structure is similar to MAX phase material, the unit cell structure is formed by interlacing transition metal MoB layer and single-layer or double-layer Al, the MoB layer is connected by strong covalent bond and ionic bond, and the Mo-Al layer is connected by weaker metal bond. The combination of the layered structure and the bond ensures that the composite material has a plurality of excellent characteristics of metal and ceramic, such as good electric conduction and conductionThermal properties, excellent self-lubricity, abrasion resistance, high fracture toughness, high damage tolerance, easy processing, and the like. In addition, dense Al can be formed due to the presence of Al 2 O 3 The protective film ensures that the MoAlB ceramic has excellent high-temperature oxidation resistance. These excellent properties make MoAlB have great application potential in the fields of heating elements, electrode materials, electrical contacts, etc.
The preparation method of the MoAlB ceramic is mainly to prepare the MoAlB ceramic by taking boron powder, molybdenum powder and aluminum powder or molybdenum boride powder and aluminum powder as raw materials and sintering the raw materials at about 1200 ℃ for 1 to 5 hours under the pressure of 30 to 60MPa through vacuum hot-pressing sintering or spark plasma sintering. MoB and Al are present in the product 3 Mo、Al 8 Mo 3 And the like, and affects the purity of the product.
Accordingly, there is a need to develop a particle size controllable MoAlB ceramic powder and a method for preparing the same to address the deficiencies of the prior art, to solve or alleviate one or more of the above-mentioned problems.
[ application ]
In view of the above, the application provides a particle-size-controllable MoAlB ceramic powder and a preparation method thereof, and particularly relates to a method for preparing the particle-size-controllable MoAlB ceramic powder by taking boron carbide powder, molybdenum powder and aluminum powder as raw materials, wherein the boron carbide powder, the molybdenum powder and the aluminum powder are reacted for 2-8 hours at a high temperature of 1200-1600 ℃, and a reaction product is leached, filtered, rinsed and dried to obtain the particle-size-controllable MoAlB ceramic powder.
In one aspect, the application provides a particle size-controllable MoAlB ceramic powder and a preparation method thereof, wherein the preparation method comprises the following steps:
s1: mixing boron carbide and molybdenum powder according to stoichiometric ratio of chemical reaction to obtain a uniformly mixed first raw material;
s2: mixing the first raw material with aluminum powder according to a preset proportion to obtain a uniformly mixed second raw material;
s3: pressing the second raw material on a tablet press to obtain a raw material green body;
s4: roasting the raw material green body obtained in the step S3 in a high-temperature furnace under the protection of inert atmosphere;
s5: and leaching, filtering, rinsing and drying the product obtained after the S4 roasting to obtain the MoAlB ceramic powder with controllable granularity.
In the aspect and any possible implementation manner described above, there is further provided an implementation manner, wherein the stoichiometric ratio of the boron carbide powder to the molybdenum powder in S1 is: 1:3-1:5.
In the aspect and any possible implementation manner as described above, there is further provided an implementation manner, wherein the preset proportion in S2 is 1-3 times of the theoretical molar ratio of the aluminum powder to the first raw material.
In the aspect and any possible implementation manner as described above, there is further provided an implementation manner, where the pressure during the sample pressing in S3 is 50-100Mpa.
In the aspect and any possible implementation manner as described above, there is further provided an implementation manner, where the baking process in S4 is: preserving heat for 2-8 hours at 1200-1600 ℃.
In aspects and any one of the possible implementations described above, there is further provided an implementation, wherein the leaching in S5 is performed with sulfuric acid or sodium hydroxide.
In the aspect and any possible implementation manner as described above, further providing an implementation manner, filtering in the step S5 is performed by using a vacuum pump for suction filtration; deionized water is adopted for rinsing; drying in a vacuum drying oven at 120 ℃ for 2 hours.
In the aspects and any possible implementation manner, there is further provided a particle size-controllable MoAlB ceramic powder, where the MoAlB ceramic powder is prepared by the preparation method.
In the aspects and any possible implementation manner described above, there is further provided an implementation manner, where the MoAlB ceramic powder is single-phase and free of other impurities.
In aspects and any possible implementation manner described above, there is further provided an implementation manner, wherein the particle size of the MoAlB ceramic powder is controllable, and the average particle size is 500nm-25 μm.
Compared with the prior art, the application can obtain the following technical effects:
(1) According to the application, boron carbide powder is used as a raw material, and compared with boron powder or molybdenum boride powder which is used as a raw material, the cost is low;
(2) The application can realize the controllable preparation of MoAlB powder with different particle diameters by adjusting the Al proportion and the reaction temperature.
Of course, it is not necessary for any of the products embodying the application to achieve all of the technical effects described above at the same time.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flow chart of a preparation method according to an embodiment of the present application.
[ detailed description ] of the application
For a better understanding of the technical solution of the present application, the following detailed description of the embodiments of the present application refers to the accompanying drawings.
It should be understood that the described embodiments are merely some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The terminology used in the embodiments of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
As shown in fig. 1, the application provides a particle size-controllable MoAlB ceramic powder and a preparation method thereof, wherein the preparation method comprises the following steps:
s1: mixing boron carbide and molybdenum powder according to stoichiometric ratio of chemical reaction to obtain a uniformly mixed first raw material;
s2: mixing the first raw material with aluminum powder according to a preset proportion to obtain a uniformly mixed second raw material;
s3: pressing the second raw material on a tablet press to obtain a raw material green body;
s4: roasting the raw material green body obtained in the step S3 in a high-temperature furnace under the protection of inert atmosphere;
s5: and leaching, filtering, rinsing and drying the product obtained after the S4 roasting to obtain the MoAlB ceramic powder with controllable granularity.
The stoichiometric ratio of the boron carbide to the molybdenum powder in the S1 is as follows: 1:3-1:5.
The preset proportion in the S2 is 1-3 times of the theoretical molar ratio of the aluminum powder to the first raw material, and the grain size of the MoAlB ceramic powder product can be regulated and controlled by adjusting the aluminum powder consumption.
The pressure in the sample pressing process in the step S3 is 50-100Mpa.
The roasting process in the step S4 is as follows: preserving heat for 2-8 hours at 1200-1600 ℃.
The leaching process in S5 adopts sulfuric acid or sodium hydroxide.
The filtering in the step S5 is carried out by adopting a vacuum pump for suction filtration; deionized water is adopted for rinsing; drying in a vacuum drying oven at 120 ℃ for 2 hours.
The application also provides the MoAlB ceramic powder with controllable granularity, which is prepared by the preparation method.
The MoAlB ceramic powder has single phase and no other impurities.
The granularity of the MoAlB ceramic powder is controllable, and the superfine MoAlB ceramic powder with the average grain diameter of about 500nm and even the ultra-coarse MoAlB ceramic powder with the average grain diameter of about 25 μm can be successfully prepared by the method.
The application relates to a preparation method of MoAlB ceramic powder with controllable granularity, which is mainly characterized in that boron powder, molybdenum powder and aluminum powder or molybdenum boride powder and aluminum powder are adopted as raw materials to be sintered by vacuum hot pressing or spark plasma sintering, and the preparation method has the problems of high preparation cost, low product purity and the like. The method uses boron carbide powder, molybdenum powder and aluminum powder as raw materials, a target product can be generated by high-temperature reaction under normal pressure and under certain conditions in argon, soluble impurities are removed from the high-temperature reaction product by leaching, and then the high-purity MoAlB ceramic powder with controllable granularity is obtained by filtering, rinsing and drying. The application relates to a novel method for synthesizing MoAlB ceramic powder with controllable granularity, which has the advantages compared with other methods that: the purity of the reaction product is high, the cost is low, and the particle size of the ceramic powder is controllable.
Embodiment one:
(1) Weighing and proportioning boron carbide powder and molybdenum powder according to the stoichiometric ratio of chemical reaction, and uniformly mixing.
(2) Uniformly mixing the mixture obtained in the step (1) with aluminum powder with the molar ratio being 1.25 times of the theoretical molar ratio.
(3) Pressing the powder obtained in (2) into a green body at a pressure of 50 MPa.
(4) And (3) placing the green body obtained in the step (3) in a crucible under the protection of argon gas, and heating and roasting at 1200 ℃ for 4 hours.
(5) And after the heat preservation is finished, cooling the reaction product to room temperature in an argon atmosphere, leaching, filtering, rinsing and drying the roasted product to obtain the superfine MoAlB ceramic powder with the average particle size of about 500 nm.
Embodiment two:
(1) Weighing and proportioning boron carbide powder and molybdenum powder according to the stoichiometric ratio of chemical reaction, and uniformly mixing.
(2) Uniformly mixing the mixture obtained in the step (1) with aluminum powder with the ratio of 1.5 times of the theoretical molar ratio.
(3) Pressing the powder obtained in (2) into a green body at a pressure of 80 MPa.
(4) And (3) placing the green body obtained in the step (3) in a crucible under the protection of argon gas, and heating and roasting at 1300 ℃ for 5 hours.
(5) And after the heat preservation is finished, cooling the reaction product to room temperature in an argon atmosphere, leaching, filtering, rinsing and drying the roasted product to obtain the ultra-coarse MoAlB ceramic powder with the average particle size of about 10 mu m.
Embodiment III:
(1) Weighing and proportioning boron carbide powder and molybdenum powder according to the stoichiometric ratio of chemical reaction, and uniformly mixing.
(2) And (3) uniformly mixing the mixture obtained in the step (1) with aluminum powder with the molar ratio being 2 times of that of the theoretical molar ratio.
(3) Pressing the powder obtained in (2) into a green body at a pressure of 100MPa.
(4) And (3) placing the green body obtained in the step (3) in a crucible under the protection of argon gas, and heating and roasting at 1500 ℃ for 8 hours.
(5) And after the heat preservation is finished, cooling the reaction product to room temperature in an argon atmosphere, leaching, filtering, rinsing and drying the roasted product to obtain the ultra-coarse MoAlB ceramic powder with the average particle size of about 25 mu m.
The MoAlB ceramic powder with controllable granularity and the preparation method thereof provided by the embodiment of the application are described in detail. The above description of embodiments is only for aiding in the understanding of the method of the present application and its core ideas; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present application, the present description should not be construed as limiting the present application in view of the above.
Certain terms are used throughout the description and claims to refer to particular components. Those of skill in the art will appreciate that a hardware manufacturer may refer to the same component by different names. The description and claims do not take the form of an element differentiated by name, but rather by functionality. As referred to throughout the specification and claims, the terms "comprising," including, "and" includes "are intended to be interpreted as" including/comprising, but not limited to. By "substantially" is meant that within an acceptable error range, a person skilled in the art is able to solve the technical problem within a certain error range, substantially achieving the technical effect. The description hereinafter sets forth a preferred embodiment for practicing the application, but is not intended to limit the scope of the application, as the description is given for the purpose of illustrating the general principles of the application. The scope of the application is defined by the appended claims.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a product or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such product or system. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a commodity or system comprising such elements.
It should be understood that the term "and/or" as used herein is merely one relationship describing the association of the associated objects, meaning that there may be three relationships, e.g., a and/or B, may represent: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
While the foregoing description illustrates and describes the preferred embodiments of the present application, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as limited to other embodiments, and is capable of numerous other combinations, modifications and environments and is capable of changes or modifications within the scope of the inventive concept as expressed herein, either as a result of the foregoing teachings or as a result of the knowledge or technology of the relevant art. And that modifications and variations which do not depart from the spirit and scope of the application are intended to be within the scope of the appended claims.
Claims (10)
1. The preparation method of the MoAlB ceramic powder with controllable granularity is characterized by comprising the following steps of:
s1: mixing boron carbide and molybdenum powder according to stoichiometric ratio of chemical reaction to obtain a uniformly mixed first raw material;
s2: mixing the first raw material with aluminum powder according to a preset proportion to obtain a uniformly mixed second raw material;
s3: pressing the second raw material on a tablet press to obtain a raw material green body;
s4: roasting the raw material green body obtained in the step S3 in a high-temperature furnace under the protection of inert atmosphere;
s5: and leaching, filtering, rinsing and drying the product obtained after the S4 roasting to obtain the MoAlB ceramic powder with controllable granularity.
2. The preparation method according to claim 1, wherein the stoichiometric ratio of the boron carbide powder to the molybdenum powder in the S1 is 1:3-1:5.
3. The preparation method according to claim 1, wherein the preset proportion in S2 is 1 to 3 times the theoretical molar ratio of the aluminum powder to the first raw material.
4. The method according to claim 1, wherein the pressure in the sample pressing process in step S3 is 50-100Mpa.
5. The method according to claim 1, wherein the baking process in S4 is: preserving heat for 2-8 hours at 1200-1600 ℃.
6. The method according to claim 1, wherein the leaching in S5 is performed with sulfuric acid or sodium hydroxide.
7. The method according to claim 1, wherein the filtering in S5 is performed by vacuum pump; deionized water is adopted for rinsing; drying in a vacuum drying oven at 120 ℃ for 2 hours.
8. A particle size controllable MoAlB ceramic powder, characterized in that the MoAlB ceramic powder is prepared by the preparation method according to any one of claims 1-7.
9. The MoAlB ceramic powder of claim 8, wherein the MoAlB ceramic powder is single phase and free of other impurities.
10. The MoAlB ceramic powder of claim 8, wherein the particle size of the MoAlB ceramic powder is controllable and the average particle size is 500nm-25 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311194652.9A CN117185820A (en) | 2023-09-15 | 2023-09-15 | MoAlB ceramic powder with controllable granularity and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311194652.9A CN117185820A (en) | 2023-09-15 | 2023-09-15 | MoAlB ceramic powder with controllable granularity and preparation method thereof |
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| Publication Number | Publication Date |
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| CN117185820A true CN117185820A (en) | 2023-12-08 |
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| CN202311194652.9A Pending CN117185820A (en) | 2023-09-15 | 2023-09-15 | MoAlB ceramic powder with controllable granularity and preparation method thereof |
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| Country | Link |
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