CN108658606B - Silicon nitride ceramic powder capable of being rapidly sintered and formed and preparation method thereof - Google Patents
Silicon nitride ceramic powder capable of being rapidly sintered and formed and preparation method thereof Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 112
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000000919 ceramic Substances 0.000 title claims abstract description 64
- 239000000843 powder Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- -1 yttrium alkoxide Chemical class 0.000 claims abstract description 35
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 18
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 10
- HHFAWKCIHAUFRX-UHFFFAOYSA-N ethoxide Chemical compound CC[O-] HHFAWKCIHAUFRX-UHFFFAOYSA-N 0.000 claims description 9
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- IKNCGYCHMGNBCP-UHFFFAOYSA-N propan-1-olate Chemical compound CCC[O-] IKNCGYCHMGNBCP-UHFFFAOYSA-N 0.000 claims description 6
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 5
- 239000002071 nanotube Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000701 coagulant Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000005245 sintering Methods 0.000 description 28
- 235000019441 ethanol Nutrition 0.000 description 22
- 238000005452 bending Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- MEWCPXSDLIWQER-UHFFFAOYSA-N aluminum oxygen(2-) yttrium(3+) Chemical compound [O-2].[Y+3].[O-2].[Al+3] MEWCPXSDLIWQER-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 230000001476 alcoholic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical group CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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Abstract
The preparation method comprises the steps of dissolving 10-15 parts by weight of yttrium alkoxide and 5-8 parts by weight of aluminum alkoxide in 250 parts by weight of an alcohol solvent 200-250 parts by weight to form a sol, adding 95-110 parts by weight of α -silicon nitride and 5-8 parts by weight of β -silicon nitride into the sol while stirring, dropwise adding ammonia water to adjust the pH value to 9-10, heating to 60-80 ℃, sealing for 4-8 hours to form a gel, calcining and drying the gel to obtain surface-modified silicon nitride, mixing the surface-modified silicon nitride with 5-8 parts by weight of boron nitride nanotubes and 8-12 parts by weight of silicon carbide whiskers to obtain the silicon nitride ceramic powder capable of being rapidly sintered and molded.
Description
Technical Field
The invention relates to the field of ceramic materials, and in particular relates to silicon nitride ceramic powder capable of being rapidly sintered and formed and a preparation method thereof.
Background
The silicon nitride ceramic has the advantages of high specific strength, high specific modulus, high temperature resistance, oxidation resistance, wear resistance and the like, has special use value in the working environment of high-temperature, high-speed and strong corrosive media, has good thermal conductivity and strong thermal shock resistance, and has low dielectric constant and dielectric loss, good high-frequency electromagnetic wave transmission performance and wide application prospect.
In the prior art, the sintering period of silicon nitride ceramics is long, and overheating phenomenon is easy to generate, so that the silicon flow is caused, and the rejection rate is increased. Therefore, the technical research of rapidly sintering and molding the silicon nitride ceramics and obtaining the silicon nitride ceramics with high yield is significant.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to provide a preparation method of silicon nitride ceramic powder capable of being rapidly sintered and formed, the prepared silicon nitride ceramic powder can be used for rapidly sintering and forming silicon nitride ceramic, and the sintered silicon nitride ceramic has the characteristics of high bending strength, good crack resistance and the like.
The other purpose of the invention is to provide a silicon nitride ceramic powder capable of being rapidly sintered and formed, which can be used for rapidly sintering and forming silicon nitride ceramic, and the silicon nitride ceramic obtained by sintering has the characteristics of high bending strength, good crack resistance and the like.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of silicon nitride ceramic powder capable of being rapidly sintered and formed, which comprises the following steps:
dissolving 10-15 parts by weight of yttrium alkoxide and 5-8 parts by weight of aluminum alkoxide in 250 parts by weight of 200-one alcohol solvent to form sol, adding 95-110 parts by weight of α -silicon nitride and 5-8 parts by weight of β -silicon nitride into the sol while stirring, dropwise adding ammonia water to adjust the pH value to 9-10, heating to 60-80 ℃, sealing for 4-8h to form gel, calcining and drying the gel to obtain surface-modified silicon nitride, and mixing the surface-modified silicon nitride with 5-8 parts by weight of boron nitride nanotubes and 8-12 parts by weight of silicon carbide whiskers to obtain the silicon nitride ceramic powder capable of being rapidly sintered and molded.
The invention provides silicon nitride ceramic powder capable of being rapidly sintered and formed, which is prepared by the preparation method.
The embodiment of the invention has the beneficial effects that:
the invention provides a preparation method of silicon nitride ceramic powder capable of being rapidly sintered and formed, which is characterized in that a composite system of α -silicon nitride and β -silicon nitride is adopted for sintering, β -silicon nitride is used for inducing α -silicon nitride to carry out crystal form transformation, so that α -silicon nitride grows on the surface of β -silicon nitride through dissolution and precipitation, the rapid sintering is facilitated, and the density and the strength of a sintered product are improved.
The silicon nitride ceramic powder capable of being rapidly sintered and formed is prepared by the preparation method, so that the silicon nitride ceramic powder can be correspondingly used for rapidly sintering and forming silicon nitride ceramic, and the silicon nitride ceramic obtained by sintering has the characteristics of high bending strength, good crack resistance and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The silicon nitride ceramic powder capable of being rapidly sintered and formed and the preparation method thereof according to the embodiment of the present invention will be specifically described below.
The invention provides a preparation method of silicon nitride ceramic powder capable of being rapidly sintered and formed, which comprises the following steps:
s1, dissolving 10-15 parts by weight of yttrium alkoxide and 5-8 parts by weight of aluminum alkoxide in 200-250 parts by weight of alcohol solvent to form sol.
S2, adding 95-110 parts by weight of α -silicon nitride and 5-8 parts by weight of β -silicon nitride into the sol while stirring, dropwise adding ammonia water to adjust the pH value to 9-10, heating to 60-80 ℃, sealing for 4-8h, and forming gel.
And S3, calcining and drying the gel to obtain the surface-modified silicon nitride.
And S4, mixing the surface-modified silicon nitride with 5-8 parts by weight of boron nitride nanotubes and 8-12 parts by weight of silicon carbide whiskers to obtain the silicon nitride ceramic powder capable of being rapidly sintered and molded.
In the method, a composite system of α -silicon nitride and β -silicon nitride is adopted for sintering, and β -silicon nitride is used for inducing α -silicon nitride to perform crystal form transformation, so that α -silicon nitride grows on the surface of β -silicon nitride through dissolution and precipitation, and the method is favorable for rapid sintering and improves the density and strength of a sintered product.
Furthermore, α -silicon nitride and β -silicon nitride are micron-level powder, specifically, α -silicon nitride is powder with purity more than 99% and particle size of about 0.2-0.5 μm, and β -silicon nitride is seed crystal with diameter of about 0.5-1 μm and length-diameter ratio of 7-10.
The sintering aid is added in the form of yttrium alkoxide and aluminum alkoxide, and the yttrium oxide-aluminum oxide sintering aid coated on the surface of the silicon nitride is formed by a sol-gel technology, so that the obtained surface-modified silicon nitride powder has better sintering activity, the crystal boundary is easy to be microcrystalline, the silicon nitride powder is suitable for rapid sintering and compact, and the silicon nitride ceramic with uniform grain size and stable performance is easy to obtain.
Alternatively, in some specific embodiments of the present invention, the alcoholic solvent is selected from at least one of ethanol, propanol and butanol. For example, the alcoholic solvent can be ethanol alone, propanol alone, butanol alone, a combination of both ethanol and propanol, a combination of both ethanol and butanol, a combination of both propanol and butanol, and a combination of ethanol with three of propanol and butanol.
If propanol is selected, it is preferably selected to be isopropanol. If butanol is selected, it is preferably selected to be n-butanol.
Further, the yttrium alkoxide and the aluminum alkoxide are optionally at least one of an ethoxide and a propoxide, for example the yttrium alkoxide can be an ethoxide alone, a propoxide alone, and a combination of both the yttrium alkoxide and the propoxide, and the aluminum alkoxide can be an ethoxide alone, a propoxide alone, and a combination of both the yttrium alkoxide and the propoxide.
The inventor researches and discovers that the generated yttrium oxide-aluminum oxide sintering aid has better coating uniformity on the surface of silicon nitride and the obtained silicon nitride powder has better sintering activity by adopting the alkoxide of the type and the alcohol solvent of the type to carry out sol-gel reaction.
In some alternative embodiments of the invention, after the addition of α -silicon nitride and β -silicon nitride and before the addition of the ammonia, there is also included the addition of 2 to 4 parts by weight of a coagulant.
The addition of the flocculating agent is beneficial to the gelation of a sol system, so that the gelation speed is higher and the gelation effect is better.
The gel calcination temperature is preferably 400-500 ℃, and the yttrium oxide-aluminum oxide sintering aid is generated by performing heat treatment on the silicon nitride powder surface while fully drying the gel. Too low temperature causes insufficient drying and incomplete conversion of yttrium oxide-aluminum oxide, and too high temperature easily causes poor wrapping effect of yttrium oxide-aluminum oxide on silicon nitride powder, so that too low or too high calcination temperature can cause adverse effect on modification effect.
On the basis, the introduction of the boron nitride nanotube and the silicon carbide whisker can further improve the toughness, the bending strength, the crack resistance and the like of the product.
Specifically, the silicon carbide whisker is used for increasing the toughness of the silicon nitride ceramic, and because the linear expansion coefficient of the silicon carbide is far greater than that of the silicon nitride, tangential residual stress can be generated in a matrix in the sintering process, so that when external force acts on the silicon nitride ceramic, the internal residual stress needs to be counteracted first, and the purpose of stress toughening is achieved. In addition, due to the difference of the expansion coefficients of the two materials, microcracks can be generated in the matrix, the effect of counteracting external force can be also achieved, and the aim of toughening the microcracks is fulfilled. Meanwhile, the silicon carbide whisker can further refine grains of the ceramic material, so that the ceramic material is better densified, and the mechanical strength of the ceramic material is improved.
The interface of the boron nitride nanotube and the silicon nitride ceramic is well combined, and under the condition that the silicon carbide whisker is matched to generate micro-cracks in a matrix, the stress at the tip of the silicon nitride ceramic crack can be absorbed, so that the generation of large stress concentration in the silicon nitride matrix is effectively prevented, when the crack is expanded to be close to the silicon carbide whisker, a strong stress shielding area can be formed at the tip of the crack, the resistance of crack expansion is increased, the strength and the crack resistance of the silicon nitride ceramic are favorably improved, and the modification effect of the silicon carbide whisker is further controllable.
Optionally, the mixing of the surface-modified silicon nitride with the boron nitride nanotubes and the silicon carbide whiskers comprises: dispersing the surface-modified silicon nitride, boron nitride nanotubes and silicon carbide whiskers in an organic solvent, stirring at the rotation speed of 400-600r/min for 1-2h, and drying at the temperature of 120-150 ℃ until the content of the organic solvent is not higher than 1 wt%.
The surface-modified silicon nitride, the boron nitride nanotube and the silicon carbide whisker are mixed in an organic solvent, so that the uniform dispersion is facilitated, and the sintering is facilitated. The dispersion is carried out in a stirring mode, so that the damage to the yttrium oxide-aluminum oxide sintering aid film layer coated on the surface of the surface-modified silicon nitride is avoided.
Further, the organic solvent is selected from at least one of methanol, ethanol and acetone, such as methanol alone, ethanol alone, acetone alone, a combination of both methanol and ethanol, a combination of both methanol and acetone, a combination of both ethanol and acetone, a combination of three of methanol, ethanol and acetone, and the like.
The research of the inventor finds that the silicon nitride ceramic powder prepared by the method can be hot-pressed for about 30min under the conditions of the temperature of 1700-1800 ℃ and the nitrogen pressure of 30MPa to obtain the compact and high-strength silicon nitride ceramic.
The invention also provides silicon nitride ceramic powder capable of being rapidly sintered and formed, which is prepared by the preparation method of the silicon nitride ceramic powder capable of being rapidly sintered and formed, so that the silicon nitride ceramic powder can be correspondingly used for rapidly sintering and forming silicon nitride ceramic, and the silicon nitride ceramic obtained by sintering has the characteristics of high bending strength, good crack resistance and the like.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
A preparation method of silicon nitride ceramic powder capable of being rapidly sintered and formed comprises the following steps:
s1, dissolving 12kg of yttrium alkoxide and 6kg of aluminum alkoxide in 220kg of alcohol solvent to form sol. Wherein the yttrium alkoxide is ethoxide, the aluminum alkoxide is ethoxide, and the alcohol solvent is absolute ethyl alcohol.
S2, adding 105kg of α -silicon nitride and 6kg of β -silicon nitride into the sol while stirring, adding 3kg of triethylenetetramine, uniformly mixing, dropwise adding ammonia water to adjust the pH value to 9-10, heating to 60-80 ℃, sealing for 6h, and forming gel.
S3, calcining and drying the gel at the temperature of 400-500 ℃ to obtain the surface modified silicon nitride.
S4, dispersing the surface-modified silicon nitride, 6kg of boron nitride nanotubes and 10kg of silicon carbide whiskers in ethanol, stirring at the rotating speed of 500r/min for 1.5h, and drying at the temperature of 120-150 ℃ until the content of the organic solvent is not higher than 1wt%, thereby obtaining the silicon nitride ceramic powder capable of being rapidly sintered and molded.
Example 2
A preparation method of silicon nitride ceramic powder capable of being rapidly sintered and formed comprises the following steps:
s1, dissolving 10kg of yttrium alkoxide and 8kg of aluminum alkoxide in 200kg of alcohol solvent to form sol. Wherein the yttrium alkoxide is ethoxide, the aluminum alkoxide is isopropoxide, and the alcohol solvent is absolute ethanol and isopropanol with the mass ratio of 1: 1.
S2, adding 95kg of α -silicon nitride and 5kg of β -silicon nitride into the sol while stirring, adding 2kg of triethylenetetramine, uniformly mixing, dropwise adding ammonia water to adjust the pH value to 9-10, heating to 60-80 ℃, sealing for 4 hours, and forming gel.
S3, calcining and drying the gel at the temperature of 400-500 ℃ to obtain the surface modified silicon nitride.
S4, dispersing the surface-modified silicon nitride, 5kg of boron nitride nanotubes and 8kg of silicon carbide whiskers in ethanol, stirring at a rotating speed of 400r/min for 2h, and then drying at the temperature of 120-150 ℃ until the content of the organic solvent is not higher than 1wt%, thereby obtaining the silicon nitride ceramic powder capable of being rapidly sintered and molded.
Example 3
A preparation method of silicon nitride ceramic powder capable of being rapidly sintered and formed comprises the following steps:
s1, dissolving 15kg of yttrium alkoxide and 5kg of aluminum alkoxide in 250kg of alcohol solvent to form sol. Wherein the yttrium alkoxide is ethoxide, the aluminum alkoxide is ethoxide, and the alcohol solvent is n-butanol.
S2, adding 110kg of α -silicon nitride and 8kg of β -silicon nitride into the sol while stirring, adding 4kg of triethylenetetramine, uniformly mixing, dropwise adding ammonia water to adjust the pH value to 9-10, heating to 60-80 ℃, sealing for 8 hours, and forming gel.
S3, calcining and drying the gel at the temperature of 400-500 ℃ to obtain the surface modified silicon nitride.
S4, dispersing the surface-modified silicon nitride, 8kg of boron nitride nanotubes and 12kg of silicon carbide whiskers in ethanol, stirring at a rotating speed of 600r/min for 1h, and drying at the temperature of 120-150 ℃ until the content of the organic solvent is not higher than 1wt%, thereby obtaining the silicon nitride ceramic powder capable of being rapidly sintered and molded.
Example 4
The preparation method of the silicon nitride ceramic powder capable of being rapidly sintered and formed is different from the preparation method of the silicon nitride ceramic powder in the embodiment 1 in that: triethylenetetramine was not added.
Example 5
The preparation method of the silicon nitride ceramic powder capable of being rapidly sintered and formed is different from the preparation method of the silicon nitride ceramic powder in the embodiment 1 in that: the surface modified silicon nitride is directly mixed with the boron nitride nanotube and the silicon carbide whisker by adopting dry powder.
Comparative example
A silicon nitride ceramic powder was prepared in the same manner as in example 1 except that yttrium oxide was used in place of yttrium alkoxide, and the total molar amount of yttrium oxide and yttrium alkoxide was the same, aluminum oxide was used in place of aluminum alkoxide, and the total molar amount of aluminum oxide and aluminum alkoxide was the same.A dry powder of yttrium oxide, aluminum oxide, α -silicon nitride and β -silicon nitride was mixed without sol-gel method, and then mixed with boron nitride nanotubes and silicon carbide whiskers by the method in S4.
Test examples
The silicon nitride ceramic powders obtained in examples 1 to 5 and comparative example were subjected to cold isostatic pressing at a pressure of 220MPa to obtain ceramic green bodies. Hot-pressing the ceramic biscuit for 30min at the temperature of 1700-1800 ℃ and the nitrogen pressure of 30MPa to obtain the silicon nitride ceramic.
The silicon nitride ceramics obtained by sintering the silicon nitride ceramic powders obtained in examples 1 to 5 and comparative example 1 were subjected to a performance test, which included: bending strength and fracture toughness were measured by three-point bending, and the measured results are shown in Table 1.
TABLE 1 silicon nitride ceramics Performance test Table
| Item | Bending strength/(Mpa) | Fracture toughness/(MPa. m)1/2) |
| Example 1 | 1029 | 9.5 |
| Example 2 | 1012 | 9.3 |
| Example 3 | 1048 | 9.6 |
| Example 4 | 926 | 8.7 |
| Example 5 | 939 | 8.8 |
| Comparative example | 832 | 7.8 |
In summary, the preparation method of the silicon nitride ceramic powder capable of being rapidly sintered and formed provided by the invention adopts a composite system of α -silicon nitride and β -silicon nitride for sintering, and β -silicon nitride induces α -silicon nitride to perform crystal form transformation, so that α -silicon nitride grows on the surface of β -silicon nitride through dissolution and precipitation, which is beneficial to rapid sintering and improves the density and strength of a sintered product.
The silicon nitride ceramic powder capable of being rapidly sintered and formed is prepared by the preparation method, so that the silicon nitride ceramic powder can be correspondingly used for rapidly sintering and forming silicon nitride ceramic, and the silicon nitride ceramic obtained by sintering has the characteristics of high bending strength, good crack resistance and the like.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (8)
1. A preparation method of silicon nitride ceramic powder capable of being rapidly sintered and formed is characterized by comprising the following steps:
dissolving 10-15 parts by weight of yttrium alkoxide and 5-8 parts by weight of aluminum alkoxide in 250 parts by weight of 200-one-phase alcohol solvent to form sol, adding 95-110 parts by weight of α -silicon nitride and 5-8 parts by weight of β -silicon nitride into the sol while stirring, dropwise adding ammonia water to adjust the pH value to 9-10, heating to 60-80 ℃, sealing for 4-8h to form gel, calcining and drying the gel to obtain surface-modified silicon nitride, mixing the surface-modified silicon nitride with 5-8 parts by weight of boron nitride nanotubes and 8-12 parts by weight of silicon carbide whiskers to obtain silicon nitride ceramic powder capable of being rapidly sintered and molded;
wherein the mixing of the surface-modified silicon nitride with the boron nitride nanotubes and the silicon carbide whiskers comprises: dispersing the surface-modified silicon nitride, the boron nitride nanotube and the silicon carbide whisker in an organic solvent, stirring at the rotating speed of 400-600r/min for 1-2h, and then drying at the temperature of 120-150 ℃ until the content of the organic solvent is not higher than 1 wt%.
2. The method according to claim 1, wherein the alcohol solvent is at least one selected from the group consisting of ethanol, propanol and butanol.
3. The method according to claim 2, wherein the propanol is isopropanol and the butanol is n-butanol.
4. The production method according to claim 1, wherein each of the yttrium alkoxide and the aluminum alkoxide is selected from at least one of an ethoxide and a propoxide.
5. The method as claimed in claim 1, wherein the gel is calcined at a temperature of 400-500 ℃.
6. The method of claim 1, further comprising adding 2 to 4 parts by weight of a coagulant after the α -silicon nitride and β -silicon nitride are added and before the ammonia is added dropwise.
7. The method of claim 6, wherein the coagulant comprises triethylenetetramine.
8. The production method according to claim 1, wherein the organic solvent is at least one selected from the group consisting of methanol, ethanol, and acetone.
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| CN101555156A (en) * | 2009-05-15 | 2009-10-14 | 山东大学 | Boron nitride crystal whisker/silicon nitride ceramic composite material and preparation method thereof |
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| CN101555156A (en) * | 2009-05-15 | 2009-10-14 | 山东大学 | Boron nitride crystal whisker/silicon nitride ceramic composite material and preparation method thereof |
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