CN108658606A - It can the molding silicon nitride ceramic of Fast Sintering and preparation method thereof - Google Patents
It can the molding silicon nitride ceramic of Fast Sintering and preparation method thereof Download PDFInfo
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- CN108658606A CN108658606A CN201810523050.6A CN201810523050A CN108658606A CN 108658606 A CN108658606 A CN 108658606A CN 201810523050 A CN201810523050 A CN 201810523050A CN 108658606 A CN108658606 A CN 108658606A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 128
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000000919 ceramic Substances 0.000 title claims abstract description 70
- 238000005245 sintering Methods 0.000 title claims abstract description 62
- 238000000465 moulding Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000012986 modification Methods 0.000 claims abstract description 20
- 230000004048 modification Effects 0.000 claims abstract description 20
- -1 yttrium alkoxide Chemical class 0.000 claims abstract description 19
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 18
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 17
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 15
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 15
- 229910052582 BN Inorganic materials 0.000 claims description 14
- 239000002071 nanotube Substances 0.000 claims description 13
- 239000003960 organic solvent Substances 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000701 coagulant Substances 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 229960001124 trientine Drugs 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 11
- 238000005336 cracking Methods 0.000 abstract description 10
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 16
- 239000000843 powder Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 150000004703 alkoxides Chemical class 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 235000015895 biscuits Nutrition 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical compound CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
Can the molding silicon nitride ceramic of Fast Sintering and preparation method thereof, belong to ceramic material field.Preparation method includes：10 15 parts by weight yttrium alkoxide and 58 parts by weight aluminium-alcohol salts are dissolved in 200 250 parts by weight alcoholic solvents, colloidal sol is formed.95 110 parts by weight alpha silicon nitrides and 58 parts by weight beta silicon nitrides are added into colloidal sol in stirring, is added dropwise after ammonium hydroxide adjusting pH value is 9 10 and is heated to 60 80 DEG C of 4 8h of sealing, form gel.Gel is calcined into drying, obtains the silicon nitride of surface modification.The silicon nitride of surface modification is mixed with 58 parts by weight boron nitride nano-tubes and 8 12 parts by weight silicon carbide whiskers, obtaining can the molding silicon nitride ceramic of Fast Sintering.Easy to operate, silicon nitride ceramic obtained can be used in the Fast Sintering molding of silicon nitride ceramics, and the silicon nitride ceramics that sintering obtains has the features such as bending strength is high and cracking resistance is good.
Description
Technical field
The present invention relates to ceramic material fields, and more particularly to one kind can the molding silicon nitride ceramic of Fast Sintering and its
Preparation method.
Background technology
Silicon nitride ceramics due to have many advantages, such as it is high than by force, it is Gao Bimo, high temperature resistant, anti-oxidant and wear-resistant, in high temperature, height
There is special use value in fast, strong corrosive medium working environment, thermal conductivity is good, and thermal shock resistance is strong, and dielectric
Constant and dielectric loss are low, have good frequency electromagnetic waves through performance, make it have the foreground of being widely applied.
In the prior art, the sintering period of silicon nitride ceramics is long, and be also easy to produce superheating phenomenon so as to cause stream silicon make waste product
Rate increases.Therefore, so that silicon nitride ceramics Fast Sintering is molded and the technical research for obtaining the silicon nitride ceramics of high yield rate seems
It is significant.
In view of this, special propose the application.
Invention content
The purpose of the present invention is to provide it is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, be made
Silicon nitride ceramic can be used in the Fast Sintering molding of silicon nitride ceramics, and the obtained silicon nitride ceramics of sintering has bending resistance
The features such as intensity is high and cracking resistance is good.
Another object of the present invention is to provide one kind can the molding silicon nitride ceramic of Fast Sintering, can be used in nitrogenizing
The Fast Sintering of silicon ceramics is molded, and the silicon nitride ceramics that sintering obtains has bending strength height and the good equal spies of cracking resistance
Point.
The present invention solves its technical problem using following technical scheme to realize.
The present invention propose it is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, including：
10-15 parts by weight yttrium alkoxide and 5-8 parts by weight aluminium-alcohol salts are dissolved in 200-250 parts by weight alcoholic solvents, formed
Colloidal sol；95-110 parts by weight α-siliconnitride and 5-8 parts by weight beta-silicon nitrides is added into colloidal sol in stirring, ammonium hydroxide is added dropwise and adjusts
PH value is heated to 60-80 DEG C of sealing 4-8h after being 9-10, form gel；Gel is calcined into drying, obtains the nitridation of surface modification
Silicon；The silicon nitride of surface modification is mixed with 5-8 parts by weight boron nitride nano-tube and 8-12 parts by weight silicon carbide whiskers, obtaining can
The molding silicon nitride ceramic of Fast Sintering.
The present invention propose one kind can the molding silicon nitride ceramic of Fast Sintering, be made by above-mentioned preparation method.
The advantageous effect of the embodiment of the present invention is：
It is provided by the invention can the molding silicon nitride ceramic of Fast Sintering preparation method, using α-siliconnitride and β-nitrogen
The compound system of SiClx is sintered, and carries out crystal transfer with beta-silicon nitride induction α-siliconnitride, α-siliconnitride is made to pass through dissolving-
It is precipitated and is grown on the surface of beta-silicon nitride, the consistency and intensity for being conducive to Fast Sintering, improving sintered products.Sintering aid is adopted
It is added with the form of yttrium alkoxide and aluminium-alcohol salt, forms the yttrium oxide-oxidation for being wrapped in silicon nitride surface by sol-gel technique
There is better sintering activity, crystal boundary to be easy to controlled micro crystallization for aluminum sinter auxiliary agent, the beta-silicon nitride powder that obtained surface is modified, and be suitable for fast
Fast densified sintering product is easily obtained the silicon nitride ceramics that crystallite dimension is uniform, performance is stablized.On this basis, boron nitride is introduced to receive
Mitron, silicon carbide whisker can further increase toughness, bending strength and cracking resistance of product etc..Pass through party's legal system
The silicon nitride ceramic obtained, hot pressing 30min or so can be obtained under conditions of 1700-1800 DEG C of temperature, nitrogen pressure 30MPa
The silicon nitride ceramics of compact high-strength.
It is provided by the invention can the molding silicon nitride ceramic of Fast Sintering, be made by above-mentioned preparation method, therefore phase
Ying Di, can be used in the Fast Sintering molding of silicon nitride ceramics, and the obtained silicon nitride ceramics of sintering have bending strength height with
And cracking resistance it is good the features such as.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to the embodiment of the present invention can the molding silicon nitride ceramic of Fast Sintering and preparation method thereof carry out it is specific
Explanation.
The present invention provide it is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, including：
S1,10-15 parts by weight yttrium alkoxide and 5-8 parts by weight aluminium-alcohol salts are dissolved in 200-250 parts by weight alcoholic solvents, shape
At colloidal sol.
S2,95-110 parts by weight α-siliconnitride and 5-8 parts by weight beta-silicon nitrides is added into colloidal sol in stirring, ammonia is added dropwise
Water, which is adjusted, is heated to 60-80 DEG C of sealing 4-8h after pH value is 9-10, form gel.
S3, gel is calcined into drying, obtains the silicon nitride of surface modification.
S4, the silicon nitride of surface modification and 5-8 parts by weight boron nitride nano-tube and 8-12 parts by weight silicon carbide whiskers are mixed
It closes, obtaining can the molding silicon nitride ceramic of Fast Sintering.
It in the above method, is sintered using the compound system of α-siliconnitride and beta-silicon nitride, α-is induced with beta-silicon nitride
Silicon nitride carries out crystal transfer, so that α-siliconnitride is passed through crystallization of the dissolution and precipitation and is grown on the surface of beta-silicon nitride, is conducive to quickly burn
Knot, the consistency and intensity for improving sintered products.
Further, α-siliconnitride and beta-silicon nitride use the powder of micron level.Specifically, α-siliconnitride is that purity is big
The powder for being about 0.2-0.5 μm in 99%, grain size；Beta-silicon nitride is the crystal seed that diameter is about 0.5-1 μm, draw ratio is 7-10.
Sintering aid is added in the form of yttrium alkoxide and aluminium-alcohol salt, and nitridation is wrapped in by sol-gel technique formation
The yttria-alumina sintering aid of silicon face, the beta-silicon nitride powder that obtained surface is modified has better sintering activity, brilliant
Boundary is easy to controlled micro crystallization, is suitable for that Fast Sintering is fine and close, is easily obtained the silicon nitride ceramics that crystallite dimension is uniform, performance is stablized.
Optionally, in some of the invention specific embodiments, alcoholic solvent in ethyl alcohol, propyl alcohol and butanol at least
It is a kind of.Such as the alcoholic solvent can be both individual ethyl alcohol, individual propyl alcohol, individual butanol, ethyl alcohol and propyl alcohol combination,
The combination of the combination of both combination, propyl alcohol and the butanol of both ethyl alcohol and butanol and ethyl alcohol with propyl alcohol and butanol three.
If select propyl alcohol, which is preferably selected as isopropanol.If select butanol, which is preferably selected as
N-butanol.
Further, yttrium alkoxide and aluminium-alcohol salt are optionally at least one of ethylate and propylate, such as yttrium alkoxide
Can be the combination of both individual ethylate, individual propylate and yttrium alkoxide and propylate, aluminium-alcohol salt can be independent
Ethylate, individual propylate and yttrium alkoxide and both propylates combination.
It is coagulated through inventor the study found that carrying out colloidal sol-using the alcoholic solvent cooperation of the alkoxide and mentioned kind of mentioned kind
Glue reacts, the uniformity that the yttria-alumina sintering aid of generation is wrapped up in silicon nitride surface more preferably, obtained silicon nitride
The sintering activity of powder is more preferable.
In some optional embodiments of the invention, it is added after α-siliconnitride and beta-silicon nitride and is added dropwise before ammonium hydroxide,
It further include addition 2-4 parts by weight coagulant.Coagulant is optionally trien.
Flocculant added with the gelation conducive to sol system, make the speed of gelation faster, the effect of gel it is more preferable.
The temperature of gel calcining is preferably 400-500 DEG C, to silicon nitride powder body surface while fully dry to gel
Face carries out heat treatment and generates yttria-alumina sintering aid.Temperature is too low to make dry insufficient, yttria-alumina turn
Change is not thorough, and the excessively high yttria-alumina that is easy to cause of temperature is ineffective to the package of beta-silicon nitride powder, therefore calcination temperature
It is too low or excessively high modified effect can all be adversely affected.
On this basis, boron nitride nano-tube, silicon carbide whisker are introduced, toughness, the bending resistance of product can be further increased
Intensity and cracking resistance etc..
Specifically, silicon carbide whisker is used to increase the toughness of silicon nitride ceramics, since the linear expansion coefficient of silicon carbide is long-range
In silicon nitride, in sintering process, tangential residual stress can be generated in the base, external force is made to be acted on to silicon nitride ceramics
When, inherent residual stress is first offset, achievees the purpose that stress toughening.Further, since the expansion coefficient difference of two kinds of materials,
Micro-crack can be generated in the base, can equally be played the role of offsetting external force, be achieved the purpose that microcrack evolution equation.Meanwhile it being carbonized
Silicon wafer must can be such that the crystal grain of ceramic material further refines, and so that ceramic material is preferably densified, improve its mechanical strength.
The interface cohesion of boron nitride nano-tube and silicon nitride ceramics is good, is generated in cooperation silicon carbide whisker makes matrix micro-
In the case of crackle, the stress of silicon nitride ceramics crack tip can be absorbed, effectively prevents and generates big in silicon nitride matrix
Stress concentration, when near crack propagation to silicon carbide whisker, crack tip can form strong stress shielding area, increase crackle
The resistance of extension is conducive to the intensity and cracking resistance that improve silicon nitride ceramics, keeps the modifying function of silicon carbide whisker further
Controllableization.
Optionally, the mixing of the silicon nitride with boron nitride nano-tube and silicon carbide whisker of surface modification includes：Surface is repaiied
Silicon nitride, boron nitride nano-tube and the silicon carbide whisker of decorations are scattered in organic solvent, are stirred with the rotating speed of 400-600r/min
1-2h, the content that organic solvent is then dried under conditions of 120-150 DEG C of temperature are not higher than 1wt%.
The silicon nitride of surface modification is mixed in organic solvent with boron nitride nano-tube and silicon carbide whisker, convenient for dispersion
Uniformly, it is conducive to sintering.Disperseed in the form of stirring, avoids the oxidation to the surface package of the silicon nitride of surface modification
Yttrium-alumina sintering auxiliary agent film layer causes to damage.
Further, organic solvent is selected from least one of methanol, ethyl alcohol and acetone, such as can be individual methanol,
Individual ethyl alcohol, individual acetone, methanol and ethyl alcohol combination, methanol and acetone combination, ethyl alcohol and acetone two
Combination, methanol and the ethyl alcohol of person and the combination etc. of acetone three.
Through inventor the study found that by silicon nitride ceramic made from the above method, in 1700-1800 DEG C of temperature, nitrogen
Hot pressing 30min or so can be obtained the silicon nitride ceramics of compact high-strength under conditions of atmospheric pressure 30MPa.
The present invention also provides one kind can the molding silicon nitride ceramic of Fast Sintering, be by it is above-mentioned can Fast Sintering at
The preparation method of the silicon nitride ceramic of type is made, therefore correspondingly, can be used in the Fast Sintering molding of silicon nitride ceramics, and
It is sintered obtained silicon nitride ceramics and has the features such as bending strength is high and cracking resistance is good.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
It is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, including：
S1,12kg yttriums alkoxide and 6kg aluminium-alcohol salts are dissolved in 220kg alcoholic solvents, form colloidal sol.Wherein yttrium alkoxide is second
Alkoxide, aluminium-alcohol salt are ethylate, and alcoholic solvent is absolute ethyl alcohol.
S2,105kg α-siliconnitrides and 6kg beta-silicon nitrides is added into colloidal sol in stirring, adds 3kg triens
It is uniformly mixed, ammonium hydroxide is added dropwise and adjusts pH value to be heated to 60-80 DEG C of sealing 6h after 9-10, forms gel.
S3, gel is calcined into drying under conditions of 400-500 DEG C of temperature, obtains the silicon nitride of surface modification.
S4, the silicon nitride of surface modification and 6kg boron nitride nano-tubes and 10kg silicon carbide whiskers are scattered in ethyl alcohol, with
The rotating speed of 500r/min stirs 1.5h, and the content that organic solvent is then dried under conditions of 120-150 DEG C of temperature is not higher than
1wt%, obtaining can the molding silicon nitride ceramic of Fast Sintering.
Embodiment 2
It is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, including：
S1,10kg yttriums alkoxide and 8kg aluminium-alcohol salts are dissolved in 200kg alcoholic solvents, form colloidal sol.Wherein yttrium alkoxide is second
Alkoxide, aluminium-alcohol salt are isopropoxide, and alcoholic solvent is that mass ratio is 1:1 absolute ethyl alcohol and isopropanol.
S2,95kg α-siliconnitrides and 5kg beta-silicon nitrides is added into colloidal sol in stirring, adds 2kg triens
It is uniformly mixed, ammonium hydroxide is added dropwise and adjusts pH value to be heated to 60-80 DEG C of sealing 4h after 9-10, forms gel.
S3, gel is calcined into drying under conditions of 400-500 DEG C of temperature, obtains the silicon nitride of surface modification.
S4, the silicon nitride of surface modification and 5kg boron nitride nano-tubes and 8kg silicon carbide whiskers are scattered in ethyl alcohol, with
The rotating speed of 400r/min stirs 2h, and the content that organic solvent is then dried under conditions of 120-150 DEG C of temperature is not higher than
1wt%, obtaining can the molding silicon nitride ceramic of Fast Sintering.
Embodiment 3
It is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, including：
S1,15kg yttriums alkoxide and 5kg aluminium-alcohol salts are dissolved in 250kg alcoholic solvents, form colloidal sol.Wherein yttrium alkoxide is second
Alkoxide, aluminium-alcohol salt are ethylate, and alcoholic solvent is n-butanol.
S2,110kg α-siliconnitrides and 8kg beta-silicon nitrides is added into colloidal sol in stirring, adds 4kg triens
It is uniformly mixed, ammonium hydroxide is added dropwise and adjusts pH value to be heated to 60-80 DEG C of sealing 8h after 9-10, forms gel.
S3, gel is calcined into drying under conditions of 400-500 DEG C of temperature, obtains the silicon nitride of surface modification.
S4, the silicon nitride of surface modification and 8kg boron nitride nano-tubes and 12kg silicon carbide whiskers are scattered in ethyl alcohol, with
The rotating speed of 600r/min stirs 1h, and the content that organic solvent is then dried under conditions of 120-150 DEG C of temperature is not higher than
1wt%, obtaining can the molding silicon nitride ceramic of Fast Sintering.
Embodiment 4
It is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, difference from example 1 is that：
It is not added with trien.
Embodiment 5
It is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, difference from example 1 is that：
The silicon nitride of surface modification is directly mixed with boron nitride nano-tube and silicon carbide whisker using dry powder.
Comparative example
A kind of preparation method of silicon nitride ceramic, difference from example 1 is that：Yttrium is replaced using yttrium oxide
Alkoxide, the yttrium oxide are identical as the moles total number of yttrium alkoxide.Aluminium-alcohol salt, the aluminium oxide and aluminium-alcohol salt is replaced to rub using aluminium oxide
Your total amount is identical.Sol-gel method is not used, after yttrium oxide, aluminium oxide, α-siliconnitride and beta-silicon nitride dry powder blend, is adopted
It is mixed with boron nitride nano-tube and silicon carbide whisker with the method in S4.
Test example
By silicon nitride ceramic made from embodiment 1-5 and comparative example using 220MPa pressure carry out isostatic cool pressing at
Type is suppressed, and biscuit of ceramics is obtained.By biscuit of ceramics hot pressing under conditions of 1700-1800 DEG C of temperature, nitrogen pressure 30MPa
30min obtains silicon nitride ceramics.
Performance survey is carried out to the silicon nitride ceramics that silicon nitride ceramics powder sintering obtains made from embodiment 1-5 and comparative example 1
Examination comprising：Bending strength and fracture toughness are measured using three-point bending method, measure that the results are shown in Table 1.
1 silicon nitride ceramics performance test table of table
| Project | Bending strength/(Mpa) | Fracture toughness/(MPam1/2) |
| Embodiment 1 | 1029 | 9.5 |
| Embodiment 2 | 1012 | 9.3 |
| Embodiment 3 | 1048 | 9.6 |
| Embodiment 4 | 926 | 8.7 |
| Embodiment 5 | 939 | 8.8 |
| Comparative example | 832 | 7.8 |
To sum up, it is provided by the invention can the molding silicon nitride ceramic of Fast Sintering preparation method, using α-siliconnitride
It is sintered with the compound system of beta-silicon nitride, crystal transfer is carried out with beta-silicon nitride induction α-siliconnitride, keeps α-siliconnitride logical
It crosses crystallization of the dissolution and precipitation to grow on the surface of beta-silicon nitride, the consistency and intensity for being conducive to Fast Sintering, improving sintered products.It burns
Knot auxiliary agent is added in the form of yttrium alkoxide and aluminium-alcohol salt, and the oxygen for being wrapped in silicon nitride surface is formed by sol-gel technique
Change yttrium-alumina sintering auxiliary agent, there is the beta-silicon nitride powder that obtained surface is modified better sintering activity, crystal boundary to be easy to crystallite
Change, be suitable for that Fast Sintering is fine and close, is easily obtained the silicon nitride ceramics that crystallite dimension is uniform, performance is stablized.On this basis, it introduces
Boron nitride nano-tube, silicon carbide whisker can further increase toughness, bending strength and cracking resistance of product etc..Pass through
Silicon nitride ceramic made from this method, hot pressing 30min or so under conditions of 1700-1800 DEG C of temperature, nitrogen pressure 30MPa
It can be obtained the silicon nitride ceramics of compact high-strength.
It is provided by the invention can the molding silicon nitride ceramic of Fast Sintering, be made by above-mentioned preparation method, therefore phase
Ying Di, can be used in the Fast Sintering molding of silicon nitride ceramics, and the obtained silicon nitride ceramics of sintering have bending strength height with
And cracking resistance it is good the features such as.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. it is a kind of can the molding silicon nitride ceramic of Fast Sintering preparation method, which is characterized in that including：
10-15 parts by weight yttrium alkoxide and 5-8 parts by weight aluminium-alcohol salts are dissolved in 200-250 parts by weight alcoholic solvents, colloidal sol is formed；
95-110 parts by weight α-siliconnitride and 5-8 parts by weight beta-silicon nitrides is added into the colloidal sol in stirring, ammonium hydroxide is added dropwise and adjusts
PH value is heated to 60-80 DEG C of sealing 4-8h after being 9-10, form gel；The gel is calcined into drying, obtains surface modification
Silicon nitride；The silicon nitride of the surface modification and 5-8 parts by weight boron nitride nano-tube and 8-12 parts by weight silicon carbide whiskers are mixed
It closes, obtaining can the molding silicon nitride ceramic of Fast Sintering.
2. preparation method according to claim 1, which is characterized in that the alcoholic solvent is in ethyl alcohol, propyl alcohol and butanol
At least one.
3. preparation method according to claim 2, which is characterized in that the propyl alcohol is isopropanol, and the butanol is positive fourth
Alcohol.
4. preparation method according to claim 1, which is characterized in that the yttrium alkoxide and the aluminium-alcohol salt are selected from ethyl alcohol
At least one of salt and propylate.
5. preparation method according to claim 1, which is characterized in that the calcination temperature of the gel is 400-500 DEG C.
6. preparation method according to claim 1, which is characterized in that be added after the α-siliconnitride and beta-silicon nitride and
It is added dropwise before the ammonium hydroxide, further includes addition 2-4 parts by weight coagulant.
7. preparation method according to claim 6, which is characterized in that the coagulant includes trien.
8. preparation method according to claim 1, which is characterized in that the silicon nitride of the surface modification and the boron nitride
The mixing of nanotube and the silicon carbide whisker includes：By the silicon nitride of the surface modification, the boron nitride nano-tube and institute
It states silicon carbide whisker to be scattered in organic solvent, 1-2h is stirred with the rotating speed of 400-600r/min, then in 120-150 DEG C of temperature
Under conditions of be dried to the organic solvent content be not higher than 1wt%.
9. preparation method according to claim 8, which is characterized in that the organic solvent is selected from methanol, ethyl alcohol and acetone
At least one of.
10. can the molding silicon nitride ceramic of Fast Sintering made from claim 1-9 any one of them preparation methods.
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