CN108383532A - A kind of dense silicon nitride ceramic material and preparation method thereof - Google Patents
A kind of dense silicon nitride ceramic material and preparation method thereof Download PDFInfo
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Abstract
A kind of dense silicon nitride ceramics and preparation method thereof, are related to ceramic material field, use alpha silicon nitride powder that a small amount of sintering aid is coordinated to be sintered, and the transformation of crystal of alpha silicon nitride powder are induced with beta silicon nitride crystal seed, to increase product density.Meanwhile the form of three-stage sintering, one-stage sintering carry out under compared with low pressure and lower temperature, allow auxiliary agent to form liquid phase, and be uniformly distributed in alpha silicon nitride powder；Bis sintering improves temperature on the basis of one-stage sintering, allows alpha silicon nitride powder body that can mutually become β phases from α phases, while being grown in beta silicon nitride seed surface by solution modeling, and the stomata on biscuit surface is closed；Finally increase air pressure on the basis of bis sintering, biscuit is made further to be densified, obtains silicon nitride ceramics.The dense silicon nitride ceramics being prepared by the above method, density have the characteristics that high intensity, high tenacity, wear resistant corrosion resistant close to the theoretical density of silicon nitride.
Description
Technical field
The present invention relates to ceramic material fields, in particular to a kind of dense silicon nitride ceramic material and its preparation
Method.
Background technology
Silicon nitride ceramics is a kind of structural ceramics haveing excellent performance, and all has high intensity at various temperatures and resists
Toughness is destroyed, while it also has higher thermal stability, hardness, wearability, inoxidizability, corrosion resistance etc., is a kind of pole
Potential structural ceramics is widely used in some high-grade, precision and advanced fields.
The existing method for preparing silicon nitride ceramics includes pressure sintering, hot isostatic pressing method, gas pressure sintering method etc., due to different works
The porosity that skill generates is different, and the silicon nitride ceramics density prepared is irregular, can generally be reached for the 80% of theoretical density
More than.But as people are higher and higher to the performance requirement of structural ceramics, the silicon nitride ceramics of these low-density has been difficult to completely
The demand of sufficient people, develop a kind of dense silicon nitride ceramics and preparation method thereof very it is necessary to.
Invention content
It is simple to operate the purpose of the present invention is to provide a kind of preparation method of dense silicon nitride ceramics, energy
The silicon nitride ceramics of enough efficiently production high compactions.
Another object of the present invention is to provide a kind of dense silicon nitride ceramics, the theory of density close to silicon nitride is close
Degree, has the characteristics that high intensity, high tenacity, wear resistant corrosion resistant.
What the embodiment of the present invention was realized in：
A kind of preparation method of dense silicon nitride ceramic material comprising：
By the α-siliconnitride powder of 100~120 parts by weight, the metal oxides of 0.5~2 parts by weight, 1~5 parts by weight
Rare earth oxide and the beta-silicon nitride crystal seed of 7~10 parts by weight uniformly mix, and are pressed into biscuit；
Biscuit is subjected to one-stage sintering at 0.1~0.3Mpa of nitrogen pressure, 1300~1500 DEG C of temperature；Then in nitrogen
0.1~0.3Mpa of pressure carries out bis sintering at 1600~1800 DEG C of temperature；Finally in 1.5~2Mpa of nitrogen pressure, temperature
Three-stage sintering is carried out at 1800~2000 DEG C.
A kind of dense silicon nitride ceramic material is prepared by the preparation method of above-mentioned dense silicon nitride ceramic material
It arrives.
The advantageous effect of the embodiment of the present invention is：
An embodiment of the present invention provides a kind of dense silicon nitride ceramics and preparation method thereof, use α-siliconnitride powder
Coordinate a small amount of sintering aid to be sintered, the transformation of crystal of α-siliconnitride powder is induced with beta-silicon nitride crystal seed, to increase production
Product density.Meanwhile the form of three-stage sintering, one-stage sintering carry out under compared with low pressure and lower temperature, and auxiliary agent is allowed to form liquid
Phase, and be uniformly distributed in α-siliconnitride powder；Bis sintering improves temperature on the basis of one-stage sintering, allows α-siliconnitride
Powder can mutually be become β phases from α phases, while be grown in beta-silicon nitride seed surface by solution modeling, and by biscuit surface
Stomata is closed；Finally increase air pressure on the basis of bis sintering, biscuit is made further to be densified, obtains silicon nitride ceramics.It is logical
The dense silicon nitride ceramics that the above method is prepared are crossed, density has high intensity, height close to the theoretical density of silicon nitride
The characteristics of toughness, wear resistant corrosion resistant.
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.
A kind of dense silicon nitride ceramics of the embodiment of the present invention and preparation method thereof are specifically described below.
An embodiment of the present invention provides a kind of preparation methods of dense silicon nitride ceramic material comprising：
S1. by the α-siliconnitride powder of 100~120 parts by weight, the metal oxide of 0.5~2 parts by weight, 1~5 parts by weight
Rare earth oxide and the beta-silicon nitride crystal seeds of 7~10 parts by weight uniformly mix, and be pressed into biscuit.
Inventor is based on α-siliconnitride powder, the auxiliary agents such as complexed metal oxide, rare earth oxide, and by above-mentioned
The rational proportion of substance prepares silicon nitride ceramics.Metal oxide includes in aluminium oxide, magnesia, zirconium oxide and titanium oxide
It is at least one.Rare earth oxide includes at least one of yttrium oxide, lanthana, cerium oxide or luteium oxide.It is metal oxide, dilute
The auxiliary agents such as native oxide form liquid phase in sintering process, if having enough liquid phases at this time and liquid phase viscosity is smaller, will occur
Silicon nitride particle phase transformation and rearrangement, and reach closelypacked effect by resetting.It is worth noting that, the content of auxiliary agent is unsuitable
Excessively high, liquid phase component is mostly present in the grain boundaries of silicon nitride ceramics with glassy state after the cooling period, can be direct if glassy state is excessive
Influence the mechanical property of silicon nitride ceramics.Meanwhile the content of auxiliary agent is also unsuitable too low, otherwise can lead to the process of densification too
Slowly, production efficiency is seriously affected.
α-siliconnitride powder compared to beta-silicon nitride raw material for, have cheap and easily-available advantage, be produced into conducive to reduction
This.Wherein, the purity of α-siliconnitride powder is more than 99%, α phase contents and is more than 95wt%, and grain size is 0.2~0.5 μm.Usual feelings
Under condition, the grain size of α-siliconnitride powder is smaller, the easier consistency for improving silicon nitride ceramics, but when the grain of α-siliconnitride powder
When diameter is too small, these fine particles are easy to agglomerate into bulky grain, and these bulky grains be easy to cause sample in sintering process
There is micropore and crackle in inside, influences the consistency and properties of product instead.The present application is paying a large amount of creation
Property labour after find, when the grain size of α-siliconnitride powder be 0.2~0.5 μm when, the consistency of obtained silicon nitride ceramics is higher,
Properties are more excellent.
Beta-silicon nitride crystal seed can play the role of induction crystallization, enable the silicon nitride preferably phase transformation of α phases, and in β-
The surface growth for nitrogenizing silicon seed, forms the silicon nitride of the β phases of long column shape.Further, β-nitrogen that the embodiment of the present application uses
A diameter of 0.5~1 μm of SiClx crystal seed, draw ratio are 7~10.Inventor has found that use is above-mentioned by a large amount of creative works
The densification degree of the silicon nitride ceramics that the beta-silicon nitride crystal seed of size obtains, intensity and toughness are higher.
Further, to the mixing of α-siliconnitride powder, metal oxide, rare earth oxide and beta-silicon nitride crystal seed, it is
α-siliconnitride powder, metal oxide, rare earth oxide and beta-silicon nitride crystal seed are scattered in organic solvent and carry out ball milling.Its
In, organic solvent includes at least one of methanol, ethyl alcohol and acetone.The quality of organic solvent is α-siliconnitride powder, metal
2~4 times of oxide, rare earth oxide and beta-silicon nitride crystal seed quality summation.Slurry after ball milling at 120~150 DEG C into
Row drying, drying can remove the organic solvent in slurry, obtain dry ceramic powder.Preferably, organic in ceramic powder
The content of solvent is controlled in 1wt% hereinafter, avoid in the subsequent sintering process gasifying due to solvent, and inside silicon nitride ceramics
Form hole.
Optionally, it is cold isostatic compaction by the method that ceramic powder is pressed into biscuit.Silicon nitride has smaller contraction
Coefficient can be suppressed according to the size of final finished in cold isostatic compaction, then is sintered.
Further, a kind of preparation method for dense silicon nitride ceramic material that the embodiment of the present invention is provided, is also wrapped
It includes：
S2. biscuit is subjected to one-stage sintering at 0.1~0.3Mpa of nitrogen pressure, 1300~1500 DEG C of temperature；Then exist
0.1~0.3Mpa of nitrogen pressure carries out bis sintering at 1600~1800 DEG C of temperature；Finally in 1.5~2Mpa of nitrogen pressure, temperature
Three-stage sintering is carried out at 1800~2000 DEG C of degree.
Optionally, the time of when a length of 1~3h of one-stage sintering, bis sintering are 6~12h, and the time of three-stage sintering is 6
~12h.
The embodiment of the present application, which uses, to be sintered three times to promote the densification of silicon nitride ceramics.One-stage sintering is compared with low pressure
It is carried out under (0.1~0.3Mpa) and lower temperature (1300~1500 DEG C), main purpose is to allow metal oxide, rare-earth oxidation
The auxiliary agents such as object, which first dissolve, forms liquid phase, and liquid phase can be more evenly distributed in inside biscuit, allows the silicon nitride of α phases can be more
Low dissolving is simultaneously dispersed to precipitate.
Bis sintering improves sintering temperature on the basis of one-stage sintering.Bis sintering is primarily to allow α-nitridation
Silicon powder can mutually be become β phases from α phases, while being precipitated and being grown in beta-silicon nitride seed surface by solution modeling, and isometric β phases are made
Silicon nitride grain is grown up, and this beta phase silicon nitride crystal grain with compared with big L/D ratio is silicon nitride material with compared with high-flexural strength
And the reason of toughness.It is also by the growth of beta phase silicon nitride that the stomata on biscuit surface is complete meanwhile during bis sintering
It is totally-enclosed.It is worth noting that, remaining stomata cannot be closed under the hyperbaric environment of three-stage sintering, it will influence most
The compactness extent of whole silicon nitride ceramics.
Three-stage sintering increases nitrogen pressure on the basis of bis sintering, in the case of high pressure-temperature, coarse etc.
Axis beta phase silicon nitride crystal grain can re-dissolve, and be precipitated and grown up again in the form of needle-shaped beta phase silicon nitride crystal grain, further increase
Add the densification degree of silicon nitride ceramics.Meanwhile nitrogen pressure also should not be too large, and nitrogen is avoided to penetrate into silicon nitride under high pressure
Ceramic inside re-forms stomata, influences to be densified.It is found by inventor's creative work, the air pressure of 1.5~2Mpa obtains
Silicon nitride ceramics densification degree it is preferable.
The embodiment of the present invention additionally provides a kind of dense silicon nitride ceramic material, by above-mentioned dense silicon nitride ceramics
The preparation method of material is prepared.Its density has high intensity, high tenacity, abrasion-proof corrosion-proof close to the theoretical density of silicon nitride
The characteristics of erosion.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of dense silicon nitride ceramic material is present embodiments provided, in parts by weight, raw material includes：
7 parts of 100 parts of α-siliconnitride powder, 0.5 part of aluminium oxide, 1 part of cerium oxide and beta-silicon nitride crystal seed.
Its specific preparation method is as follows：
S1. above-mentioned raw materials are mixed with 250 parts of absolute ethyl alcohol, slurry is made in ball milling 1h in the ball mill.
S2. above-mentioned slurry is dried at 120 DEG C, obtains ceramic powder.Organic solvent content is in ceramic powder
0.6wt%.
S3. biscuit is made by cold isostatic press in above-mentioned ceramic powder.
S4. biscuit is subjected to one-stage sintering, time 3h at nitrogen pressure 0.1Mpa, 1300 DEG C of temperature.
S5. nitrogen pressure 0.1Mpa is kept, increases temperature to 1600 DEG C of progress bis sinterings, time 12h.
S6. nitrogen pressure is increased to 1.5Mpa, increases temperature to 1800 DEG C of progress three-stage sinterings, time 12h obtains nitrogen
SiClx ceramics.
The density that the silicon nitride ceramics is measured by drainage is 3.41g/cm3, reach the 99.1% of theoretical density.
It is 1150MPa, fracture toughness 11.3MPam to measure its bending strength by three-point bending method1/2。
Embodiment 2
A kind of dense silicon nitride ceramic material is present embodiments provided, in parts by weight, raw material includes：
10 parts of 120 parts of α-siliconnitride powder, 2 parts of magnesia, 2 parts of yttrium oxide, 3 parts of lanthana and beta-silicon nitride crystal seed.
Its specific preparation method is as follows：
S1. above-mentioned raw materials are mixed with 300 parts of acetone, slurry is made in ball milling 2h in the ball mill.
S2. above-mentioned slurry is dried at 150 DEG C, obtains ceramic powder.Organic solvent content is in ceramic powder
0.5wt%.
S3. biscuit is made by cold isostatic press in above-mentioned ceramic powder.
S4. biscuit is subjected to one-stage sintering, time 1h at nitrogen pressure 0.3Mpa, 1500 DEG C of temperature.
S5. nitrogen pressure 0.3Mpa is kept, increases temperature to 1800 DEG C of progress bis sinterings, time 6h.
S6. nitrogen pressure is increased to 2Mpa, increases temperature to 2000 DEG C of progress three-stage sinterings, time 6h is nitrogenized
Silicon ceramics.
The density that the silicon nitride ceramics is measured by drainage is 3.40g/cm3, reach the 98.8% of theoretical density.
It is 1200MPa, fracture toughness 11.5MPam to measure its bending strength by three-point bending method1/2。
Embodiment 3
A kind of dense silicon nitride ceramic material is present embodiments provided, in parts by weight, raw material includes：
100 parts of α-siliconnitride powder, 1 part of zirconium oxide, 1 part of magnesia, 1 part of cerium oxide, 1 part of luteium oxide, 1 part of yttrium oxide,
And 8 parts of beta-silicon nitride crystal seed.
Its specific preparation method is as follows：
S1. above-mentioned raw materials are mixed with 400 parts of absolute ethyl alcohol, slurry is made in ball milling 1h in the ball mill.
S2. above-mentioned slurry is dried at 120 DEG C, obtains ceramic powder.Organic solvent content is in ceramic powder
0.8wt%.
S3. biscuit is made by cold isostatic press in above-mentioned ceramic powder.
S4. biscuit is subjected to one-stage sintering, time 2h at nitrogen pressure 0.2Mpa, 1300 DEG C of temperature.
S5. nitrogen pressure 0.2Mpa is kept, increases temperature to 1700 DEG C of progress bis sinterings, time 10h.
S6. nitrogen pressure is increased to 2Mpa, increases temperature to 2000 DEG C of progress three-stage sinterings, time 12h is nitrogenized
Silicon ceramics.
The density that the silicon nitride ceramics is measured by drainage is 3.42g/cm3, reach the 99.4% of theoretical density.
It is 1150MPa, fracture toughness 10.9MPam to measure its bending strength by three-point bending method1/2。
Embodiment 4
A kind of dense silicon nitride ceramic material is present embodiments provided, in parts by weight, raw material includes：
120 parts of α-siliconnitride powder, 0.5 part of aluminium oxide, 1.5 parts of titanium oxide, 1 part of cerium oxide, 2 parts of lanthana and β-
Nitrogenize 8 parts of silicon seed.
Its specific preparation method is as follows：
S1. above-mentioned raw materials are mixed with 350 parts of absolute ethyl alcohol, slurry is made in ball milling 1h in the ball mill.
S2. above-mentioned slurry is dried at 120 DEG C, obtains ceramic powder.Organic solvent content is in ceramic powder
0.9wt%.
S3. biscuit is made by cold isostatic press in above-mentioned ceramic powder.
S4. biscuit is subjected to one-stage sintering, time 3h at nitrogen pressure 0.3Mpa, 1350 DEG C of temperature.
S5. nitrogen pressure 0.3Mpa is kept, increases temperature to 1700 DEG C of progress bis sinterings, time 8h.
S6. nitrogen pressure is increased to 1.5Mpa, increases temperature to 1850 DEG C of progress three-stage sinterings, time 8h obtains nitrogen
SiClx ceramics.
The density that the silicon nitride ceramics is measured by drainage is 3.40g/cm3, reach the 98.9% of theoretical density.
It is 1100MPa, fracture toughness 10.8MPam to measure its bending strength by three-point bending method1/2。
In conclusion an embodiment of the present invention provides a kind of dense silicon nitride ceramics and preparation method thereof, α-is used
Beta-silicon nitride powder coordinates a small amount of sintering aid to be sintered, and induces the crystal form of α-siliconnitride powder to turn with beta-silicon nitride crystal seed
Change, to increase product density.Meanwhile the form of three-stage sintering, one-stage sintering are carried out under compared with low pressure and lower temperature, are allowed
Auxiliary agent forms liquid phase, and is uniformly distributed in α-siliconnitride powder；Bis sintering improves temperature on the basis of one-stage sintering,
It allows α-siliconnitride powder that can mutually become β phases from α phases, while being grown in beta-silicon nitride seed surface by solution modeling, and will
The stomata on biscuit surface is closed；Finally increase air pressure on the basis of bis sintering, biscuit is made further to be densified, is nitrogenized
Silicon ceramics.The dense silicon nitride ceramics being prepared by the above method, density have close to the theoretical density of silicon nitride
The characteristics of high intensity, high tenacity, wear resistant corrosion resistant.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of dense silicon nitride ceramic material, which is characterized in that including：
By the α-siliconnitride powder of 100~120 parts by weight, the rare earth of the metal oxide of 0.5~2 parts by weight, 1~5 parts by weight
Oxide and the beta-silicon nitride crystal seed of 7~10 parts by weight uniformly mix, and are pressed into biscuit；
The biscuit is subjected to one-stage sintering at 0.1~0.3Mpa of nitrogen pressure, 1300~1500 DEG C of temperature；Then in nitrogen
0.1~0.3Mpa of pressure carries out bis sintering at 1600~1800 DEG C of temperature；Finally in 1.5~2Mpa of nitrogen pressure, temperature
Three-stage sintering is carried out at 1800~2000 DEG C.
2. preparation method according to claim 1, which is characterized in that the purity of the α-siliconnitride powder is more than 99%, α
Phase content is more than 95wt%, and grain size is 0.2~0.5 μm.
3. preparation method according to claim 1, which is characterized in that a diameter of 0.5~1 μ of the beta-silicon nitride crystal seed
M, draw ratio are 7~10.
4. preparation method according to claim 1, which is characterized in that the metal oxide include aluminium oxide, magnesia,
At least one of zirconium oxide and titanium oxide.
5. preparation method according to claim 1, which is characterized in that the rare earth oxide include yttrium oxide, lanthana,
At least one of cerium oxide or luteium oxide.
6. preparation method according to claim 1, which is characterized in that when a length of 1~3h of the one-stage sintering, described two
The time of section sintering is 6~12h, and the time of the three-stage sintering is 6~12h.
7. preparation method according to claim 1, which is characterized in that aoxidized to the α-siliconnitride powder, the metal
The mixing of object, the rare earth oxide and the beta-silicon nitride crystal seed is to aoxidize the α-siliconnitride powder, the metal
Object, the rare earth oxide and the beta-silicon nitride crystal seed are scattered in organic solvent and carry out ball milling, then in 120~150 DEG C
Lower drying, obtains ceramic powder.
8. preparation method according to claim 7, which is characterized in that the organic solvent includes methanol, ethyl alcohol and acetone
At least one of.
9. preparation method according to claim 8, which is characterized in that be by the method that the ceramic powder is pressed into biscuit
Cold isostatic compaction.
10. a kind of dense silicon nitride ceramic material, which is characterized in that be densified nitrogen by claim 1~9 any one of them
The preparation method of SiClx ceramic material is prepared.
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| CN109970454A (en) * | 2019-03-20 | 2019-07-05 | 广东工业大学 | A kind of transition metal oxide inhibit silicon nitride phase transformation method and its silicon nitride ceramics obtained |
| CN109987943A (en) * | 2019-04-04 | 2019-07-09 | 天津大学 | A kind of preparation method of beta-silicon nitride powder |
| CN111393170A (en) * | 2020-03-19 | 2020-07-10 | 西安澳秦新材料有限公司 | Method for preparing high-density silicon nitride ceramic through multi-factor optimization and prepared silicon nitride ceramic |
| CN113213948A (en) * | 2021-05-31 | 2021-08-06 | 福建工程学院 | Preparation method of silicon nitride ceramic material with multilevel structure |
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| CN109678524A (en) * | 2019-02-22 | 2019-04-26 | 苏州玄陶商务咨询有限公司 | A kind of silicon nitride ceramics implantation material and preparation method thereof that performance is controllable |
| CN109678524B (en) * | 2019-02-22 | 2021-08-24 | 苏州玄陶商务咨询有限公司 | Silicon nitride ceramic implant with controllable performance and preparation method thereof |
| CN109970454A (en) * | 2019-03-20 | 2019-07-05 | 广东工业大学 | A kind of transition metal oxide inhibit silicon nitride phase transformation method and its silicon nitride ceramics obtained |
| CN109987943A (en) * | 2019-04-04 | 2019-07-09 | 天津大学 | A kind of preparation method of beta-silicon nitride powder |
| CN111393170A (en) * | 2020-03-19 | 2020-07-10 | 西安澳秦新材料有限公司 | Method for preparing high-density silicon nitride ceramic through multi-factor optimization and prepared silicon nitride ceramic |
| CN115551818A (en) * | 2020-05-07 | 2022-12-30 | Ａｇｃ株式会社 | Method for producing ceramic sintered body and ceramic sintered body |
| WO2022156634A1 (en) * | 2021-01-20 | 2022-07-28 | 中国科学院上海硅酸盐研究所 | Preparation method for copper plate-covered silicon nitride ceramic substrate |
| CN113213948A (en) * | 2021-05-31 | 2021-08-06 | 福建工程学院 | Preparation method of silicon nitride ceramic material with multilevel structure |
| CN115849918A (en) * | 2021-09-27 | 2023-03-28 | 赛默肯(苏州)电子新材料有限公司 | Silicon nitride ceramic material, substrate, raw material composition of silicon nitride ceramic material, preparation method of silicon nitride ceramic material and application of silicon nitride ceramic material |
| CN117800740A (en) * | 2022-09-26 | 2024-04-02 | 比亚迪股份有限公司 | Silicon nitride ceramic composition, silicon nitride ceramic and preparation method of silicon nitride ceramic |
| CN117303913A (en) * | 2023-10-19 | 2023-12-29 | 衡阳凯新特种材料科技有限公司 | High-performance silicon nitride sealing ring and preparation method thereof |
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