CN104119079A - Sintering method for improving performance consistency of silicon nitride material - Google Patents
Sintering method for improving performance consistency of silicon nitride material Download PDFInfo
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- CN104119079A CN104119079A CN201410379641.2A CN201410379641A CN104119079A CN 104119079 A CN104119079 A CN 104119079A CN 201410379641 A CN201410379641 A CN 201410379641A CN 104119079 A CN104119079 A CN 104119079A
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Abstract
The invention relates to a sintering method for improving the performance consistency of a silicon nitride material. The sintering method comprises the following steps: A. adding magnesium oxide and lanthanum oxide into a silicon nitride raw material to prepare a mixed material, conducting wet-process mixing and fining treatment to the mixed material, and drying; B. feeding the raw material, treated in the step A, into a metal mold, firstly conducting mechanical dry pressing, then sealing and carrying out isostatic cool pressing to prepare a biscuit with required shapes; C. feeding the biscuit, prepared in the step B, into an atmospheric sintering furnace for performing atmospheric sintering; D. roughly processing the appearance of the biscuit, sintered in the step C, so as to guarantee the appearance size consistency of the materials, then wrapping with graphite paper, feeding into a predesigned graphite mold, the size of which is consistent with the appearance size of the biscuit sintered in the step C, and then conducting hot-pressed sintering to obtain silicon nitride having high material performance consistency. Compared with the prior art, the sintering method has the advantages of being low in cost, small in material discretness, simple to operate, beneficial to industrial production, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of silicon nitride, especially relate to a kind of sintering method that improves silicon nitride material consistency of performance.
Background technology
The characteristics such as that silicon nitride ceramic material has is high temperature resistant, wear-resistant, the coefficient of expansion is little, intensity is high, corrosion-resistant, high rigidity, light specific gravity, range of application is very extensive, it is one of key part promoting China's equipment producing apparatus level, but due to preparation technology's difference, be silicon nitride material equally, but performance difference is very large.Industrialization sintered silicon nitride ceramic method is mainly as follows at present:
1, reaction sintering method: the method is to utilize silicon raw material and nitrogen to react and be prepared from high temperature, advantage is that technique is simple, easy and simple to handle, cost is low.Silicon nitride ceramics shortcoming prepared by this technique: densification is poor, the pore of existence 20% left and right, intensity is low, and bending strength, generally at 200～300Mpa, is only suitable for being applied in low side field.
2, gas pressure sintering method; To utilize silicon nitride raw material to add certain sintering aid, be filled with certain pressure nitrogen in the condition of high temperature, realize the method for silicon nitride ceramics sintering densification, nitrogen is as pressure medium, general nitrogen pressure is no more than 10MPa, this technological advantage can be produced complicated shape goods, and cost can meet requirement on industrial application.At 700～800Mpa, there is certain pore in bending strength, bulk porosity is generally 0.06%, and shortcoming is that the comparison of coherence of material is poor, can only apply as middle-end material, cannot meet the requirement of silicon nitride as the application of high-end field material.
3, hot-pressing sintering method: be to utilize silicon nitride raw material to add certain sintering aid, apply certain mechanical external force in the condition of high temperature, realize the method for silicon nitride ceramics sintering densification, this technological advantage material is completely fine and close, bulk porosity is generally 0.02%, bending strength, at 900～1000MPa, meets the application of silicon nitride material as high-end field material completely.Shortcoming can only sintering simple shape material, manufacturing cost is high.
4, HIP sintering method: be to utilize silicon nitride raw material to add certain sintering aid, be filled with high pressure nitrogen in the condition of high temperature, realize the method for silicon nitride ceramics sintering densification, nitrogen is as pressure medium, general nitrogen pressure 100～200MPa, this technological advantage can be produced complicated shape goods, and material bending strength is at 800～1000Mpa, bulk porosity, generally 0.02%, meets the requirement of silicon nitride as the application of high-end field material.Shortcoming cost is high, complex operation.The method critical process is also controlled by external at present.
Summary of the invention
Object of the present invention is exactly to provide in order to overcome the defect that above-mentioned prior art exists that a kind of low cost, material discreteness are little, simple to operate, the sintering method of the raising silicon nitride material consistency of performance that is beneficial to suitability for industrialized production.
Object of the present invention can be achieved through the following technical solutions:
A sintering method that improves silicon nitride material consistency of performance, comprises the following steps:
The preparation of A, raw material:
In silicon nitride raw material, add magnesium oxide and lanthanum trioxide, be made into mixture, magnesian quality is 8～10% of mixture quality, the quality of lanthanum trioxide is 5～10% of mixture quality, mixture was through the thinning processing of 20～60 hours, make the particle diameter of mixture all be less than 2um, dry;
B, forming of green body:
The raw material that processing of step A is good packs metal pattern into, adopts first mechanical dry-pressing, and then sealing, carries out cold isostatic compaction, the biscuit of the preparation shape that requires;
C, gas pressure sintering:
Biscuit prepared by step B, packs gas pressure sintering stove into, carries out gas pressure sintering under nitrogen atmosphere, and sintering temperature is at 1780～1850 DEG C, and nitrogen pressure is at 8～10Mpa;
D, hot pressed sintering:
To the blank shape roughing after step C sintering, ensure the consistence of material physical dimension, then superscribe graphite paper, pack in the graphite jig of the blank shape consistent size after pre-designed and step C sintering, carry out again hot pressed sintering, the sintering temperature of hot pressed sintering is 1700～1800 DEG C, and the mechanical pressure applying, at 40～150Mpa, obtains the silicon nitride that material property consistence is high.
Compared with prior art, the present invention adopts the double sintering method that gas pressure sintering method and hot-pressing sintering method combine to prepare silicon nitride, has the following advantages:
1, this technology can reach HIP sintering method and prepares properties of materials: bulk porosity is 0.02%, and bending strength is at 800～1000Mpa;
2, tooling cost is relatively low, and this technique can reduce the cost of hot-pressing sintering method 50%;
3, the discreteness of material is little, and the method has solved the large defect of silicon nitride material discreteness of gas pressure sintering, is mechanical external force due to what apply, can guarantee the consistency of performance of every product material, therefore can meet high-end applications requirement;
4, can prepare complicated shape goods, because silicon nitride product strength after gas pressure sintering is higher, adopt hot pressed sintering, hot pressed sintering die design and charging are fairly simple comparatively speaking, limited by shape;
5, simple to operate, be conducive to suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
A kind of sintering high strength silicon nitride material method, first gets 8 kilograms of silicon nitride raw materials, adds 1 kilogram, magnesium oxide, 1 kilogram of lanthanum trioxide, and process alcohol wet-mixed, thinning processing 30 hours, detect particle diameter at 1.5um, then dry; Pack the raw material of handling well into metal pattern again, be pressed into cylindric goods, and then then sealing, carry out cold isostatic compaction.Next by the biscuit of the cylinder goods that suppress, pack gas pressure sintering stove into, carry out gas pressure sintering, sintering temperature is at 1800 degrees Celsius, and nitrogen pressure is at 8Mpa.The simple roughing of cylinder blank shape that next it will be sintered, ensure the consistence of material physical dimension, then superscribe graphite paper, it is pre-designed packing into, in the size graphite jig consistent with cylinder blank, carry out hot pressed sintering, sintering temperature is at 1760 degrees Celsius again, and the mechanical pressure applying is at 120Mpa.After testing, the silicon nitride cylinder bending strength of process the method sintering is at 900MPa, and bulk porosity is 0.02%.
Embodiment 2
A sintering method that improves silicon nitride material consistency of performance, comprises the following steps:
The preparation of A, raw material:
In 8.7 kilograms of silicon nitride raw materials, add 0.8 kilogram of magnesium oxide and 0.5 kilogram of lanthanum trioxide, be made into mixture, magnesian quality is 8% of mixture quality, the quality of lanthanum trioxide is 5% of mixture quality, mixture was through the thinning processing of 20 hours, detect particle diameter at 1.6um, dry;
B, forming of green body:
The raw material that processing of step A is good packs metal pattern into, adopts first mechanical dry-pressing, is pressed into rectangle, and then sealing, carries out cold isostatic compaction, the biscuit of the preparation shape that requires;
C, gas pressure sintering:
Biscuit prepared by step B, packs gas pressure sintering stove into, carries out gas pressure sintering under nitrogen atmosphere, and sintering temperature is at 1780 DEG C, and nitrogen pressure is at 8Mpa;
D, hot pressed sintering:
To the blank shape roughing after step C sintering, ensure the consistence of material physical dimension, then superscribe graphite paper, pack in the graphite jig of the blank shape consistent size after pre-designed and step C sintering, carry out again hot pressed sintering, the sintering temperature of hot pressed sintering is 1700 DEG C, and the mechanical pressure applying, at 40Mpa, obtains the silicon nitride that material property consistence is high.
After testing, the silicon nitride cylinder bending strength of the present embodiment sintering is at 980MPa, and bulk porosity is 0.02%.
Embodiment 3
A sintering method that improves silicon nitride material consistency of performance, comprises the following steps:
The preparation of A, raw material:
In 8.3 kilograms of silicon nitride raw materials, add 0.9 kilogram of magnesium oxide and 0.8 kilogram of lanthanum trioxide, be made into mixture, magnesian quality is 9% of mixture quality, the quality of lanthanum trioxide is 8% of mixture quality, mixture was through the thinning processing of 60 hours, detect particle diameter at 1.6um, dry;
B, forming of green body:
The raw material that processing of step A is good packs metal pattern into, adopts first mechanical dry-pressing, and then sealing, carries out cold isostatic compaction, the biscuit of the preparation shape that requires;
C, gas pressure sintering:
Biscuit prepared by step B, packs gas pressure sintering stove into, carries out gas pressure sintering under nitrogen atmosphere, and sintering temperature is at 1850 DEG C, and nitrogen pressure is at 10Mpa;
D, hot pressed sintering:
To the blank shape roughing after step C sintering, ensure the consistence of material physical dimension, then superscribe graphite paper, pack in the graphite jig of the blank shape consistent size after pre-designed and step C sintering, carry out again hot pressed sintering, the sintering temperature of hot pressed sintering is 1800 DEG C, and the mechanical pressure applying, at 150Mpa, obtains the silicon nitride that material property consistence is high.
After testing, the silicon nitride cylinder bending strength of the present embodiment sintering is at 940MPa, and bulk porosity is 0.017%.
The above-mentioned description to embodiment is can understand and use invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various amendments to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art are according to announcement of the present invention, and not departing from improvement and the amendment that category of the present invention makes all should be within protection scope of the present invention.
Claims (5)
1. a sintering method that improves silicon nitride material consistency of performance, is characterized in that, comprises the following steps:
The preparation of A, raw material:
In silicon nitride raw material, add magnesium oxide and lanthanum trioxide, be made into mixture, mixture is dry after wet-mixed, thinning processing;
B, forming of green body:
The raw material that processing of step A is good packs metal pattern into, adopts first mechanical dry-pressing, and then sealing, carries out cold isostatic compaction, the biscuit of the preparation shape that requires;
C, gas pressure sintering:
Biscuit prepared by step B, packs gas pressure sintering stove into, carries out gas pressure sintering;
D, hot pressed sintering:
To the blank shape roughing after step C sintering, the consistence that ensures material physical dimension, then superscribes graphite paper, packs in the graphite jig of the blank shape consistent size after pre-designed and step C sintering, carry out again hot pressed sintering, obtain the silicon nitride that material property consistence is high.
2. a kind of sintering method that improves silicon nitride material consistency of performance according to claim 1, is characterized in that, in steps A, magnesian quality is 8～10% of mixture quality, and the quality of lanthanum trioxide is 5～10% of mixture quality.
3. a kind of sintering method that improves silicon nitride material consistency of performance according to claim 1, it is characterized in that, in steps A, add mixture after magnesium oxide and lanthanum trioxide through the thinning processing of 20～60 hours, make the particle diameter of mixture all be less than 2um.
4. a kind of sintering method that improves silicon nitride material consistency of performance according to claim 1, is characterized in that, in step C, carries out gas pressure sintering under nitrogen atmosphere, and sintering temperature is at 1780～1850 DEG C, and nitrogen pressure is at 8～10Mpa.
5. a kind of sintering method that improves silicon nitride material consistency of performance according to claim 1, is characterized in that, in step D, the sintering temperature of described hot pressed sintering is 1700～1800 DEG C, and the mechanical pressure applying is at 40～150Mpa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819450A (en) * | 2016-03-29 | 2016-08-03 | 上海泛联科技股份有限公司 | Silicon nitride ceramic tail gas hood for polycrystalline silicon reducing furnace and preparation method of tail gas hood |
| CN111548163A (en) * | 2020-05-18 | 2020-08-18 | 北京中材人工晶体研究院有限公司 | Method for preparing silicon nitride ceramic balls for large-size wind power generation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057826A (en) * | 1990-07-05 | 1992-01-15 | 清华大学 | Silicon nitride-based composite ceramic and piston head thereof |
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2014
- 2014-08-04 CN CN201410379641.2A patent/CN104119079B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057826A (en) * | 1990-07-05 | 1992-01-15 | 清华大学 | Silicon nitride-based composite ceramic and piston head thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819450A (en) * | 2016-03-29 | 2016-08-03 | 上海泛联科技股份有限公司 | Silicon nitride ceramic tail gas hood for polycrystalline silicon reducing furnace and preparation method of tail gas hood |
| CN111548163A (en) * | 2020-05-18 | 2020-08-18 | 北京中材人工晶体研究院有限公司 | Method for preparing silicon nitride ceramic balls for large-size wind power generation |
| CN111548163B (en) * | 2020-05-18 | 2022-07-15 | 北京中材人工晶体研究院有限公司 | Method for preparing silicon nitride ceramic ball for large-size wind power generation |
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Denomination of invention: A Sintering Method for Improving the Consistency of Properties of Silicon Nitride Materials Effective date of registration: 20230828 Granted publication date: 20160120 Pledgee: Industrial Bank Co.,Ltd. Shanghai Jiading sub branch Pledgor: Shanghai Unite Technology Co.,Ltd. Registration number: Y2023310000488 |
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