CN104119079B - A kind of sintering method improving silicon nitride material consistency of performance - Google Patents
A kind of sintering method improving silicon nitride material consistency of performance Download PDFInfo
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Abstract
The present invention relates to a kind of sintering method improving silicon nitride material consistency of performance, comprise the following steps: add magnesium oxide and lanthanum trioxide in A, silicon nitride raw material, be made into mixture, mixture is dry after wet-mixed, thinning processing; B, raw material good for processing of step A is loaded metal pattern, adopt first mechanical dry-pressing, and then seal, carry out cold isostatic compaction, the biscuit of the required shape of preparation; C, the biscuit prepared by step B, load gas pressure sintering stove, carry out gas pressure sintering; D, to step C sintering after blank shape roughing, ensure the consistence of material profile size, then graphite paper is superscribed, load pre-designed with step C sintering after blank shape consistent size graphite jig in, carry out hot pressed sintering again, obtain the silicon nitride that material property consistence is high.Compared with prior art, the present invention have low cost, material discrete little, simple to operate, be beneficial to the advantages such as suitability for industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of silicon nitride, especially relate to a kind of sintering method improving silicon nitride material consistency of performance.
Background technology
Silicon nitride ceramic material have high temperature resistant, wear-resistant, the coefficient of expansion is little, intensity is high, corrosion-resistant, the characteristic such as high rigidity, light specific gravity, range of application widely, it is one of key part promoting China's equipment manufacturing equipment level, but because preparation technology is different, be silicon nitride material equally, but performance difference is very large.Current industrialization sintered silicon nitride ceramic method is mainly as follows:
1, reaction sintering method: the method utilizes silicon raw material and nitrogen to react at high temperature to be prepared from, and advantage is that technique is simple, easy and simple to handle, and cost is low.Silicon nitride ceramics shortcoming prepared by this technique: densification is poor, there is the pore of about 20%, 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; Utilize silicon nitride raw material to add certain sintering aid, certain pressure nitrogen is filled with 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 produce 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 high-end field materials application.
3, hot-pressing sintering method: be utilize silicon nitride raw material to add certain sintering aid, certain mechanical external force is applied 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 sinter the material of simple shape, and manufacturing cost is high.
4, HIP sintering method: be utilize silicon nitride raw material to add certain sintering aid, high pressure nitrogen is filled with 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 produce complicated shape goods, and material bending strength is at 800 ~ 1000Mpa, bulk porosity, generally 0.02%, meets the requirement of silicon nitride as high-end field materials application.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 provide to overcome defect that above-mentioned prior art exists that a kind of low cost, material discrete 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:
Improve a sintering method for silicon nitride material consistency of performance, comprise the following steps:
The preparation of A, raw material:
Magnesium oxide and lanthanum trioxide is added in silicon nitride raw material, 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, the particle diameter of mixture is made all to be less than 2um, dry;
B, forming of green body:
Raw material good for processing of step A is loaded metal pattern, adopts first mechanical dry-pressing, and then seal, carry out cold isostatic compaction, the biscuit of the required shape of preparation;
C, gas pressure sintering:
Biscuit prepared by step B, load gas pressure sintering stove, carry out gas pressure sintering in a nitrogen atmosphere, 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 profile size, then graphite paper is superscribed, load pre-designed with step C sintering after blank shape consistent size graphite jig in, carry out hot pressed sintering again, the sintering temperature of hot pressed sintering is 1700 ~ 1800 DEG C, and the mechanical pressure of applying, at 40 ~ 150Mpa, obtains the silicon nitride that material property consistence is high.
Compared with prior art, the double sintering method that the present invention adopts gas pressure sintering method and hot-pressing sintering method to 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, this method solves the large defect of silicon nitride material discreteness of gas pressure sintering, is mechanical external force, can guarantees the consistency of performance of every part product material, therefore can meet high-end applications requirement due to what apply;
4, can prepare complicated shape goods, because after gas pressure sintering, silicon nitride product strength is higher, at employing hot pressed sintering, hot pressed sintering die design is fairly simple with charging comparatively speaking, no longer limits 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 MATERIALS METHODS, first gets silicon nitride raw material 8 kilograms, adds 1 kilogram, magnesium oxide, lanthanum trioxide 1 kilogram, through alcohol wet-mixed, thinning processing 30 hours, detects particle diameter at 1.5um, then dry; Again the raw material handled well is loaded metal pattern, be pressed into cylindric goods, and then then seal, carry out cold isostatic compaction.Next the biscuit of cylinder goods will suppressed, load gas pressure sintering stove, 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 profile size, then graphite paper is superscribed, loading is pre-designed, in the graphite jig that size is consistent with cylinder blank, carry out hot pressed sintering again, sintering temperature is at 1760 degrees Celsius, and the mechanical pressure of applying is at 120Mpa.After testing, through the method sintering silicon nitride cylinder bending strength at 900MPa, bulk porosity is 0.02%.
Embodiment 2
Improve a sintering method for silicon nitride material consistency of performance, comprise the following steps:
The preparation of A, raw material:
0.8 kilogram of magnesium oxide and 0.5 kilogram of lanthanum trioxide is added in 8.7 kilograms of silicon nitride raw materials, 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:
Raw material good for processing of step A is loaded metal pattern, adopts first mechanical dry-pressing, be pressed into rectangle, and then seal, carry out cold isostatic compaction, the biscuit of the required shape of preparation;
C, gas pressure sintering:
Biscuit prepared by step B, load gas pressure sintering stove, carry out gas pressure sintering in a nitrogen atmosphere, 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 profile size, then graphite paper is superscribed, load pre-designed with step C sintering after blank shape consistent size graphite jig in, carry out hot pressed sintering again, the sintering temperature of hot pressed sintering is 1700 DEG C, and the mechanical pressure of 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
Improve a sintering method for silicon nitride material consistency of performance, comprise the following steps:
The preparation of A, raw material:
0.9 kilogram of magnesium oxide and 0.8 kilogram of lanthanum trioxide is added in 8.3 kilograms of silicon nitride raw materials, 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:
Raw material good for processing of step A is loaded metal pattern, adopts first mechanical dry-pressing, and then seal, carry out cold isostatic compaction, the biscuit of the required shape of preparation;
C, gas pressure sintering:
Biscuit prepared by step B, load gas pressure sintering stove, carry out gas pressure sintering in a nitrogen atmosphere, 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 profile size, then graphite paper is superscribed, load pre-designed with step C sintering after blank shape consistent size graphite jig in, carry out hot pressed sintering again, the sintering temperature of hot pressed sintering is 1800 DEG C, and the mechanical pressure of 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%.
Above-mentioned is can understand and use invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (4)
1. improve a sintering method for silicon nitride material consistency of performance, it is characterized in that, comprise the following steps:
The preparation of A, raw material:
Add magnesium oxide and lanthanum trioxide in silicon nitride raw material, be made into mixture, magnesian quality is 8 ~ 10% of mixture quality, and the quality of lanthanum trioxide is 5 ~ 10% of mixture quality, and mixture is dry after wet-mixed, thinning processing;
B, forming of green body:
Raw material good for processing of step A is loaded metal pattern, adopts first mechanical dry-pressing, and then seal, carry out cold isostatic compaction, the biscuit of the required shape of preparation;
C, gas pressure sintering:
The biscuit prepared by step B, loads gas pressure sintering stove, carries out gas pressure sintering;
D, hot pressed sintering:
To the blank shape roughing after step C sintering, ensure the consistence of material profile size, then superscribe graphite paper, load pre-designed with step C sintering after blank shape consistent size graphite jig in, carry out hot pressed sintering again, obtain the silicon nitride that material property consistence is high.
2. a kind of sintering method improving silicon nitride material consistency of performance according to claim 1, it is characterized in that, in steps A, add the 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.
3. a kind of sintering method improving silicon nitride material consistency of performance according to claim 1, is characterized in that, in step C, carry out gas pressure sintering in a nitrogen atmosphere, sintering temperature is at 1780 ~ 1850 DEG C, and nitrogen pressure is at 8 ~ 10Mpa.
4. a kind of sintering method improving 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 of applying is at 40 ~ 150Mpa.
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| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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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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