CN100465132C - Preparation method of carborundum composite-phase ceramic - Google Patents
Preparation method of carborundum composite-phase ceramic Download PDFInfo
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- CN100465132C CN100465132C CNB2007100672761A CN200710067276A CN100465132C CN 100465132 C CN100465132 C CN 100465132C CN B2007100672761 A CNB2007100672761 A CN B2007100672761A CN 200710067276 A CN200710067276 A CN 200710067276A CN 100465132 C CN100465132 C CN 100465132C
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Abstract
The invention discloses a producing method for carborundum complex phase ceram including a compound powder composed of carborundum and yttrium aluminitum garnet, firstly orderly doing a dry pressing and prepressing and cold isopressing, then sintering the disposed biscuit in vacuum without pressure; the weight percent proportion of the compound powder: 85-95% of carborundum and 5-15% of carborundum and yttrium aluminitum garnet; the preparing process including: 1) respectively adding the aluminum nitrate, yttrium nitrate into deionized water, then slowly adding methenamine solution, blending for 10-20 minutes at 35-80 DEG C to obtain transparent sol carborundum and yttrium aluminitum garnet; 2) adding carborundum fine powder, blending for 15-30 minutes in the water of 50-80 DEG C to obtain compound gel; 3) after the compound gel dry, heat processing for 2-6 hours at 900-920 DEG C to obtain compound powder. The produced carborundum complex phase ceram has a good mechanical property and a good thermal property.
Description
Technical field
The present invention relates to a kind of preparation method of carborundum composite-phase ceramic.
Background technology
Silicon carbide ceramics has many good characteristics as a kind of high-temperature structural ceramics, and is good etc. as wear resistance, high thermal conductivity and electric insulating quality, semiconductive and electric conductivity, heat-resisting, corrosion-resistant and high-temperature mechanics and thermal property.Silicon carbide ceramics has been widely used in industrial circle and national defense industry such as machinery, electronics, petrochemical complex, metallurgy, and has been confirmed as the 4th kind of basic machinery sealing material since metal, aluminum oxide, Wimet in the world.
But high-purity silicon carbide is difficult to carry out densification sintering, needs to add sintering aid usually.Sintering aid is generally commonly used B-C, Al-B-C, Al
2O
3, AlN-Y
2O
3, Al
2O
3-Re
2O
3Deng, Re is one or more of rare earth element, wherein the most effective sintering aid is Al
2O
3-Y
2O
3, with yttrium aluminum garnet (Y
3Al
5O
12, be called for short YAG) and be the silicon carbide ceramics of main sintering aid, owing under lower temperature, can realize densification sintering, be considered to one of silicon carbide-based ceramic body system that has most development prospect.
Prepare the method for silicon carbide ceramics about yttrium aluminum garnet as sintering aid, open in many pieces of communiques such as publication US 445238, CN1552664A.Aforesaid method generally adopts the mechanical blending method directly to introduce aluminum oxide and yttrium oxide mixture, utilizes under the high temperature aluminum oxide and yttrium oxide to generate yttrium aluminum garnet and prepares carborundum composite-phase ceramic; Aforesaid method exists following shortcoming: batch mixing is irregular, causes sintering aid skewness in silicon carbide substrate; And sintering temperature need be controlled at more than 1950 ℃, produces volatilization thereby cause aluminum oxide and silicon carbide to react, and causes the loss of effective constituent.
Summary of the invention
Thereby providing, the technical problem to be solved in the present invention a kind ofly can improve the carborundum composite-phase ceramic preparation method that the carborundum composite-phase ceramic sintering character improves its mechanical property and thermal property.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of carborundum composite-phase ceramic, comprise the composite granule of forming by silicon carbide and yttrium aluminum garnet, earlier composite granule is adopted successively dry-pressing precompressed and cold isostatic pressing end pressing to handle, the biscuit that will handle the back gained again carries out vacuum non-pressure sintering; The weight percent of this composite granule consists of: 85%～95% silicon carbide and 5%～15% yttrium aluminum garnet; The preparation process of this composite granule may further comprise the steps:
1), aluminum nitrate, Yttrium trinitrate added respectively in the deionized water to mix stirred 8～12 minutes, the atomic molar of described yttrium and aluminium is than being 3:5, the weight sum of described aluminum nitrate and Yttrium trinitrate and the weight ratio of deionized water are 2.5～7.7:100; Slowly add hexamethylenetetramine solution again, mix at 35～80 ℃ and stirred 10～20 minutes, obtain the yttrium aluminum garnet of vitreosol shape, the weight ratio of described hexamethylenetetramine solution and deionized water is 0.25～1:100;
2), in the yttrium aluminum garnet of above-mentioned vitreosol shape, add carbide fine powder, obtained plural gel in 15～30 minutes through 50 ℃～80 ℃ stirring in water bath;
3), treat above-mentioned plural gel ageing drying after, obtained composite granule in 2～6 hours 900 ℃～920 ℃ thermal treatments.
Improvement as the preparation method of carborundum composite-phase ceramic of the present invention: the pressure of dry-pressing precompressed is 100～180MPa, and the pressure of cold isostatic pressing end pressing is 200～250MPa; Sintering temperature is that 1860 ℃～1900 ℃, time are 1～4 hour.
The preparation method of carborundum composite-phase ceramic of the present invention belongs to a kind of preparation method who introduces the carborundum composite-phase ceramic of sintering aid, and specifically, particularly colloidal sol-gel is introduced the preparation method of the silicon carbide ceramics of yttrium aluminum garnet.
The present invention is that the contriver obtains through conscientiously studying, testing.The present invention adopts the inorganic salt sol-gel processing to introduce the sintering agent yttrium aluminum garnet, has realized the thorough mixing and the uniform distribution of sintering agent and silicon carbide substrate; And adopt two one-step forming technology, realized the densification sintering of composite granule at a lower temperature.Therefore can overcome the shortcoming of mechanical blending method of the prior art; Effectively realize the sintering agent homogenization of composition, improve the activity of composite granule, reduced sintering temperature, improved the sintering character of silicon carbide ceramics, improved the mechanical property and the thermal property of silicon carbide ceramics.According to the carborundum composite-phase ceramic that the present invention makes, its density is 3.15～3.25g/cm
3, hardness is 22～28GPa, and bending strength is 450～600MPa, and fracture toughness property is 4.5～7MPam
1/2
Description of drawings
Fig. 1 is the composite granule stereoscan photograph that makes in the process of the present invention;
Fig. 2 is the stereoscan photograph in the carborundum composite-phase ceramic cross section that finally makes of the present invention.
Embodiment
The preparation method of embodiment 1, a kind of carborundum composite-phase ceramic, carry out following steps (following umber is weight part) successively:
1), be precursor material with Yttrium trinitrate, aluminum nitrate, hexamethylenetetramine is a catalyzer, deionized water is made solvent; Yttrium trinitrate, aluminum nitrate added respectively mix in 100 parts the deionized water and stirred 10 minutes, the atomic molar of yttrium and aluminium is than being 3:5, and the weight sum of aluminum nitrate and Yttrium trinitrate is 4 parts; The hexamethylenetetramine solution that slowly adds 0.25 part again mixes stirring 15 minutes at 50 ℃, obtains the yttrium aluminum garnet of vitreosol shape;
2), in containing the above-mentioned transparent yttrium aluminum garnet colloidal sol of 8 parts of yttrium aluminum garnets, add 92 parts of carbide fine powder, obtained plural gel in 15 minutes through 80 ℃ of stirred in water bath;
3), treat above-mentioned plural gel ageing drying after, obtained silicon carbide composite powder body in 4 hours 900 ℃～920 ℃ thermal treatments, the apparent pattern of this composite granule as shown in Figure 1;
4), above-mentioned composite granule is adopted 100～180MPa dry-pressing precompressed earlier, use 200～250MPa cold isostatic pressing end pressing again, obtain biscuit; Biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 1860 ℃ of insulations 4 hours, obtain carborundum composite-phase ceramic.
This carborundum composite-phase ceramic density is 3.15～3.25g/cm
3, hardness is 22～28GPa, and bending strength is 450～600MPa, and fracture toughness property is 4.5～7MPam
1/2Its structure as shown in Figure 2.
The preparation method of embodiment 2, a kind of carborundum composite-phase ceramic, carry out following steps (following umber is weight part) successively:
1), be precursor material with Yttrium trinitrate, aluminum nitrate, hexamethylenetetramine is a catalyzer, deionized water is made solvent; Yttrium trinitrate, aluminum nitrate added respectively mix in 100 parts the deionized water and stirred 8 minutes, the atomic molar of yttrium and aluminium is than being 3:5, and the weight sum of aluminum nitrate and Yttrium trinitrate is 2.5 parts; The hexamethylenetetramine solution that slowly adds 0.5 part again mixes stirring 20 minutes at 35 ℃, obtains the yttrium aluminum garnet of vitreosol shape;
2), in containing the above-mentioned transparent yttrium aluminum garnet colloidal sol of 5 parts of yttrium aluminum garnets, add 95 parts of carbide fine powder, obtained plural gel in 30 minutes through 50 ℃ of stirred in water bath;
3), treat above-mentioned plural gel ageing drying after, obtained silicon carbide composite powder body in 2 hours 900 ℃～920 ℃ thermal treatments;
4), above-mentioned composite granule is adopted 100～180MPa dry-pressing precompressed earlier, use 200～250MPa cold isostatic pressing end pressing again, obtain biscuit; Biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 1900 ℃ of insulations 1 hour, obtain carborundum composite-phase ceramic.
This carborundum composite-phase ceramic density is 3.15～3.25g/cm
3, hardness is 22～28GPa, and bending strength is 450～600MPa, and fracture toughness property is 4.5～7MPam
1/2
The preparation method of embodiment 3, a kind of carborundum composite-phase ceramic, carry out following steps (following umber is weight part) successively:
1), be precursor material with Yttrium trinitrate, aluminum nitrate, hexamethylenetetramine is a catalyzer, deionized water is made solvent; Yttrium trinitrate, aluminum nitrate added respectively mix in 100 parts the deionized water and stirred 12 minutes, the atomic molar of yttrium and aluminium is than being 3:5, and the weight sum of aluminum nitrate and Yttrium trinitrate is 7.7 parts; The hexamethylenetetramine solution that slowly adds 1 part again mixes stirring 10 minutes at 80 ℃, obtains the yttrium aluminum garnet of vitreosol shape;
2), in containing the above-mentioned transparent yttrium aluminum garnet colloidal sol of 15 parts of yttrium aluminum garnets, add 85 parts of carbide fine powder, obtained plural gel in 20 minutes through 70 ℃ of stirred in water bath;
3), treat above-mentioned plural gel ageing drying after, obtained silicon carbide composite powder body in 6 hours 900 ℃～920 ℃ thermal treatments;
4), above-mentioned composite granule is adopted 100～180MPa dry-pressing precompressed earlier, use 200～250MPa cold isostatic pressing end pressing again, obtain biscuit; Biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 1880 ℃ of insulations 2 hours, obtain carborundum composite-phase ceramic.
This carborundum composite-phase ceramic density is 3.15～3.25g/cm
3, hardness is 22～28GPa, and bending strength is 450～600MPa, and fracture toughness property is 4.5～7MPam
1/2
In order to prove the superiority of the prepared carborundum composite-phase ceramic performance of the inventive method, the contriver has made following simultaneous test:
Adopt the mechanical blending method preparation of prior art: the mixture of aluminum oxide and yttrium oxide and the weight ratio of silicon carbide are 8:92, and wherein yttrium and aluminium atomic molar are than being 3:5.
Aluminum oxide and yttrium oxide are directly joined the SiC powder, and deionized water is a ball-milling medium, and mechanical ball milling blend 6 hours prepares silicon carbide composite powder body; 180MPa dry-pressing precompressed, 250MPa cold isostatic pressing end pressing are adopted in the shaping of composite granule; Biscuit is put into vacuum non-pressure sintering furnace, be warming up to 1950 ℃ of insulations 1 hour, obtain relatively sample of required silicon carbide ceramics.Its volume density 3.20g/cm
3, hardness is 22GPa, and bending strength is 450MPa, and fracture toughness property is 4.9m
1/2
Two kinds of carborundum composite-phase ceramics of the inventive method and simultaneous test method gained are compared obtain:
The present invention is that sol-gel processing is introduced in the silicon carbide composite powder body of yttrium aluminum garnet preparation, and the distribution of yttrium aluminum garnet is more even, and sintering temperature reduces by 50 ℃～100 ℃, and the structure and the mechanical property of silicon carbide ceramics are more superior.This is because adopt sol-gel processing to form yttrium aluminum garnet sintering aid phase at silicon carbide in advance, liquidus temperature (1760 ℃) at yttrium aluminum garnet just can form liquid phase, densification silicon carbide, and the mechanical blending method need be more than 1760 ℃, aluminum oxide and yttrium oxide just begin the generation yttrium aluminum garnet that reacts, and the generation liquid phase is carried out densification, therefore only just can finish the silicon carbide densification process in higher temperature, if aluminum oxide and yttrium oxide skewness in silicon carbide substrate, must cause sintering temperature higher, silicon carbide ceramics structure and degradation.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (2)
1, a kind of preparation method of carborundum composite-phase ceramic comprises the composite granule of being made up of silicon carbide and yttrium aluminum garnet, earlier composite granule is adopted successively dry-pressing precompressed and cold isostatic pressing end pressing to handle, and the biscuit that will handle the back gained again carries out vacuum non-pressure sintering; It is characterized in that: the weight percent of described composite granule consists of: 85%～95% silicon carbide and 5%～15% yttrium aluminum garnet; The preparation process of described composite granule may further comprise the steps:
1), aluminum nitrate, Yttrium trinitrate added respectively in the deionized water to mix stirred 8～12 minutes, the atomic molar of described yttrium and aluminium is than being 3:5, the weight sum of described aluminum nitrate and Yttrium trinitrate and the weight ratio of deionized water are 2.5～7.7:100; Slowly add hexamethylenetetramine solution again, mix at 35～80 ℃ and stirred 10～20 minutes, obtain the yttrium aluminum garnet of vitreosol shape, the weight ratio of described hexamethylenetetramine solution and deionized water is 0.25～1:100;
2), in the yttrium aluminum garnet of above-mentioned vitreosol shape, add carbide fine powder, obtained plural gel in 15～30 minutes through 50 ℃～80 ℃ stirring in water bath;
3), treat above-mentioned plural gel ageing drying after, obtained composite granule in 2～6 hours 900 ℃～920 ℃ thermal treatments.
2, the preparation method of carborundum composite-phase ceramic according to claim 1 is characterized in that: the pressure of described dry-pressing precompressed is 100～180MPa, and the pressure of described cold isostatic pressing end pressing is 200～250MPa; Described sintering temperature is that 1860 ℃～1900 ℃, time are 1～4 hour.
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| CN101182211B (en) * | 2007-11-09 | 2010-06-02 | 浙江大学 | Nano silicon carbide ceramic preparation method |
| CN101811890B (en) * | 2009-12-28 | 2012-09-05 | 河北理工大学 | Acid-resisting complex phase ceramic coating and preparation method thereof |
| CN102757237B (en) * | 2012-06-28 | 2013-11-06 | 航天材料及工艺研究所 | Method for adding ceramic material sintering aid |
| CN106045521A (en) * | 2016-05-27 | 2016-10-26 | 台州东新密封有限公司 | Method using hot pressed sintering to prepare dry-gas-seal rotating ring |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0664971A (en) * | 1992-08-19 | 1994-03-08 | Mitsubishi Heavy Ind Ltd | Sintered compact of ceramics |
| EP0648717A2 (en) * | 1993-10-12 | 1995-04-19 | Isuzu Ceramics Research Institute Co., Ltd. | Reaction sintered ceramics and method of producing the same |
| CN1587203A (en) * | 2004-07-01 | 2005-03-02 | 西北第二民族学院 | High toughness high hardness silicon carbide ceramic lqiuid phase sintering method |
| CN1785900A (en) * | 2005-10-28 | 2006-06-14 | 浙江大学 | Silicon carbide base multiphase composite ceramic and its preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0664971A (en) * | 1992-08-19 | 1994-03-08 | Mitsubishi Heavy Ind Ltd | Sintered compact of ceramics |
| EP0648717A2 (en) * | 1993-10-12 | 1995-04-19 | Isuzu Ceramics Research Institute Co., Ltd. | Reaction sintered ceramics and method of producing the same |
| CN1587203A (en) * | 2004-07-01 | 2005-03-02 | 西北第二民族学院 | High toughness high hardness silicon carbide ceramic lqiuid phase sintering method |
| CN1785900A (en) * | 2005-10-28 | 2006-06-14 | 浙江大学 | Silicon carbide base multiphase composite ceramic and its preparation method |
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