CN102757237A - Method for adding ceramic material sintering aid - Google Patents
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Abstract
The invention provides a method for adding a ceramic material sintering aid. The method comprises the following steps of: (1) adding a nitrate of the sintering aid into deionized water, and stirring until the nitrate is fully dissolved; (2) immersing a pre-sintered silicon carbide or silicon nitride ceramic body into a container which is filled with a sintering aid saline solution, and vacuum-pumping; and dipping under a certain pressure condition, and thus immersing the sintering aid saline solution into the ceramic body; and (3) drying an obtained ceramic body after the immersion under the condition from the room temperature to temperature of 90 DEG C, and obtaining a product. The method provided by the invention has the advantages that the distribution uniformity of the sintering aid in the ceramic body is effectively improved, the densification for the ceramic sintering is facilitated, and the mechanical performance of the ceramic material is increased. Since the solution viscosity of the sintering aid is lower, the flowability of the sintering aid is better, the sintering aid can be fully immersed into the ceramic body and is good in distribution uniformity, thus the problem of nonuniform distribution of the sintering aid in the ceramic is effectively solved, and the sintering performance and the mechanical property of the ceramic are improved.
Description
Technical field
The present invention relates to the structural ceramics field, be specifically related to a kind of adding method of stupalith sintering aid.
Background technology
High performance structure ceramic has performances such as high firmness, HS, high temperature resistant, resistance to chemical attack, high heat conductance, is widely used in each industrial circle, like silit and silicon nitride ceramics.The introducing and the distribution thereof of such ceramic sintering, structure and performance and sintering aid have confidential relation, and the preparation of composite granule is to obtain one of key of high performance structures composite ceramic material.If the total composition of composite granule all adopts chemosynthesis, then the technology cost is too high, and is difficult to obtain identical synthesis condition.If with the ceramic powder is matrix, introduce sintering aid and prepare composite granule, the introducing mode of sintering aid seems particularly crucial so.Present introducing mode is mainly the mechanical blending method, promptly reaches direct introducing sintering aid powder according to a certain ratio, carries out mechanical blending with ceramic powder, thereby obtains composite granule.Though this method is simple to operate, because density and powder granularity difference can cause sintering aid skewness in ceramic powder, reduce the sintering character of composite granule, the mechanical property of final influence pottery.
Summary of the invention
The object of the present invention is to provide a kind of adding method of stupalith sintering aid,, improve the sintering character and the mechanical property of pottery to overcome existing sintering aid problem of uneven distribution in ceramic body.
Realize the object of the invention technical scheme: a kind of adding method of stupalith sintering aid, it comprises the steps:
(1) preparation of sintering aid salts solution: the nitrate salt of sintering aid is joined in the deionized water, and stirring makes it to dissolve fully; The nitrate salt of described sintering aid is the one or more combination in aluminum nitrate, magnesium nitrate, Yttrium trinitrate, nitrate of baryta, nitrocalcite, samaric nitrate, europium nitrate, ytterbium nitrate or the Gadolinium trinitrate; The nitrate salt of this sintering aid and the mass ratio of deionized water are (3 ~ 20): 100;
(2) dipping: silit after the presintering or silicon nitride ceramics base substrate are immersed in the container of the sintering aid salts solution that step (1) gained is housed, make ceramic body submerge fully in this solution; Vacuumize then; Dipping 10min～48h under 1Mpa～10Mpa pressure condition is immersed in the ceramic body sintering aid salts solution again;
(3) drying:, obtain product at room temperature to 90 ℃ following baking step (2) dipping back gained ceramic body.
The adding method of aforesaid a kind of stupalith sintering aid, its step (2) is described to vacuumize and does, vacuum tightness≤0.1Pa, and the pumpdown time is 10min～48h.
The adding method of aforesaid a kind of stupalith sintering aid, silit or silicon nitride ceramics base substrate after the described presintering of its step (2) be, silit or silicon nitride ceramics base substrate be sintering 1h～2h under 600 ℃ ~ 1000 ℃, condition of nitrogen gas.
The adding method of aforesaid a kind of stupalith sintering aid, its step (3) is described to be 30min～7 day at room temperature to 90 a ℃ following drying time.
Effect of the present invention is: the present invention is through being made into certain density solution with the corresponding salt of sintering aid, and the method through impregnating by pressure makes it to infiltrate in the ceramic body, and the ceramic body oven dry after will flooding then is retained in the ceramic body sintering aid.This method has effectively been improved the homogeneity that sintering aid distributes in ceramic body, help the densification of ceramic post sintering, improves the mechanical property of stupalith.Because the soltion viscosity of sintering aid is lower; Better mobile, can fully be immersed in the ceramic body, and have good distributing homogeneity; Efficiently solve sintering aid in the inner problem of uneven distribution of pottery, improved ceramic sintering character and mechanical property.
Description of drawings
Fig. 1 is the stereoscan photograph of the silicon nitride ceramics of the present invention's preparation.
Embodiment
Further describe below in conjunction with accompanying drawing and specific embodiment adding method a kind of stupalith sintering aid of the present invention.
Embodiment 1
The adding method of a kind of stupalith sintering aid of the present invention, it comprises the steps:
(1) preparation of sintering aid salts solution: aluminum nitrate and magnesium nitrate are joined in the deionized water, and stirring makes it to dissolve fully; Described aluminum nitrate: magnesium nitrate: deionized water=5:5:90 (mass ratio);
(2) dipping: the silicon nitride ceramics base substrate after the presintering (the silicon nitride ceramics base substrate is sintering 2h under 600 ℃, condition of nitrogen gas) is immersed in the container of magnesium nitrate that step (1) gained is housed and aluminum nitrate aqueous solution, makes ceramic body submerge fully in this solution; Vacuumize then, vacuum tightness≤0.1Pa, the pumpdown time is 30min; Dipping 2h under the 2Mpa pressure condition is immersed in the ceramic body sintering aid salts solution again;
(3) drying: the gained ceramic body in 80 ℃ of following baking steps (2) dipping back, obtain the equally distributed silicon nitride ceramics product of sintering aid, its stereoscan photograph is as shown in Figure 1.
Embodiment 2
The adding method of a kind of stupalith sintering aid of the present invention, it comprises the steps:
(1) preparation of sintering aid salts solution: aluminum nitrate and Yttrium trinitrate are joined in the deionized water, and stirring makes it to dissolve fully; Described aluminum nitrate: Yttrium trinitrate: deionized water=4:6:90 (mass ratio);
(2) dipping: the silicon nitride ceramics base substrate after the presintering (the silicon nitride ceramics base substrate is sintering 1.5h under 800 ℃, condition of nitrogen gas) is immersed in the container of Yttrium trinitrate that step (1) gained is housed and aluminum nitrate aqueous solution, makes ceramic body submerge fully in this solution; Vacuumize then, vacuum tightness≤0.1Pa, the pumpdown time is 1h; Dipping 2h under the 2Mpa pressure condition is immersed in the ceramic body sintering aid salts solution again;
(3) drying: the gained ceramic body in 80 ℃ of following baking steps (2) dipping back obtains the equally distributed silicon nitride ceramics product of sintering aid.
Embodiment 3
The adding method of a kind of stupalith sintering aid of the present invention, it comprises the steps:
(1) preparation of sintering aid salts solution: aluminum nitrate and magnesium nitrate are joined in the deionized water, and stirring makes it to dissolve fully; Described aluminum nitrate: magnesium nitrate: deionized water=5:5:90 (mass ratio);
(2) dipping: the silicon carbide ceramic body after the presintering (silicon carbide ceramic body is sintering 1h under 700 ℃, condition of nitrogen gas) is immersed in the container of magnesium nitrate that step (1) gained is housed and aluminum nitrate aqueous solution, makes ceramic body submerge fully in this solution; Vacuumize then, vacuum tightness≤0.1Pa, the pumpdown time is 1h; Dipping 2h under the 2Mpa pressure condition is immersed in the ceramic body sintering aid salts solution again;
(3) drying: the gained ceramic body in 60 ℃ of following baking steps (2) dipping back obtains the equally distributed silicon carbide ceramics product of sintering aid.
Embodiment 4
The adding method of a kind of stupalith sintering aid of the present invention, it comprises the steps:
(1) preparation of sintering aid salts solution: aluminum nitrate is joined in the deionized water, and stirring makes it to dissolve fully; Described aluminum nitrate: deionized water=10:100 (mass ratio);
(2) dipping: (silicon carbide ceramic body is sintering 1h under 1000 ℃, condition of nitrogen gas) is immersed in the container of the aluminum nitrate aqueous solution that step (1) gained is housed with the silicon carbide ceramic body after the presintering, makes ceramic body submerge fully in this solution; Vacuumize then, vacuum tightness≤0.1Pa, the pumpdown time is 10min; Dipping 48h under the 1Mpa pressure condition is immersed in the ceramic body sintering aid salts solution again;
(3) drying: at room temperature baking step (2) floods back gained ceramic body, and drying time is 7 days, obtains the equally distributed silicon carbide ceramics product of sintering aid.
Embodiment 5
The adding method of a kind of stupalith sintering aid of the present invention, it comprises the steps:
(1) preparation of sintering aid salts solution: nitrocalcite and nitrate of baryta are joined in the deionized water, and stirring makes it to dissolve fully; Described nitrocalcite: nitrate of baryta: deionized water=10:10:100 (mass ratio);
(2) dipping: the silicon nitride ceramics base substrate after the presintering (the silicon nitride ceramics base substrate is sintering 1.5h under 700 ℃, condition of nitrogen gas) is immersed in the container of nitrocalcite that step (1) gained is housed and barium nitrate aqueous solution, makes ceramic body submerge fully in this solution; Vacuumize then, vacuum tightness≤0.1Pa, the pumpdown time is 48h; Dipping 10min under the 10Mpa pressure condition is immersed in the ceramic body sintering aid salts solution again;
(3) drying: the gained ceramic body in 90 ℃ of following baking steps (2) dipping back, drying time is 30min, obtains the equally distributed silicon nitride ceramics product of sintering aid.
Embodiment 6
The adding method of a kind of stupalith sintering aid of the present invention, it comprises the steps:
(1) preparation of sintering aid salts solution: europium nitrate, ytterbium nitrate and Gadolinium trinitrate are joined in the deionized water, and stirring makes it to dissolve fully; Described europium nitrate: ytterbium nitrate: Gadolinium trinitrate: deionized water=1:1:1:100 (mass ratio);
(2) dipping: (silicon carbide ceramic body is sintering 2h under 600 ℃, condition of nitrogen gas) is immersed in the container of the sintering aid salts solution that step (1) gained is housed with the silicon carbide ceramic body after the presintering, makes ceramic body submerge fully in this solution; Vacuumize then, vacuum tightness 0.1Pa, the pumpdown time is 24h; Dipping 10h under the 5Mpa pressure condition is immersed in the ceramic body sintering aid salts solution again;
(3) drying: the gained ceramic body in 50 ℃ of following baking steps (2) dipping back, drying time is 3 days, obtains the equally distributed silicon carbide ceramics product of sintering aid.
Claims (4)
1. the adding method of a stupalith sintering aid, it is characterized in that: this method comprises the steps:
(1) preparation of sintering aid salts solution: the nitrate salt of sintering aid is joined in the deionized water, and stirring makes it to dissolve fully; The nitrate salt of described sintering aid is the one or more combination in aluminum nitrate, magnesium nitrate, Yttrium trinitrate, nitrate of baryta, nitrocalcite, samaric nitrate, europium nitrate, ytterbium nitrate or the Gadolinium trinitrate; The nitrate salt of this sintering aid and the mass ratio of deionized water are (3 ~ 20): 100;
(2) dipping: silit after the presintering or silicon nitride ceramics base substrate are immersed in the container of the sintering aid salts solution that step (1) gained is housed, make ceramic body submerge fully in this solution; Vacuumize then; Dipping 10min～48h under 1Mpa～10Mpa pressure condition is immersed in the ceramic body sintering aid salts solution again;
(3) drying:, obtain product at room temperature to 90 ℃ following baking step (2) dipping back gained ceramic body.
2. the adding method of a kind of stupalith sintering aid according to claim 1 is characterized in that: step (2) is described to vacuumize and does, vacuum tightness≤0.1Pa, and the pumpdown time is 10min～48h.
3. the adding method of a kind of stupalith sintering aid according to claim 1; It is characterized in that: silit or silicon nitride ceramics base substrate after the described presintering of step (2) be, silit or silicon nitride ceramics base substrate be sintering 1h～2h under 600 ℃ ~ 1000 ℃, condition of nitrogen gas.
4. the adding method of a kind of stupalith sintering aid according to claim 1 is characterized in that: step (3) is described to be 30min～7 day at room temperature to 90 a ℃ following drying time.
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| CN103274696A (en) * | 2013-04-19 | 2013-09-04 | 北京中材人工晶体研究院有限公司 | Heat wave-transmission porous ceramic material and preparation method thereof |
| WO2018045782A1 (en) * | 2016-09-09 | 2018-03-15 | 深圳市绎立锐光科技开发有限公司 | Preparation method for ceramic composite material, ceramic composite material, and light source apparatus |
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| CN108752015A (en) * | 2018-06-12 | 2018-11-06 | 佛山市华强协兴陶瓷有限公司 | A kind of ceramic material sintering aid and preparation method thereof |
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| WO2018045782A1 (en) * | 2016-09-09 | 2018-03-15 | 深圳市绎立锐光科技开发有限公司 | Preparation method for ceramic composite material, ceramic composite material, and light source apparatus |
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