CN108264355A - A kind of new and effective evaporation boat semiconductive ceramic - Google Patents

A kind of new and effective evaporation boat semiconductive ceramic Download PDF

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Publication number
CN108264355A
CN108264355A CN201810109920.5A CN201810109920A CN108264355A CN 108264355 A CN108264355 A CN 108264355A CN 201810109920 A CN201810109920 A CN 201810109920A CN 108264355 A CN108264355 A CN 108264355A
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evaporation boat
semiconductive ceramic
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silicon nitride
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杨自芬
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Hefei Zhuo Zhuo Electric Power Co Ltd
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Hefei Zhuo Zhuo Electric Power Co Ltd
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Abstract

The invention belongs to evaporation boat processing technique fields, and in particular to a kind of new and effective evaporation boat semiconductive ceramic.The semiconductive ceramic includes following ingredient：Boron nitride, titanium boride, aluminium nitride, silicon nitride, aluminium oxide, magnesia, calcium carbonate, silver powder, rare earth element additive, sodium cellulose glycolate and foaming agent.Wherein silicon nitride passes through modification, and the modified hydrochloric acid solution using butter of tin and antimony trichloride is handled；The sintering of the semiconductive ceramic carries out in sintering furnace, and sintering temperature is filled with the inert gas that air pressure is 14 18MPa and is protected at 2,100 2300 DEG C in sintering furnace.The evaporation boat surface texture of ceramics manufacture is fine and close, and air gap is contained in inside, and fever is uniform during use, and high-temperature behavior is excellent, not easy to break, high mechanical strength, and service life is long.

Description

A kind of new and effective evaporation boat semiconductive ceramic
Technical field
The invention belongs to evaporation boat processing technique fields, and in particular to a kind of new and effective evaporation boat semiconductive ceramic.
Background technology
Evaporation boat is using heat generating components in technique for vacuum coating, sends out heat thermogenetic by metal, gold by evaporation boat Belong to compound evaporation, then substrate surface is attached to by deposition technique and forms plated film, due to needing to generate a large amount of heat, bear The temperature of superelevation, therefore, evaporation boat are that a key of technique for vacuum coating easily consumes component.
The semiconductive ceramic that conventional evaporation boat uses is not fine and close enough there are material surface, and internal uniformity is poor to be lacked Point, this causes in use, and evaporation boat is with when bearing quick raised excessive temperature, easily bursting, material is led Electrically fluctuate larger, heat production is not sufficiently stable, and influences the consistency and quality of coating of metallic solution.In addition, the reason of because of structure, High-temperature behavior performance is not sufficiently stable, also poor with the wetting sex expression of plated metal liquid.
Invention content
In view of the above problems, the purpose of the present invention is to provide a kind of new and effective evaporation boat semiconductive ceramic, the pottery The evaporation boat surface texture of porcelain manufacture is fine and close, and air gap is contained in inside, and fever is uniform during use, and high-temperature behavior is excellent, not easy to break, High mechanical strength, service life are long.
A kind of new and effective evaporation boat semiconductive ceramic, according to mass fraction, including following ingredient：Boron nitride 80-90 Part, 85-100 parts of titanium boride, 20-35 parts of aluminium nitride, 15-18 parts of silicon nitride, 6-9 parts of aluminium oxide, 5-8 parts of magnesia, calcium carbonate 7-13 parts, 0.5-2 parts of silver powder, 3-6 parts of rare earth element additive, 8-10 parts of sodium cellulose glycolate, 4-6 parts of foaming agent.
Preferably, which includes following ingredient：84-86 parts of boron nitride, 90-93 parts of titanium boride, aluminium nitride 28- 30 parts, 16-17 parts of silicon nitride, 7-8 parts of aluminium oxide, 6-7 parts of magnesia, 10-11 parts of calcium carbonate, 1-1.2 parts of silver powder, rare earth element 4-5 parts of additive, 8-9 parts of sodium cellulose glycolate, 5-6 parts of foaming agent.
Wherein, the mesh number of boron nitride, titanium boride, aluminium nitride, silicon nitride, aluminium oxide, magnesia and each material of calcium carbonate is equal For 400-500 mesh.
Contain two or more in La, Ce, Y, Lu and Sc element in the rare earth element additive of the present invention.
By modification, modification includes the following steps silicon nitride in the present invention：Butter of tin and trichlorine is configured Change the hydrochloric acid solution of antimony, using the pH value of hydrochloric acid conditioning solution to 2-3, then be added to be formed in solution by alpha-silicon nitride powders and starch Material, 50-80min is reacted at a temperature of 40-45 DEG C, supernatant and chlorion are removed by way of centrifuge washing, using Microwave drying treatment, the temperature of microwave drying is 100-120 DEG C, obtains required modified silicon nitride.
It is further preferred that foaming agent selects poly- propionamide.
The preparation method of the semiconductive ceramic is as follows：Dispensing is carried out according to mass fraction shared by each raw material, dispensing is sent into It is uniformly mixed into batch mixer, sodium cellulose glycolate and foaming agent into batch mixer, and adds in and account for mixture quality 0.2-0.3 Distilled water again, is uniformly mixing to obtain blank, blank is sent to compression molding in mold obtains formed body, and formed body is sent into It is sintered into the hot-pressed sintering furnace of sealing, wherein, the temperature of Isothermal sinter is 2100-2300 DEG C, sintering time 2-3h.
Preferably, the briquetting pressure of mold process is 100-120 tons.
Preferably, by vacuum state in sintering furnace before temperature is increased to 1500 DEG C in sintering furnace, reach in temperature Inert gas is filled in 1500 DEG C of backward sintering furnace, it is 14-18MPa to keep the air pressure in sintering furnace, and Isothermal sinter process is protected Hold the air pressure.
A kind of new and effective evaporation boat semiconductive ceramic provided by the invention compared with prior art, has following excellent Point：
The boron nitride, titanium boride and aluminium nitride material of mainstream have first been selected in the main body ceramic material of the type semiconductive ceramic, has been passed through The corrosion resistance that modified silicon nitride further improves material is added, so as to which the substance in high temperature molten aluminum be avoided to be deposited Journey extends the service life of product to the corrosiveness of evaporation boat.
The use of rare earth element additive in material can improve the heat resisting temperature of material, allow material in vacuum-sintering Journey makes material internal structure more uniform, and forms on surface fine and close structure, allow evaporation boat in use with molten aluminum Fully wetting；In addition, because the electric conductivity of the ceramics can be consistent under temperature change state, therefore it is more steady to generate heat It is fixed, evaporation boat is reduced because of the failure rate that high temperature changes and bursts.
A small amount of foaming agent is added in, and burnt under the protection of vacuum and inert atmosphere in the type semiconductive ceramic material Knot, therefore miniature air gap can be formed in material internal, these air gaps can carry out heat conduction and buffering, further improve The consistency of evaporation boat fever process, avoids because without air gap, heat conductive process can not form buffering, and temperature change is violent Cause to burst；The gas in air can also be avoided to enter, and sintering ceramics are internal to lead to non-uniform air-gap, influences the steady of evaporation boat Fixed fever.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It should be understood that specific implementation described herein Mode is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
Embodiment 1
A kind of new and effective evaporation boat semiconductive ceramic, according to mass fraction, including following ingredient：80 parts of boron nitride, boronation 85 parts of titanium, 20 parts of aluminium nitride, 15 parts of silicon nitride, 6 parts of aluminium oxide, 5 parts of magnesia, 7 parts of calcium carbonate, 0.5 part of silver powder, rare earth element 3 parts of additive, 8 parts of sodium cellulose glycolate, 4 parts of foaming agent.
Wherein, the mesh number of boron nitride, titanium boride, aluminium nitride, silicon nitride, aluminium oxide, magnesia and each material of calcium carbonate is equal For 400 mesh；Foaming agent selects poly- propionamide.
Contain La, Ce element in the rare earth element additive of the present embodiment.
By modification, modification includes the following steps silicon nitride in the present embodiment：Butter of tin and three is configured Alpha-silicon nitride powders using the pH value of hydrochloric acid conditioning solution to 2, then are added to be formed in solution and starch by the hydrochloric acid solution of antimony chloride Material, reacts 50min at a temperature of 40 DEG C, supernatant and chlorion is removed by way of centrifuge washing, done using microwave Dry processing, the temperature of microwave drying is 100 DEG C, obtains required modified silicon nitride.
The preparation method of the semiconductive ceramic is as follows：Dispensing is carried out according to mass fraction shared by each raw material, dispensing is sent into It is uniformly mixed into batch mixer, sodium cellulose glycolate and foaming agent into batch mixer, and adds in and account for 0.2 times of mixture quality Distilled water is uniformly mixing to obtain blank, and blank is sent to compression molding in mold obtains formed body, formed body is sent to close It is sintered in the hot-pressed sintering furnace of envelope, wherein, the temperature of Isothermal sinter is 2100 DEG C, sintering time 2h.
Wherein, the briquetting pressure of mold process is 100 tons；Temperature will be in sintering furnace before being increased to 1500 DEG C in sintering furnace Vacuum state reaches 1500 DEG C rear in temperature and inert gas is filled with into sintering furnace, keeps the air pressure in sintering furnace to be 14MPa, Isothermal sinter process keep the air pressure.
Embodiment 2
A kind of new and effective evaporation boat semiconductive ceramic, according to mass fraction, including following ingredient：90 parts of boron nitride, boronation 100 parts of titanium, 35 parts of aluminium nitride, 18 parts of silicon nitride, 9 parts of aluminium oxide, 8 parts of magnesia, 13 parts of calcium carbonate, 2 parts of silver powder, rare earth element 6 parts of additive, 10 parts of sodium cellulose glycolate, 6 parts of foaming agent.
Wherein, the mesh number of boron nitride, titanium boride, aluminium nitride, silicon nitride, aluminium oxide, magnesia and each material of calcium carbonate is equal For 500 mesh；Foaming agent selects poly- propionamide.
Contain Y, Lu element in the rare earth element additive of the present embodiment.
By modification, modification includes the following steps silicon nitride in the present embodiment：Butter of tin and three is configured Alpha-silicon nitride powders using the pH value of hydrochloric acid conditioning solution to 3, then are added to be formed in solution and starch by the hydrochloric acid solution of antimony chloride Material, reacts 80min at a temperature of 45 DEG C, supernatant and chlorion is removed by way of centrifuge washing, done using microwave Dry processing, the temperature of microwave drying is 120 DEG C, obtains required modified silicon nitride.
The preparation method of the semiconductive ceramic is as follows：Dispensing is carried out according to mass fraction shared by each raw material, dispensing is sent into It is uniformly mixed into batch mixer, sodium cellulose glycolate and foaming agent into batch mixer, and adds in and account for 0.3 times of mixture quality Distilled water is uniformly mixing to obtain blank, and blank is sent to compression molding in mold obtains formed body, formed body is sent to close It is sintered in the hot-pressed sintering furnace of envelope, wherein, the temperature of Isothermal sinter is 2300 DEG C, sintering time 3h.
Wherein, the briquetting pressure of mold process is 120 tons；Temperature will be in sintering furnace before being increased to 1500 DEG C in sintering furnace Vacuum state reaches 1500 DEG C rear in temperature and inert gas is filled with into sintering furnace, keeps the air pressure in sintering furnace to be 18MPa, Isothermal sinter process keep the air pressure.
Embodiment 3
A kind of new and effective evaporation boat semiconductive ceramic, according to mass fraction, including following ingredient：85 parts of boron nitride, boronation 90 parts of titanium, 30 parts of aluminium nitride, 16 parts of silicon nitride, 8 parts of aluminium oxide, 7 parts of magnesia, 10 parts of calcium carbonate, 1.2 parts of silver powder, rare earth member Plain 4 parts of additive, 9 parts of sodium cellulose glycolate, 5 parts of foaming agent.
Wherein, the mesh number of boron nitride, titanium boride, aluminium nitride, silicon nitride, aluminium oxide, magnesia and each material of calcium carbonate is equal For 450 mesh；Foaming agent selects poly- propionamide.
Contain Ce, Y, Sc element in the rare earth element additive of the present embodiment.
By modification, modification includes the following steps silicon nitride in the present embodiment：Butter of tin and three is configured Alpha-silicon nitride powders using the pH value of hydrochloric acid conditioning solution to 2.5, are then added in solution and are formed by the hydrochloric acid solution of antimony chloride Slurry reacts 65min at a temperature of 43 DEG C, supernatant and chlorion is removed by way of centrifuge washing, using microwave It is dried, the temperature of microwave drying is 110 DEG C, obtains required modified silicon nitride.
The preparation method of the semiconductive ceramic is as follows：Dispensing is carried out according to mass fraction shared by each raw material, dispensing is sent into It is uniformly mixed into batch mixer, sodium cellulose glycolate and foaming agent into batch mixer, and adds in and account for 0.25 times of mixture quality Distilled water, be uniformly mixing to obtain blank, blank is sent to compression molding in mold obtains formed body, and formed body is sent to It is sintered in the hot-pressed sintering furnace of sealing, wherein, the temperature of Isothermal sinter is 2200 DEG C, sintering time 2.5h.
Wherein, the briquetting pressure of mold process is 110 tons；Temperature will be in sintering furnace before being increased to 1500 DEG C in sintering furnace Vacuum state reaches 1500 DEG C rear in temperature and inert gas is filled with into sintering furnace, keeps the air pressure in sintering furnace to be 16MPa, Isothermal sinter process keep the air pressure.
Embodiment 4
A kind of new and effective evaporation boat semiconductive ceramic, according to mass fraction, including following ingredient：80 parts of boron nitride, boronation 100 parts of titanium, 35 parts of aluminium nitride, 16 parts of silicon nitride, 7 parts of aluminium oxide, 8 parts of magnesia, 7 parts of calcium carbonate, 0.8 part of silver powder, rare earth member Plain 5 parts of additive, 10 parts of sodium cellulose glycolate, 4 parts of foaming agent.
Wherein, the mesh number of boron nitride, titanium boride, aluminium nitride, silicon nitride, aluminium oxide, magnesia and each material of calcium carbonate is equal For 400 mesh；Foaming agent selects poly- propionamide.
Contain La, Y, Sc element in the rare earth element additive of the present embodiment.
By modification, modification includes the following steps silicon nitride in the present embodiment：Butter of tin and three is configured Alpha-silicon nitride powders using the pH value of hydrochloric acid conditioning solution to 3, then are added to be formed in solution and starch by the hydrochloric acid solution of antimony chloride Material, reacts 70min at a temperature of 45 DEG C, supernatant and chlorion is removed by way of centrifuge washing, done using microwave Dry processing, the temperature of microwave drying is 120 DEG C, obtains required modified silicon nitride.
The preparation method of the semiconductive ceramic is as follows：Dispensing is carried out according to mass fraction shared by each raw material, dispensing is sent into It is uniformly mixed into batch mixer, sodium cellulose glycolate and foaming agent into batch mixer, and adds in and account for 0.3 times of mixture quality Distilled water is uniformly mixing to obtain blank, and blank is sent to compression molding in mold obtains formed body, formed body is sent to close It is sintered in the hot-pressed sintering furnace of envelope, wherein, the temperature of Isothermal sinter is 2100 DEG C, sintering time 2.5h.
Wherein, the briquetting pressure of mold process is 110 tons；Temperature will be in sintering furnace before being increased to 1500 DEG C in sintering furnace Vacuum state reaches 1500 DEG C rear in temperature and inert gas is filled with into sintering furnace, keeps the air pressure in sintering furnace to be 18MPa, Isothermal sinter process keep the air pressure.
Performance test
By experiment test, the evaporation boat heating efficiency of the semiconductive ceramic manufacture of the present embodiment improves 5-9%, service life Improve 10-15%.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring the substantive content of the present invention.

Claims (9)

1. a kind of new and effective evaporation boat semiconductive ceramic, it is characterised in that：According to mass fraction, the semiconductive ceramic packet Include following ingredient：80-90 parts of boron nitride, 85-100 parts of titanium boride, 20-35 parts of aluminium nitride, 15-18 parts of silicon nitride, aluminium oxide 6-9 Part, 5-8 parts of magnesia, 7-13 parts of calcium carbonate, 0.5-2 parts of silver powder, 3-6 parts of rare earth element additive, sodium cellulose glycolate 8- 10 parts, 4-6 parts of foaming agent.
2. a kind of new and effective evaporation boat semiconductive ceramic according to claim 1, it is characterised in that：The semiconductor pottery Porcelain includes following ingredient：84-86 parts of boron nitride, 90-93 parts of titanium boride, 28-30 parts of aluminium nitride, 16-17 parts of silicon nitride, aluminium oxide 7-8 parts, 6-7 parts of magnesia, 10-11 parts of calcium carbonate, 1-1.2 parts of silver powder, 4-5 parts of rare earth element additive, hydroxymethyl cellulose 8-9 parts of sodium, 5-6 parts of foaming agent.
3. a kind of new and effective evaporation boat semiconductive ceramic according to claim 1, it is characterised in that：The boron nitride, Titanium boride, aluminium nitride, silicon nitride, aluminium oxide, magnesia and each material of calcium carbonate mesh number be 400-500 mesh.
4. a kind of new and effective evaporation boat semiconductive ceramic according to claim 1, it is characterised in that：The rare earth element Contain two or more in La, Ce, Y, Lu and Sc element in additive.
5. a kind of new and effective evaporation boat semiconductive ceramic according to claim 1, it is characterised in that：The silicon nitride warp Modification is crossed, modification includes the following steps：The hydrochloric acid solution of butter of tin and antimony trichloride is configured, is adjusted using hydrochloric acid Then alpha-silicon nitride powders are added in solution to 2-3 and form slurry, 50- is reacted at a temperature of 40-45 DEG C by the pH value of solution 80min removes supernatant and chlorion by way of centrifuge washing, using microwave drying treatment, the temperature of microwave drying It is 100-120 DEG C, obtains required modified silicon nitride.
6. a kind of new and effective evaporation boat semiconductive ceramic according to claim 1, it is characterised in that：The foaming agent choosing With poly- propionamide.
7. a kind of new and effective evaporation boat semiconductive ceramic according to claim 1, it is characterised in that：The semiconductive pottery The preparation method of porcelain is as follows：Dispensing is carried out according to mass fraction shared by each raw material, dispensing is sent in batch mixer and is uniformly mixed, Sodium cellulose glycolate and foaming agent into batch mixer, and the distilled water for accounting for 0.2-0.3 times of mixture quality is added in, it stirs evenly Blank is obtained, blank is sent to compression molding in mold obtains formed body, and formed body is sent to the hot-pressed sintering furnace of sealing In be sintered, wherein, the temperature of Isothermal sinter is 2100-2300 DEG C, sintering time 2-3h.
8. a kind of new and effective evaporation boat semiconductive ceramic according to claim 7, it is characterised in that：The mold process Briquetting pressure be 100-120 tons.
9. a kind of new and effective evaporation boat semiconductive ceramic according to claim 7, it is characterised in that：In the sintering furnace Temperature is increased to vacuum state in sintering furnace before 1500 DEG C, and reach 1500 DEG C rear in temperature is filled with into sintering furnace Inert gas, it is 14-18MPa to keep the air pressure in sintering furnace, and Isothermal sinter process keeps the air pressure.
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CN103805822A (en) * 2013-09-26 2014-05-21 山东鹏程特种陶瓷有限公司 High-performance four-component conductive ceramics evaporating boat and production process thereof
CN104177089A (en) * 2014-09-15 2014-12-03 山东理工大学 Process for preparing zirconium boride based conductive ceramic evaporation boat
CN104609865A (en) * 2015-02-09 2015-05-13 广东工业大学 Preparation method of silicon nitride-based conductive ceramic and molding method of silicon nitride-based conductive ceramic cutting tool
CN105081327A (en) * 2015-08-28 2015-11-25 南通高欣耐磨科技股份有限公司 High-strength and shock-resistance type metal ceramic composite lining plate and preparation method thereof

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CN103805822A (en) * 2013-09-26 2014-05-21 山东鹏程特种陶瓷有限公司 High-performance four-component conductive ceramics evaporating boat and production process thereof
CN104177089A (en) * 2014-09-15 2014-12-03 山东理工大学 Process for preparing zirconium boride based conductive ceramic evaporation boat
CN104609865A (en) * 2015-02-09 2015-05-13 广东工业大学 Preparation method of silicon nitride-based conductive ceramic and molding method of silicon nitride-based conductive ceramic cutting tool
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* Cited by examiner, † Cited by third party
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CN117185833A (en) * 2023-09-13 2023-12-08 信阳中毅高热材料有限公司 Light heat-insulating refractory ceramic material and preparation method thereof
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Application publication date: 20180710