CN106631041A - Production and manufacturing technology of silicon nitride ceramic tiny component - Google Patents

Production and manufacturing technology of silicon nitride ceramic tiny component Download PDF

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Publication number
CN106631041A
CN106631041A CN201710009608.4A CN201710009608A CN106631041A CN 106631041 A CN106631041 A CN 106631041A CN 201710009608 A CN201710009608 A CN 201710009608A CN 106631041 A CN106631041 A CN 106631041A
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workpiece
silicon nitride
manufacturing technology
encapsulation
element manufacturing
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Abstract

The invention discloses a production and manufacturing technology of a silicon nitride ceramic tiny component. The technology comprises the following steps of preparing materials for production including ceramic main powder, a sintering auxiliary agent, heterogeneous particles, a defoaming agent, deionized water and a bonding agent; mixing the heterogeneous particles into deionized water; adding the defoaming agent to prepare uniform slurry; mixing the ceramic main powder into the uniform slurry; performing drying after the uniform stirring; then, crushing the materials into powder A; adding the bonding agent into the powder A; using a sweet dumpling rolling method for manufacturing a required workpiece; using a plastic bath ceramic biscuit encapsulation method for performing encapsulation; adding the sintering auxiliary agent; using a firstly higher and then lower heat insulation measure for performing sintering treatment on the workpiece. The comprehensive measures of the crystal grain refining, micrometer toughening and nanometer reinforcement, the firstly higher and then lower heat insulation method and the like are used for improving the performance index of the silicon nitride ceramic. The plastic bath encapsulation method is used for solving the encapsulation problem of the biscuit in a complicated shape; the production efficiency of the tiny workpiece encapsulation is greatly improved.

Description

A kind of silicon nitride ceramics micro-element manufacturing technology
Technical field
The present invention relates to Materials Science and Engineering technical field, more particularly to a kind of silicon nitride ceramics micro-element production system Make technology.
Background technology
The production path of advanced ceramics is：（1）Dispensing-（2）Batch mixing and abrasive material-(3) granulate ---（4）Shaping ---（5） Isostatic cool pressing ---（6）Degumming ---（7）Sintering.Each link affects the quality of product in existing technique.Composition is different Just determine the microstructure of material so as to just determine its various performances；The method of abrasive material and time and subsequent sintering System determines that the grain size of sintered body also has significant effect to performance.Isostatic cool pressing determines the density of biscuit so as to determine The size in the space of sintered body and distribution etc..All there is the space being extremely improved in existing links.
Micro-element must assure that its microstructure is uniform and can not have oversized defect such as due to size reason Cavity, therefore processed through calm pressure before sintering.And due to traditional method, to carry out efficiency too low therefore compel to be essential Invent a kind of new method that can form higher production efficiency.Based on above statement, the present invention proposes a kind of silicon nitride Ceramic micro-element manufacturing technology.
The content of the invention
The invention aims to shortcoming present in prior art is solved, and a kind of silicon nitride ceramics for proposing is small Part manufacturing technology.
A kind of silicon nitride ceramics micro-element manufacturing technology, the manufacturing technology include design of material/formula, Shaping and biscuit densification and three parts of sintering technology；Specifically include following steps：
S1, preparation production material：The main powder of ceramics, sintering aid, heterogeneous particles, deaeration agent, deionized water, binding agent；
S2, heterogeneous particles are mixed in deionized water, add deaeration agent to make uniform sizing material and be mixed into ceramic main powder, after stirring Drying, is then comminuted into powders A；
S3, binding agent is added using the powders A obtained by step S2, workpiece needed for being obtained using " rolling Lantern Festival " method, and utilize " modeling The biscuit of ceramics package method of bath " is packaged to it；
S4, the workpiece to completing to encapsulate in step S3 are sintered, and sintering aid are added in sintering process, first by workpiece liter Temperature is arrived to 1750～1780 DEG C, and after 10～20min of insulation 30～40 DEG C are reduced, and continues to be incubated, and temperature retention time is for during conventional insulation Between 2 times.
Preferably, the ceramic main powder in step S1 is silicon nitride powder of the phase containing α not less than 92, and free silica is less than 0.2%, iron and calcium impurities are not more than 100ppm, and granularity D50 is less than 0.5 micron.
Preferably, the sintering aid in step S1 is lanthana, yittrium oxide, magnesia, aluminum oxide cerium oxide, oxidation One or more in strontium, aluminium nitride and niobium oxide, granularity is nanoscale, and total amount is in 8～12%WT.
Preferably, the heterogeneous particles in step S1 are one or more in titanium nitride, titanium carbide and aluminium nitride, its Consumption is 3～5%WT of ceramic main powder amount, and granularity is 5～10 times of ceramic main powder.
Preferably, the binding agent in step S1 is the polyvinyl alcohol of 0.2～3% concentration.
Preferably, obtained powders A is equally applicable to require high rigidity, high-fracture toughness, high abrasion in step S2 In, the part of big size, obtained final product using traditional forming method shaping.
Preferably, the biscuit of ceramics package method of " the modeling bath " in step S3 specifically includes two kinds：A, use macromolecule Polymer coats film in surface of the work as cladding medium with immersion way, and workpiece is dissolved and is soaked in liquid state colloid, Vibrations disperse to remove the bubble of surface of the work, drench dry after then workpiece is pulled out from liquid state colloid, and vibrations disperse to prevent work The mutual adhesion of part, workpiece is dried in the drying box of 300～800 DEG C of high temperature, and keeps mutual adhesion between workpiece；B, use High molecular polymer coats film in surface of the work, by cladding melting glue as cladding medium with the mode solidified after fusing Workpiece is solidified by help of drying, and avoids mutual adhesion between workpiece；The cladding medium is polyvinyl alcohol, polyvinyl alcohol contracting One or more in butyraldehyde, polyethylene and polypropylene；The liquid state colloid concentration is higher than the workpiece for compression molding；It is described Melting gum concentration is less than the workpiece for compression molding.
Preferably, during encapsulation technology in step S3 is equally applicable, the encapsulation of large complicated part.
A kind of silicon nitride ceramics micro-element manufacturing technology proposed by the present invention, to silicon nitride advanced ceramics material from Powder composition, mix grinding arrive again to shaping and sinter related link and all done optimization processing, and the quality for making material has obtained very big carrying Rise, particularly invented " modeling bath package method " and, to substantially increasing micro-element production efficiency, be capable of achieving to produce in enormous quantities, this It is bright to take low frit thermal-insulating method related measure after crystal grain refinement, micron toughness reinforcing nanometer reinforcement and first height, improve silicon nitride pottery The performance indications of porcelain, with " modeling bath " package method, solve the problems, such as the encapsulation of complicated shape biscuit, drastically increase microscale workpieces The production efficiency of encapsulation, by refining powder, reduces the pore size of sintered body, reduces porosity, improves the densification of tissue Degree, using low Insulation after first height, effectively inhibits too growing up for crystal grain, and the silicon nitride microballon of present invention production can It is used for mobile phone, notebook computer, medicine equipment, refill for ball-point pen and the micro- bearing in terms of it to produce；Can use as mill Jie's ball In the manufacture of superfine powder such as nano-powder, can be used for pharmacy such as breaking-wall cell etc., have a extensive future.
Specific embodiment
The present invention is made with reference to specific embodiment further explain.
Embodiment
A kind of silicon nitride ceramics micro-element manufacturing technology proposed by the present invention, including design of material/formula, shaping And biscuit densification and three parts of sintering technology；Specifically include following steps：
S1, preparation production material：The main powder of ceramics, sintering aid, heterogeneous particles, deaeration agent, deionized water, binding agent, wherein The main powder of ceramics is silicon nitride powder of the phase containing α not less than 92, and free silica is less than 0.2%, and iron and calcium impurities are not more than 100ppm, particle Degree D50 is less than 0.5 micron；Sintering aid be lanthana, yittrium oxide, magnesia, aluminum oxide cerium oxide, strontium oxide strontia, aluminium nitride and One or more in niobium oxide, granularity is nanoscale, and total amount is in 10%WT；Heterogeneous particles are titanium nitride, titanium carbide and nitridation One or more in aluminium, its consumption is the 4%WT of ceramic main powder amount, and granularity is 8 times of ceramic main powder；Binding agent is 2% dense The polyvinyl alcohol of degree；
S2, heterogeneous particles are mixed in deionized water, add deaeration agent to make uniform sizing material and be mixed into ceramic main powder, after stirring Drying, is then comminuted into powders A；
S3, binding agent is added using the powders A obtained by step S2, workpiece needed for being obtained using " rolling Lantern Festival " method, and utilize " modeling The biscuit of ceramics package method of bath " is packaged to it, wherein the biscuit of ceramics package method of " modeling bath " specifically includes two kinds：A, use High molecular polymer coats film in surface of the work as cladding medium with immersion way, and by workpiece liquid is dissolved and be soaked in In colloid, vibrations dispersion removes the bubble of surface of the work, drenches dry after then workpiece is pulled out from liquid state colloid, vibrations dispersion with The mutual adhesion of workpiece is prevented, workpiece is dried in the drying box of 500 DEG C of high temperature, and keep mutual adhesion between workpiece；B, make With high molecular polymer as cladding medium, film is coated in surface of the work, by cladding melting glue with the mode solidified after fusing Workpiece solidified by help of drying, and avoid mutual adhesion between workpiece；The cladding medium is polyvinyl alcohol, polyvinyl alcohol One or more in butyral, polyethylene and polypropylene；The liquid state colloid concentration is higher than the workpiece for compression molding；Institute Melting gum concentration is stated less than the workpiece for compression molding；
S4, the workpiece to completing to encapsulate in step S3 are sintered, and sintering aid are added in sintering process, first by workpiece liter Temperature is arrived to 1750 DEG C, and after insulation 15min 35 DEG C are reduced, and continues to be incubated, and temperature retention time is 2 times of conventional temperature retention time.
Obtained powders A is equally applicable to require high rigidity, high-fracture toughness, high abrasion in the present embodiment step S2 In, the part of big size, obtained final product using traditional forming method shaping；During encapsulation technology in step S3 is equally applicable, it is big The encapsulation of type complex component.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.

Claims (8)

1. a kind of silicon nitride ceramics micro-element manufacturing technology, it is characterised in that the manufacturing technology includes material Design/formula, shaping and biscuit densification and three parts of sintering technology；Specifically include following steps：
S1, preparation production material：The main powder of ceramics, sintering aid, heterogeneous particles, deaeration agent, deionized water, binding agent；
S2, heterogeneous particles are mixed in deionized water, add deaeration agent to make uniform sizing material and be mixed into ceramic main powder, after stirring Drying, is then comminuted into powders A；
S3, binding agent is added using the powders A obtained by step S2, workpiece needed for being obtained using " rolling Lantern Festival " method, and utilize " modeling The biscuit of ceramics package method of bath " is packaged to it；
S4, the workpiece to completing to encapsulate in step S3 are sintered, and sintering aid are added in sintering process, first by workpiece liter Temperature is arrived to 1750～1780 DEG C, and after 10～20min of insulation 30～40 DEG C are reduced, and continues to be incubated, and temperature retention time is for during conventional insulation Between 2 times.
2. a kind of silicon nitride ceramics micro-element manufacturing technology according to claim 1, it is characterised in that the step Ceramic main powder in rapid S1 is silicon nitride powder of the phase containing α not less than 92, and free silica is less than 0.2%, and iron and calcium impurities are not more than 100ppm, granularity D50 is less than 0.5 micron.
3. a kind of silicon nitride ceramics micro-element manufacturing technology according to claim 1, it is characterised in that the step Sintering aid in rapid S1 is in lanthana, yittrium oxide, magnesia, aluminum oxide cerium oxide, strontium oxide strontia, aluminium nitride and niobium oxide One or more, granularity is nanoscale, and total amount is in 8～12%WT.
4. a kind of silicon nitride ceramics micro-element manufacturing technology according to claim 1, it is characterised in that the step Heterogeneous particles in rapid S1 are one or more in titanium nitride, titanium carbide and aluminium nitride, its consumption be ceramic main powder amount 3～ 5%WT, granularity is 5～10 times of ceramic main powder.
5. a kind of silicon nitride ceramics micro-element manufacturing technology according to claim 1, it is characterised in that the step Binding agent in rapid S1 is the polyvinyl alcohol of 0.2～3% concentration.
6. a kind of silicon nitride ceramics micro-element manufacturing technology according to claim 1, it is characterised in that the step In rapid S2 obtained powders A be equally applicable to require in high rigidity, high-fracture toughness, high abrasion, the part of big size, adopt Obtained final product with traditional forming method shaping.
7. a kind of silicon nitride ceramics micro-element manufacturing technology according to claim 1, it is characterised in that the step The biscuit of ceramics package method of " modeling bath " in rapid S3 specifically includes two kinds：A, using high molecular polymer as cladding medium, use Immersion way coats film in surface of the work, and workpiece is dissolved and is soaked in liquid state colloid, and vibrations dispersion removes surface of the work Bubble, drench dry after then workpiece is pulled out from liquid state colloid, vibrations dispersion to prevent the mutual adhesion of workpiece, by workpiece in height It is dried in the drying box of 300～800 DEG C of temperature, and keeps mutual adhesion between workpiece；B, using high molecular polymer as cladding Medium, film is coated in surface of the work with the mode solidified after fusing, and the workpiece of cladding melting glue is solidified by help of drying, And avoid mutual adhesion between workpiece；The cladding medium is in polyvinyl alcohol, polyvinyl butyral resin, polyethylene and polypropylene One or more；The liquid state colloid concentration is higher than the workpiece for compression molding；The melting gum concentration is less than for mould Molded workpiece.
8. a kind of silicon nitride ceramics micro-element manufacturing technology according to claim 1, it is characterised in that the step During encapsulation technology in rapid S3 is equally applicable, the encapsulation of large complicated part.
CN201710009608.4A 2017-01-06 2017-01-06 Production and manufacturing technology of silicon nitride ceramic tiny component Pending CN106631041A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107673765A (en) * 2017-09-18 2018-02-09 上海大学 The preparation method of silicon nitride ceramics
CN113735594A (en) * 2021-08-25 2021-12-03 北京科技大学 Method for preparing high-thermal-conductivity silicon nitride ceramic through hot-pressing sintering
CN115321988A (en) * 2021-05-11 2022-11-11 宁波银瓷新材料有限公司 Fiber-reinforced silicon nitride ceramic composite material and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613202A (en) * 2009-07-21 2009-12-30 上海材料研究所 Adopt glass encapsulating heat and other static pressuring processes to prepare the method for silicon nitride ceramic ball
CN103011834A (en) * 2012-11-28 2013-04-03 大连大友高技术陶瓷有限公司 Preparation method for high-compactness composite ceramic
CN104098336A (en) * 2013-04-15 2014-10-15 中国科学院上海硅酸盐研究所 Method for preparing high-thermal-conductivity high-strength silicon nitride ceramic
CN104529470A (en) * 2014-12-08 2015-04-22 北京中材人工晶体研究院有限公司 Silicon nitride powder material preparation method
CN105016738A (en) * 2014-04-30 2015-11-04 广东工业大学 Silicon nitride ceramic and preparation method thereof
CN105819865A (en) * 2016-03-08 2016-08-03 江苏金盛陶瓷科技有限公司 High heat conduction silicon nitride material and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613202A (en) * 2009-07-21 2009-12-30 上海材料研究所 Adopt glass encapsulating heat and other static pressuring processes to prepare the method for silicon nitride ceramic ball
CN103011834A (en) * 2012-11-28 2013-04-03 大连大友高技术陶瓷有限公司 Preparation method for high-compactness composite ceramic
CN104098336A (en) * 2013-04-15 2014-10-15 中国科学院上海硅酸盐研究所 Method for preparing high-thermal-conductivity high-strength silicon nitride ceramic
CN105016738A (en) * 2014-04-30 2015-11-04 广东工业大学 Silicon nitride ceramic and preparation method thereof
CN104529470A (en) * 2014-12-08 2015-04-22 北京中材人工晶体研究院有限公司 Silicon nitride powder material preparation method
CN105819865A (en) * 2016-03-08 2016-08-03 江苏金盛陶瓷科技有限公司 High heat conduction silicon nitride material and preparation method thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
吴玉程: "《工程材料基础》", 31 December 2014, 合肥工业大学出版社 *
林彬荫: "《耐火材料原料》", 28 February 2015, 冶金工业出版社 *
电气电子绝缘技术手册编辑委员会: "《电气电子绝缘技术手册》", 31 January 2008, 机械工业出版社 *
陈华辉: "《耐磨材料应用手册》", 31 October 2012, 机械工业出版社 *
陈照锋: "《产品造型设计材料与工艺》", 29 February 2016, 西安电子科技大学出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107673765A (en) * 2017-09-18 2018-02-09 上海大学 The preparation method of silicon nitride ceramics
CN115321988A (en) * 2021-05-11 2022-11-11 宁波银瓷新材料有限公司 Fiber-reinforced silicon nitride ceramic composite material and preparation method thereof
CN113735594A (en) * 2021-08-25 2021-12-03 北京科技大学 Method for preparing high-thermal-conductivity silicon nitride ceramic through hot-pressing sintering

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Application publication date: 20170510