CN105541341A - Method for preparing high-compactness silicon nitride ceramic by adding composite additives - Google Patents

Method for preparing high-compactness silicon nitride ceramic by adding composite additives Download PDF

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CN105541341A
CN105541341A CN201610017072.6A CN201610017072A CN105541341A CN 105541341 A CN105541341 A CN 105541341A CN 201610017072 A CN201610017072 A CN 201610017072A CN 105541341 A CN105541341 A CN 105541341A
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silicon nitride
compactness
oxide
nitride ceramics
preparing high
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张红冉
刘久明
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Hebei Corefra Silicon Nitride Material Co Ltd
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Hebei Corefra Silicon Nitride Material Co Ltd
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Abstract

The invention relates to the technical field of ceramic materials, in particular to a method for preparing high-compactness silicon nitride ceramic by adding composite additives. Auxiliary materials are prepared from, by mass, 70-90% of silicon nitride, 4-15% of metal oxide, 3-12% of rare earth oxide, 0.5-3% of a binding agent, 0-8% of silicon dioxide, 0-3% of cesium fluoride, 0-1% of a dispersing agent and 0-0.15% of a defoaming agent. The raw materials, grinding medium balls and dispersing media are mixed and dried and then are screened, and granulation powder is obtained; the granulation powder is placed in a mold to be pressed into green bodies, the green bodies are placed in a sintering furnace after being dried, and the high-compactness silicon nitride ceramic is obtained through sintering under nitrogen protection. By mans of the preparation method, the silicon nitride ceramic can be sintered at normal pressure, operation is easy, convenient and feasible, cost is low, and the preparation method is suitable for industrial production. Besides, the silicon nitride ceramic obtained through sintering is good in compactness and high in bending strength and can be widely used as structural element materials in the fields of machinery, metallurgy, aerospace and the like.

Description

A kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics
Technical field
The invention belongs to technical field of ceramic material, be specifically related to a kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics.
Background technology
Silicon nitride ceramics is as a kind of high-temperature structural material of excellence, have that physical strength is high, high temperature resistant, good thermal shock, density are little, corrosion-resistant, anti-oxidant, self-lubricating plurality of advantages, day by day be subject to people's attention, be now applied in the fields such as mechanical workout, aerospace, military affairs, life.High-speed cutting, the cutting of large impact power and screw thread process can be carried out with the cutter that silicon nitride is produced.Silicon nitride bearing can at high temperature, burn at a high speed, run well under the severe condition such as unlubricated.Install the automobile of silicon nitride electrothermal plug, when the winter starting of cold, glow plug only needs preheating ten second.The turibine rotor rotational inertia made with silicon nitride can reduce 40%.As can be seen here, silicon nitride ceramics has the performance of many excellences in all trades and professions.Believe along with silicon nitride ceramic powder produce, the improving constantly of shaping, sintering technology, silicon nitride ceramics will obtain and apply more widely.
Silicon nitride sintering processing conventional at present has HIP sintering, reaction sintering, normal pressure-sintered, gas pressure sintering.Wherein HIP sintering pressure is high, and equipment is complicated, and manufacturing technique requirent is tight, and production efficiency is lower, and cost is high.The silicon nitride ceramics compactness that reaction sintering is produced is poor, and void content is high, finally has remaining unreacted reactant in goods.Normal pressure-sintered cost is low, and goods, the efficiency that can sinter various complicated shape are high, and from practicality, the normal pressure-sintered of silicon nitride is one of Main way of research.Normal pressure-sintered general employing liquid phase sintering mode.In order to prepare the silicon nitride ceramics of high compactness, generally add sintering aid, make its at high temperature with the SiO of silicon nitride surface 2reaction forms liquid phase, by rearrangement, the dissolving-precipitation acceleration of sintering densification of particle.Conventional sintering aid has Al 2o 3, MgO, ZrO 2, SiO 2, Y 2o 3, La 2o 3, Sm 2o 3, Lu 2o 3, CeO 2, AlPO 4and its composite assistant.We select the composite assistant adding metal oxide and rare earth oxide for this reason, adopt normal atmosphere sintering method to prepare the silicon nitride ceramics of high-compactness.
Summary of the invention
The object of this invention is to provide a kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics.Present method is simple to operate, and facilitate feasible, cost is low, and be applicable to suitability for industrialized production, obtained silicon nitride ceramics compactness is good, and bending strength is high.The technical solution adopted in the present invention is:
Step one: dried raw material is prepared burden by following mass percent: silicon nitride 70 ~ 90%, metal oxide 4 ~ 15%, rare earth oxide 3 ~ 12%, binding agent 0.5 ~ 3%, silicon-dioxide 0 ~ 8%, cesium fluoride 0 ~ 3%, dispersion agent 0 ~ 1%, defoamer 0 ~ 0.15%.Above-mentioned raw materials being put into planetary ball mill adopts wet-mixed evenly to obtain mixed slurry, dries rear mistake 14 ~ 40 mesh sieve obtain preformed pelletizing to slurry;
Step 2: granulation powder described in step one is put into mould and carries out dry-pressing formed, obtain base substrate;
Step 3: put into multifunctional sintering furnace by after body drying described in step 2, is warming up to certain temperature and is incubated, cooling to room temperature with the furnace, obtain the block silicon nitride ceramics of high-compactness after insulation terminates under nitrogen atmosphere protection.
Metal oxide described in step one is one or more in aluminum oxide, magnesium oxide, zirconium white or titanium oxide, rare earth oxide is one or more in yttrium oxide, lanthanum trioxide, cerium oxide or lutecium oxide, binding agent is the one in polyvinyl alcohol, polyvinyl butyral acetal, polyoxyethylene glycol or resol, ball-milling medium is silicon nitride ball, dispersion medium is deionized water, dispersion agent is ammonium polyacrylate, and defoamer is tbp.
Silicon nitride purity described in step one is not less than 99%, α phase content and is not less than 92%, and meso-position radius is 0.3 ~ 1.2 μm, and the purity of metal oxide is not less than 98%, and rare earth oxide purity is not less than 98%, and the alcoholysis degree of polyvinyl alcohol is not more than 90%.
The rotating speed of the ball mill described in step one is 200r/min ~ 600r/min, and Ball-milling Time is 2 ~ 6h.
Dry-pressing formed pressure described in step 2 is 10 ~ 30MPa, and the dwell time is 30 ~ 120s.
Nitrogen atmosphere pressure described in step 3 is 0.2 ~ 2 normal atmosphere, and holding temperature is 1600 DEG C ~ 1800 DEG C, and soaking time is 1 ~ 2h.
The present invention take silicon nitride as main raw material, add a certain proportion of metal oxide and rare earth oxide as sintering aid, these sintering aids when exceeding its eutectic point temperature and the silicon-dioxide of silicon nitride surface trace form liquid phase, particle realizes tightly packed by carrying out rearrangement in this liquid phase.After cooling, liquid phase is that glassy phase is stayed in sintered compact, only has silicon nitride phase in sintered compact.
Preparation method of the present invention with metal oxide-rare-earth oxidation objects system for sintering aid achieves sintered silicon nitride ceramic under normal pressure, simple, convenient feasible, be applicable to suitability for industrialized production.Simultaneously the silicon nitride ceramics compactness prepared of the method is good, and bending strength is high, meets the actual needs used.
Embodiment
Below in conjunction with case study on implementation, the present invention is described further, but be not only confined to embodiment.
Embodiment 1
1g polyvinyl alcohol (alcoholysis degree is 88%) is made into the polyvinyl alcohol solution of 10mL by heating, stirring.Silicon nitride 82g (D50=0.45 μm, α=94.2%), aluminum oxide 10g, yttrium oxide 8g, tbp solution 0.04g, deionized water 90mL, above-mentioned polyvinyl alcohol solution 10mL are put into ball grinder.Ball grinder is put into planetary ball mill mix, rotating speed 580r/min, Ball-milling Time 2h.
Cross 18 mesh sieve after the above-mentioned slurry mixed being put into loft drier oven dry and obtain pelletizing.Pelletizing is placed in mould dry-pressing formed, forming pressure is 15MPa, and the dwell time is 60s, obtains treating sintering briquette body.Put into multifunctional sintering furnace by after body drying, at 1730 DEG C, be incubated 1h.All the time using 0.6 atmospheric nitrogen as protection of inert gas atmosphere in intensification, insulation, temperature-fall period.
The density of the silicon nitride ceramics that the present embodiment obtains reaches 98.7% of theoretical density, and bending strength is 928MPa.
Embodiment 2
Silicon nitride 81g (D50=0.55 μm, α=94.2%), aluminum oxide 3g, yttrium oxide powder 5g, lanthanum trioxide 5g, silicon-dioxide 6g, polyvinyl alcohol 1g, deionized water 100mL are put into ball grinder and carry out ball milling, rotating speed 580r/min, Ball-milling Time 6h.Cross 18 mesh sieve after being dried by uniform for above-mentioned ball milling slurry, obtain granulation powder.Pelletizing is placed in mould to carry out dry-pressing formed, and forming pressure is 20MPa, and dwell time 60s obtains pre-burning base substrate.Be placed in multifunctional sintering furnace by body drying and sinter, sintering temperature is 1650 DEG C, and soaking time is 1h.All the time using 2 atmospheric nitrogen as protection of inert gas atmosphere in whole sintering process.
The density of the silicon nitride ceramics that the present embodiment obtains reaches 97% of theoretical density, and bending strength is 830MPa.
Embodiment 3
Silicon nitride 88g (D50=0.95 μm, α=92.5%), aluminum oxide 3g, magnesium oxide 5g, yttrium oxide 4g, polyglycol solution 40mL (concentration 5%), ammonium polyacrylate 0.8g, tbp solution 0.06g, deionized water 45mL are put in ball grinder and carry out wet-milling, rotating speed 580r/min, Ball-milling Time 4h.Solution after mixing is dried, crosses 40 mesh sieves and carry out granulation.Pelletizing is put into mould dry-pressing formed, forming pressure 25MPa, dwell time 100s, obtains base substrate.Base substrate is incubated 2h at 1700 DEG C and obtains silicon nitride ceramics, nitrogen protection atmosphere pressure is 0.4 normal atmosphere.
The silicon nitride ceramics relative density that the present embodiment obtains reaches 98%, and ablation rate is 0.6%, and bending strength is 890MPa.
Embodiment 4
Alpha-silicon nitride powders 87g (D50=0.89 μm, α=93%), magnesium oxide powder 3g, cerium oxide 3g, lutecium oxide powder 3g, cesium fluoride 4g, polyvinyl alcohol solution 20mL (concentration is 10%), deionized water 80mL are put into ball grinder ball milling, rotating speed 580r/min, Ball-milling Time 4h.Cross 40 mesh sieves after being dried by mixing solutions, obtain pelletizing.Undertaken dry-pressing formed by pelletizing, pressure is 25MPa, pressurize 120s.Base substrate is placed in multifunctional sintering furnace sinter, sintering temperature is 1750 DEG C, and insulation 2h, nitrogen pressure is 0.5 normal atmosphere.
The silicon nitride ceramics density that the present embodiment obtains reaches 99% of theoretical density, and bending strength is 940MPa.

Claims (7)

1. add the method that composite assistant prepares high-compactness silicon nitride ceramics, it is characterized in that, comprise the following steps:
Step one: dried raw material is weighed by following mass percent: silicon nitride 70 ~ 90%, metal oxide 4 ~ 15%, rare earth oxide 3 ~ 12%, binding agent 0.5 ~ 3%, silicon-dioxide 0 ~ 8%, cesium fluoride 0 ~ 3%, dispersion agent 0 ~ 1%, defoamer 0 ~ 0.15%, puts into planetary ball mill and adopts wet-mixed evenly to obtain mixed slurry by above-mentioned raw materials, dry rear mistake 14 ~ 40 mesh sieve obtain preformed pelletizing to slurry;
Step 2: granulation powder described in step one is put into mould and carries out dry-pressing formed, obtain base substrate;
Step 3: put into multifunctional sintering furnace by after the body drying in step 2, is warming up to certain temperature and is incubated, cooling to room temperature with the furnace, obtain the block silicon nitride ceramics of high-compactness after insulation terminates under nitrogen atmosphere protection.
2. according to a kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics according to claim 1, its feature exists, metal oxide described in step one is one or more in aluminum oxide, magnesium oxide, zirconium white or titanium oxide, rare earth oxide is one or more in yttrium oxide, lanthanum trioxide, cerium oxide or lutecium oxide, binding agent is the one in polyvinyl alcohol, polyvinyl butyral acetal, polyoxyethylene glycol or resol, ball-milling medium is silicon nitride ball, dispersion medium is deionized water, dispersion agent is ammonium polyacrylate, and defoamer is tbp.
3., according to a kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics according to claim 2, it is characterized in that, the alcoholysis degree of described polyvinyl alcohol is not more than 90%.
4. according to a kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics according to claim 1, it is characterized in that, described silicon nitride purity is not less than 99%, α phase content is not less than 92%, meso-position radius is 0.3 ~ 1.2 μm, the purity of metal oxide is not less than 98%, and rare earth oxide purity is not less than 98%.
5. according to a kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics according to claim 1, it is characterized in that, the rotating speed of ball mill described in step one is 200r/min ~ 600r/min, and Ball-milling Time is 2 ~ 6h.
6., according to a kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics according to claim 1, it is characterized in that, dry-pressing formed pressure described in step 2 is 10 ~ 30MPa, and the dwell time is 30 ~ 120s.
7. according to a kind of method of adding composite assistant and preparing high-compactness silicon nitride ceramics according to claim 1; it is characterized in that; nitrogen protection atmosphere described in step 3 is 0.2 ~ 2 normal atmosphere, and holding temperature is 1600 DEG C ~ 1800 DEG C, and soaking time is 1 ~ 2h.
CN201610017072.6A 2016-01-12 2016-01-12 Method for preparing high-compactness silicon nitride ceramic by adding composite additives Pending CN105541341A (en)

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CN105908106A (en) * 2016-06-23 2016-08-31 王莹 High-strength and wear-resistant oxide-based metal ceramic bearing and preparation method thereof
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CN106083068A (en) * 2016-06-15 2016-11-09 中国科学院上海硅酸盐研究所 A kind of preparation method of water base pelletize the directly silicon nitride ceramics of cold isostatic compaction
CN106086723A (en) * 2016-06-23 2016-11-09 王莹 A kind of high-strength wearable boride-base cerment bearing and preparation method thereof
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CN106673668A (en) * 2016-12-14 2017-05-17 宜兴市华井科技有限公司 Silicon nitride ceramic and preparation method thereof
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CN106747471A (en) * 2017-01-19 2017-05-31 新德隆特种陶瓷（大连）有限公司 A kind of fabric dividing cutter
CN106747469A (en) * 2016-12-27 2017-05-31 郑州源冉生物技术有限公司 A kind of high-performance silicon nitride ceramic material and preparation method thereof
CN107651965A (en) * 2017-11-15 2018-02-02 石家庄铁道大学 A kind of silicon nitride ceramic material and preparation method thereof
CN107879747A (en) * 2017-11-28 2018-04-06 上海骏宇陶塑制品有限公司 A kind of silicon nitride ceramics and preparation method thereof
CN109305816A (en) * 2017-07-27 2019-02-05 中国科学院上海硅酸盐研究所 A kind of normal pressure-sintered method for preparing high heat conductivity silicon nitride ceramics
CN109987943A (en) * 2019-04-04 2019-07-09 天津大学 A kind of preparation method of beta-silicon nitride powder
CN110922193A (en) * 2019-12-20 2020-03-27 上海步进精密陶瓷有限公司 Preparation method of silicon nitride ceramic ball
CN111302808A (en) * 2018-12-12 2020-06-19 山东工业陶瓷研究设计院有限公司 Wave-transparent high-dielectric ceramic material and preparation method and application thereof
CN111393170A (en) * 2020-03-19 2020-07-10 西安澳秦新材料有限公司 Method for preparing high-density silicon nitride ceramic through multi-factor optimization and prepared silicon nitride ceramic
CN112341206A (en) * 2020-11-05 2021-02-09 衡阳凯新特种材料科技有限公司 Forming method of rare earth praseodymium-holmium-stabilized silicon nitride ceramic
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CN112898029A (en) * 2021-01-30 2021-06-04 埃克诺新材料（大连）有限公司 Preparation method of silicon nitride substrate raw material
CN113135761A (en) * 2021-04-28 2021-07-20 白山市科学技术研究所 Method for preparing silicon nitride ceramic from low-grade diatomite
CN113880591A (en) * 2021-10-28 2022-01-04 深圳市辰昱科技有限公司 Silicon nitride-based ceramic body and method for in-situ self-generating zirconium nitride coating on surface of silicon nitride-based ceramic
CN115340388A (en) * 2022-09-06 2022-11-15 烟台核晶陶瓷新材料有限公司 Preparation method of silicon nitride square brick for mono-like ingot casting and quartz crucible
CN115521152A (en) * 2022-10-09 2022-12-27 苏州艾成科技技术有限公司 Auxiliary agent for sintering silicon nitride
CN116239387A (en) * 2023-02-09 2023-06-09 中国科学院金属研究所 Preparation method of high-strength silicon nitride by using medium/high entropy multi-element rare earth sintering aid
CN116730725A (en) * 2023-06-05 2023-09-12 衡阳凯新特种材料科技有限公司 Silicon nitride composite ceramic material for lift tube, preparation method and application

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CN106747474A (en) * 2017-02-28 2017-05-31 安徽拓吉泰新型陶瓷科技有限公司 The preparation method of high heat conductivity silicon nitride ceramics
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CN109305816A (en) * 2017-07-27 2019-02-05 中国科学院上海硅酸盐研究所 A kind of normal pressure-sintered method for preparing high heat conductivity silicon nitride ceramics
CN109305816B (en) * 2017-07-27 2022-04-05 浙江多面体新材料有限公司 Method for preparing high-thermal-conductivity silicon nitride ceramic by normal-pressure sintering
CN107651965A (en) * 2017-11-15 2018-02-02 石家庄铁道大学 A kind of silicon nitride ceramic material and preparation method thereof
CN107879747A (en) * 2017-11-28 2018-04-06 上海骏宇陶塑制品有限公司 A kind of silicon nitride ceramics and preparation method thereof
CN111302808A (en) * 2018-12-12 2020-06-19 山东工业陶瓷研究设计院有限公司 Wave-transparent high-dielectric ceramic material and preparation method and application thereof
CN109987943A (en) * 2019-04-04 2019-07-09 天津大学 A kind of preparation method of beta-silicon nitride powder
CN110922193A (en) * 2019-12-20 2020-03-27 上海步进精密陶瓷有限公司 Preparation method of silicon nitride ceramic ball
CN111393170A (en) * 2020-03-19 2020-07-10 西安澳秦新材料有限公司 Method for preparing high-density silicon nitride ceramic through multi-factor optimization and prepared silicon nitride ceramic
CN112341206A (en) * 2020-11-05 2021-02-09 衡阳凯新特种材料科技有限公司 Forming method of rare earth praseodymium-holmium-stabilized silicon nitride ceramic
CN112851364A (en) * 2021-01-30 2021-05-28 埃克诺新材料（大连）有限公司 Sintering method of silicon nitride substrate
CN112898029A (en) * 2021-01-30 2021-06-04 埃克诺新材料（大连）有限公司 Preparation method of silicon nitride substrate raw material
CN112851364B (en) * 2021-01-30 2022-11-15 埃克诺新材料（大连）有限公司 Sintering method of silicon nitride substrate
CN113135761A (en) * 2021-04-28 2021-07-20 白山市科学技术研究所 Method for preparing silicon nitride ceramic from low-grade diatomite
CN113880591A (en) * 2021-10-28 2022-01-04 深圳市辰昱科技有限公司 Silicon nitride-based ceramic body and method for in-situ self-generating zirconium nitride coating on surface of silicon nitride-based ceramic
CN115340388A (en) * 2022-09-06 2022-11-15 烟台核晶陶瓷新材料有限公司 Preparation method of silicon nitride square brick for mono-like ingot casting and quartz crucible
CN115521152A (en) * 2022-10-09 2022-12-27 苏州艾成科技技术有限公司 Auxiliary agent for sintering silicon nitride
CN116239387A (en) * 2023-02-09 2023-06-09 中国科学院金属研究所 Preparation method of high-strength silicon nitride by using medium/high entropy multi-element rare earth sintering aid
CN116730725A (en) * 2023-06-05 2023-09-12 衡阳凯新特种材料科技有限公司 Silicon nitride composite ceramic material for lift tube, preparation method and application

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