CN102557652A - Preparation method for special silicon nitride ceramic compounded by cerium oxide - Google Patents

Preparation method for special silicon nitride ceramic compounded by cerium oxide Download PDF

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Publication number
CN102557652A
CN102557652A CN201010620784XA CN201010620784A CN102557652A CN 102557652 A CN102557652 A CN 102557652A CN 201010620784X A CN201010620784X A CN 201010620784XA CN 201010620784 A CN201010620784 A CN 201010620784A CN 102557652 A CN102557652 A CN 102557652A
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China
Prior art keywords
silicon nitride
cerium oxide
preparation
nitride ceramics
oxide composite
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Pending
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CN201010620784XA
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Chinese (zh)
Inventor
陈海
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SUZHOU ZHONGGAO NEW MATERIAL TECHNOLOGY CO LTD
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SUZHOU ZHONGGAO NEW MATERIAL TECHNOLOGY CO LTD
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Priority to CN201010620784XA priority Critical patent/CN102557652A/en
Publication of CN102557652A publication Critical patent/CN102557652A/en
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Abstract

The invention relates to the technical field of ceramic material, in particular to a method for producing high-performance silicon nitride (Si3N4) ceramic via pressureless sintering by using cerium oxide (Ce2O3) as an additive. The silicon nitride ceramic comprises the following components with the following contents in percentage by mass: 8-15% of cerium oxide, and 85-92% of silicon nitride. The invention is aimed at overcoming the shortages in the prior art, and providing a method for producing high-performance silicon nitride ceramic via pressureless sintering by using cerium oxide as an additive, and the method can be widely used for preparing components and parts in the fields of chemical industry, machinery, metallurgy, aerospace etc.

Description

The preparation method of cerium oxide composite nitride implanting special silicon nitride ceramics
[technical field]
The present invention relates to a kind of technical field of ceramic material, specifically is a kind of cerium oxide (Ce 2O 3) as additive pressureless sintering production high-performance silicon nitride (Si 3N 4) ceramic method.
[background technology]
Silicon nitride ceramics has excellent mechanical behavior under high temperature, is acknowledged as one of the most rising high temperature resistant structure ceramics.Silicon nitride is as a kind of covalent linkage platform thing, and spread coefficient is little, does not have fusing point, decomposes ammonification and silicon about 2173K, is difficult to sintering.Common silicon nitride ceramics respond sintering and hot pressed sintering, the reaction sintering density is poor, poor mechanical property, though hot pressed sintering density is high, mechanical property is good, cost is higher, is difficult to scale operation.And pressureless sintering falls between, because silicon nitride ceramics is the covalent linkage compound, and the pressureless sintering difficulty, the density that improves the pressureless sintering silicon nitride ceramics becomes the research focus, adds rare earth oxide usually as sintering aid, like iridium oxide.But the cost of iridium oxide is higher, and is unfavorable for the application of silicon nitride.We select for use cerium oxide as sintered density and the mechanical property of additive to improve silicon nitride for this reason.
[summary of the invention]
The objective of the invention is to overcome the deficiency of prior art, the method for a kind of cerium oxide as additive pressureless sintering production high-performance silicon nitride ceramics is provided.Working method of the present invention is simple, and cost is low, is prone to realize industrialization production; The silicon nitride ceramics that cerium oxide of the present invention is produced as additive pressureless sintering has the density height, the characteristics that mechanical property is good.
The present invention realizes through following technical scheme:
The silicon nitride ceramics that cerium oxide involved in the present invention is produced as additive pressureless sintering, component and mass percentage content are: cerium oxide 8%~15%, silicon nitride 85%~92%.
5~7 microns of described cerium oxide granularities, 0.4~0.7 micron of silicon nitride granularity.
The silicon nitride ceramics method that cerium oxide involved in the present invention is produced as additive pressureless sintering comprises the steps:
Step 1 takes by weighing cerium oxide and silicon nitride ceramics powder respectively, in planetary ball mill, changes mixing 2 hours with PM 270~330; Dispersion medium is an absolute ethyl alcohol; 60 ℃ of oven dry, the time is 2~3 hours subsequently, cerium oxide that obtains mixing and silicon nitride ceramics mixed powder;
Step 2 at 75~100Mpa forming under the pressure, forms biscuit with the mixed powder of step 1;
Step 3, with the biscuit in the step 2 in vacuum carbon tube furnace under nitrogen protection, under 1400~1550 ℃ of temperature, be incubated 12~18 hours.
Step 4 is taken out the silicon nitride ceramics that burns till in the step 3 detection volume density and mechanical property.
In the step 1, the weight percent of said cerium oxide is 8%~15%, and the weight percent of silicon nitride is 85%~92%.
In the step 1, α-Si in the said silicon nitride 3N 4Content is greater than 90%.
In the step 1, Ce in the said cerium oxide 2O 3Content is greater than 98%.
In the step 3, said nitrogen gas pressure is 1~2 normal atmosphere.
In the step 4, said mechanical property is a folding strength.
Among the present invention, described cerium oxide plays the effect of sintering aid, under 1400~1550 ℃ of high temperature sintering conditions, forms liquid phase, makes the silicon nitride ceramics densification.
The present invention has following beneficial effect: the silicon nitride ceramics compactness extent is high, and mechanical property is good, satisfies the actual needs that use.This preparation method is simple, and cost is low, is prone to realize industrialization production.
[embodiment]
Below in conjunction with embodiment the present invention is described further.Production technology of the present invention is to implement easily to this professional people.Present embodiment provided detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment
Cerium oxide is Ganzhou Jiarun novel material ltd, and silicon nitride powder is the M11 powder that German Starck company produces.Take by weighing 8% cerium oxide and 92% silicon nitride powder respectively according to weight percent.
Above-mentioned two kinds of powder (QM-3SP2 of Nanjing Univ. Instrument Factory type) in planetary ball mill are mixed, and rotating speed 300 changes 1.5 hours time.With the forming under the pressure of powder mix, biscuit (the flourish electric furnace ZT-40-20 of ltd of Shanghai occasion type) 1450 ℃ in vacuum carbon tube furnace is incubated 16 hours at 80Mpa.
The volume density of the silicon nitride ceramics that present embodiment obtains is 3.26g/cm 3, folding strength is 671Mpa.

Claims (7)

1. the silicon nitride ceramics produced as additive pressureless sintering of the related cerium oxide of the preparation method of cerium oxide composite nitride implanting special silicon nitride ceramics, component and mass percentage content are: cerium oxide 8%~15%, silicon nitride 85%~92%.5~7 microns of described cerium oxide granularities, 0.4~0.7 micron of silicon nitride granularity.
2. the silicon nitride ceramics method that the related cerium oxide of the preparation method of cerium oxide composite nitride implanting special silicon nitride ceramics according to claim 1 is produced as additive pressureless sintering comprises the steps:
Step 1 takes by weighing cerium oxide and silicon nitride ceramics powder respectively, in planetary ball mill, changes mixing 2 hours with PM 270~330; Dispersion medium is an absolute ethyl alcohol; 60 ℃ of oven dry, the time is 2~3 hours subsequently, cerium oxide that obtains mixing and silicon nitride ceramics mixed powder;
Step 2 at 75~100Mpa forming under the pressure, forms biscuit with the mixed powder of step 1;
Step 3, with the biscuit in the step 2 in vacuum carbon tube furnace under nitrogen protection, under 1400~1550 ℃ of temperature, be incubated 12~18 hours.
Step 4 is taken out the silicon nitride ceramics that burns till in the step 3 detection volume density and mechanical property.
3. the preparation method of cerium oxide composite nitride implanting special silicon nitride ceramics according to claim 2, the weight percent that it is characterized in that cerium oxide described in the step 1 is 8%~15%, the weight percent of silicon nitride is 85%~92%.
4. the preparation method of cerium oxide composite nitride implanting special silicon nitride ceramics according to claim 2 is characterized in that in the step 1, α-Si in the said silicon nitride 3N 4Content is greater than 90%.
5. the preparation method of cerium oxide composite nitride implanting special silicon nitride ceramics according to claim 2 is characterized in that in the step 1, Ce in the said cerium oxide 2O 3Content is greater than 98%.
6. the preparation method of cerium oxide composite nitride implanting special silicon nitride ceramics according to claim 2 is characterized in that in the step 3, and said nitrogen gas pressure is 1~2 normal atmosphere.
7. the preparation method of cerium oxide composite nitride implanting special silicon nitride ceramics according to claim 2 is characterized in that in the step 4, and said mechanical property is a folding strength.
CN201010620784XA 2010-12-29 2010-12-29 Preparation method for special silicon nitride ceramic compounded by cerium oxide Pending CN102557652A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103319181A (en) * 2013-06-18 2013-09-25 上海中耐高温材料有限公司 Method for producing low-cost silicon nitride ceramic
CN104370536A (en) * 2014-10-28 2015-02-25 倪娟形 Special toughened high-temperature-resistant ceramic for fuel engine cylinder liners and preparation method thereof
CN106810264A (en) * 2015-11-27 2017-06-09 衡阳凯新特种材料科技有限公司 A kind of preparation method of silicon nitride ceramics

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103319181A (en) * 2013-06-18 2013-09-25 上海中耐高温材料有限公司 Method for producing low-cost silicon nitride ceramic
CN104370536A (en) * 2014-10-28 2015-02-25 倪娟形 Special toughened high-temperature-resistant ceramic for fuel engine cylinder liners and preparation method thereof
CN106810264A (en) * 2015-11-27 2017-06-09 衡阳凯新特种材料科技有限公司 A kind of preparation method of silicon nitride ceramics

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Application publication date: 20120711