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CN101402449A - Process for producing zirconium nitride-silicon nitride composite powder - Google Patents

Process for producing zirconium nitride-silicon nitride composite powder Download PDF

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Publication number
CN101402449A
CN101402449A CNA2008100120807A CN200810012080A CN101402449A CN 101402449 A CN101402449 A CN 101402449A CN A2008100120807 A CNA2008100120807 A CN A2008100120807A CN 200810012080 A CN200810012080 A CN 200810012080A CN 101402449 A CN101402449 A CN 101402449A
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composite powder
silicon nitride
powder body
zirconium nitride
raw materials
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马北越
于景坤
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Abstract

The invention belongs to a technology for preparing a composite powder body and relates to a method for preparing zirconium nitride-silicon nitride composite powder body. The method comprises the following steps: minerals and industrial wastes containing ZrO2 and SiO2 and a carbonous material are used as raw materials; and by adjusting the mixture ratio of the raw materials, heating temperature, heat insulation time, gas flow and other parameters, the zirconium nitride-silicon nitride composite powder body is synthesized in a high-temperature atmosphere furnace by a carbothermal nitridation method. The method has the advantages of simple preparation process, low prices of raw materials, and good performance of the synthesized composition powder body.

Description

The preparation method of zirconium nitride-silicon nitride composite powder
Technical field:
The invention belongs to the composite granule technology of preparing, is to contain ZrO specifically 2, SiO 2Mineral and trade waste and carbonaceous material etc. be raw material, by the technology of the synthetic zirconium nitride-silicon nitride composite powder of carbothermal reduction-nitridation method.
Background technology:
Because zirconium nitride has high-melting-point, high strength, high tenacity and advantages of good abrasion and low-temperature superconducting performance, make it be widely used in fields such as machinery and electronics.The good in oxidation resistance of silicon nitride, intensity and hardness height are widely used as high temperature resistant, wear-resistant component, high speed cutting tool and radome etc., and its Application Areas relates to industries such as pottery, machinery, chemical industry, electronics and military project.Particularly use the matrix material of above-mentioned two kinds of feedstock production to have better thermal shock resistance, anti-scour property and hot strength and toughness.But in the process of preparation matrix material, the normal existence introduces thing and disperses in mutually inadequately evenly and super-fine powder is introduced problems such as price lattice costliness at base, makes the price rising of zirconium nitride-silicon nitride composite powder goods, improved the production cost of goods.
Summary of the invention:
The present invention is to contain ZrO 2, SiO 2Mineral or industrial solid castoff and carbonaceous material be raw material, by adjusting parameters such as proportioning raw materials, Heating temperature, soaking time and gas flow, utilize carbothermal reduction-nitridation method synthetic at an easy rate zirconium nitride-silicon nitride composite powder in high-temperature atmosphere furnace.Its advantage is that preparation technology is simple, raw materials used low price, and synthetic composite granule performance is good.
Description of drawings:
The invention will be further described as example to use zircon and carbon dust raw material below in conjunction with accompanying drawing:
Fig. 1 is p N 2 = 0.1 MPa ZrO under the condition 2-SiO 2-C-N 2The equilibrium diagram of system.(a) is carbon dust and silicon-dioxide generate silicon oxynitride under nitrogen atmosphere reaction among Fig. 1, that is, and and 2SiO 2(s)+3C (s)+N 2(g)=Si 2N 2O (s)+3CO (g); (b) is carbon dust and silicon-dioxide generate silicon nitride under nitrogen atmosphere reaction among Fig. 1, that is, and and 3SiO 2(s)+6C (s)+2N 2(g)=Si 3N 4(s)+6CO (g); (c) be zirconium white and carbon dust generate zirconium nitride under nitrogen atmosphere reaction, 2ZrO 2(s)+4C (s)+N 2(g)=2ZrN (s)+4CO (g).Regional A is ZrO among Fig. 1 2(s), SiO 2(s) and C (s) coexisting region; Area B ZrO 2(s), Si 2N 2O (s) and C (s) coexisting region; Zone C is ZrO 2(s), Si 3N 4(s) and C (s) coexisting region; Region D is ZrN (s), Si 3N 4(s) and C (s) coexisting region.
ZrSiO 4Or ZrO2,SiO 2In the heating process following reaction may take place with C under nitrogen atmosphere:
ZrSiO 4(s)=ZrO 2(s)+SiO 2(s)                 (1)
SiO 2(s)+C(s)=SiO(g)+CO(g) (2)
SiO(g)+2C(s)=SiC(s)+CO(g) (3)
SiO(g)+C(s)+N 2(g)=Si 2N 2O(s)+CO(g) (4)
Si 2N 2O(s)+SiO 2(s)+3C(s)+N 2(g)=Si 3N 4(s)+3CO(g) (5)
3SiO(g)+3C(s)+2N 2(g)=Si 3N 4(s)+3CO(g) (6)
3SiO 2(s)+6C(s)+2N 2(g)=Si 3N 4(s)+6CO(g) (7)
ZrO 2(s)+C(s)=ZrO(g)+CO(g) (8)
2ZrO(g)+2C(s)+N 2(g)=2ZrN(s)+2CO(g) (9)
2ZrO 2(s)+4C(s)+N 2(g)=2ZrN(s)+4CO(g) (10)
3ZrSiO 4(s)+6C(s)+2N 2(g)=3ZrO 2(s)+Si 3N 4(s)+6CO(g) (11)
6ZrSiO 4(s)+24C(s)+7N 2(g)=6ZrN(s)+2Si 3N 4(s)+24CO(g)?(12)
By formula (1)~(12) as can be known, this ZrO 2-SiO 2-C-N 2Reaction process complexity in the system if control bad Heating temperature, furnace atmosphere and carbon add-on etc., SiC and Si may occur in the product 2N 2Impurity phases such as O.
Therefore,, need to select suitable processing parameter if will obtain zirconium nitride-silicon nitride composite powder, as: raw material composition, Heating temperature and soaking time etc.
Embodiment:
Embodiment 1:
Table 1 is during for fixedly soaking time 6h, nitrogen pressure 0.1MPa and nitrogen flow 1.0L/min, and raw material composition (massfraction) and Heating temperature are to the influence of synthetic zirconium nitride-silicon nitride composite powder phase composite under the nitrogen atmosphere.ZS represents ZrSiO in the table 1 4Phase, Z represents ZrO 2Phase, S represents SiO 2Phase, SO represents Si 2N 2The O phase, SN represents Si 3N 4Phase, SC represents the SiC phase, and ZN represents the ZrN phase, and C represents the carbon phase.
Table 1 raw material composition and Heating temperature are to the influence of product phase composite
Figure A20081001208000041
Embodiment 2:
Table 2 is that fixedly raw material is formed (ZrSiO 4/ C=100/40), when nitrogen pressure 0.10MPa and nitrogen flow 1.0L/min, Heating temperature and soaking time are to the influence of synthetic zirconium nitride-silicon nitride composite powder phase composite.ZS represents ZrSiO in the table 2 4Phase, Z represents ZrO 2Phase, S represents SiO 2Phase, SO represents Si 2N 2The O phase, SN represents Si 3N 4Phase, SC represents the SiC phase, and ZN represents the ZrN phase, and C represents the carbon phase.
Table 2 Heating temperature and soaking time are to the influence of product phase composite
Figure A20081001208000051
By table 1 and table 2 as can be known, by the control proportioning raw materials, factors such as Heating temperature and soaking time can successfully be prepared zirconium nitride-silicon nitride composite powder.

Claims (1)

1. the preparation method of a zirconium nitride-silicon nitride composite powder is characterized in that to contain ZrO 2, SiO 2Natural mineral and trade waste and carbonaceous material etc. be raw material, be equipped with zirconium nitride-silicon nitride composite powder by the carbothermal reduction-nitridation legal system.
CNA2008100120807A 2008-06-30 2008-06-30 Process for producing zirconium nitride-silicon nitride composite powder Pending CN101402449A (en)

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Application Number Priority Date Filing Date Title
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104098346A (en) * 2013-04-02 2014-10-15 中国科学院宁波材料技术与工程研究所 Preparation method of golden yellow zirconium nitride coating on base surface
CN107459356A (en) * 2017-09-14 2017-12-12 北京大学 A kind of preparation method of silicon nitride composite diphase material
CN107777673A (en) * 2017-11-13 2018-03-09 武汉科技大学 A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof
CN109923062A (en) * 2016-09-29 2019-06-21 三菱综合材料电子化成株式会社 Zirconium nitride powder and its manufacturing method
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

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104098346A (en) * 2013-04-02 2014-10-15 中国科学院宁波材料技术与工程研究所 Preparation method of golden yellow zirconium nitride coating on base surface
CN109923062A (en) * 2016-09-29 2019-06-21 三菱综合材料电子化成株式会社 Zirconium nitride powder and its manufacturing method
CN109923062B (en) * 2016-09-29 2023-04-11 三菱综合材料电子化成株式会社 Zirconium nitride powder and method for producing same
CN107459356A (en) * 2017-09-14 2017-12-12 北京大学 A kind of preparation method of silicon nitride composite diphase material
CN107777673A (en) * 2017-11-13 2018-03-09 武汉科技大学 A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof
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

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