CN105884375B - A kind of Si3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics - Google Patents

A kind of Si3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics Download PDF

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CN105884375B
CN105884375B CN201610178439.2A CN201610178439A CN105884375B CN 105884375 B CN105884375 B CN 105884375B CN 201610178439 A CN201610178439 A CN 201610178439A CN 105884375 B CN105884375 B CN 105884375B
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composite conductive
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aln
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江涌
吴澜尔
黄新华
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North Minzu University
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Abstract

A kind of Si3N4‑TiZrN2TiN composite conductive ceramics, synthesizing the raw material of the composite conductive ceramic includes：Si3N4、ZrN、TiN、Y2O3、La2O3、AlN；Include Si in the final product of the composite conductive ceramic3N4The solid solution TiZrN of phase, TiN phases and metal nitride2Phase.Wherein, the addition of AlN, which avoids, adds in Al in usual manner2O3Caused volatilization, and adding in AlN can make the surface ratio of final products add in Al2O3It is smooth；Name of the present invention gives a kind of Si3N4‑TiZrN2The lqiuid phase sintering method of TiN composite conductive ceramics.The present invention has the beneficial effect that：1. resistivity is low；The composite conductive ceramic of the present invention is 10 with SX1944 four-point probe test samples resistance‑2Ω cm magnitudes, well below similar product.2. high mechanical strength；The composite conductive ceramic of the present invention is 10kg with load, and the Vickers hardness for the conditioned measurement sample that pressing time is 5s is 14.7GPa；The fracture toughness that sample is calculated using the crack length of indentation hardness four corners extension is 7.8MPa.m0.5Maintain the original intensity of silicon nitride ceramics and hardness.

Description

A kind of Si3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics
Technical field：
The present invention relates to conductivity ceramics technical fields, specifically, are related to a kind of Si3N4-TiZrN2- TiN composite conductings The lqiuid phase sintering method of ceramics.
Background technology：
Silicon nitride (Si3N4) it is a kind of good structural ceramic material of performance, there is light weight, high intensity, high rigidity, height Corrosion resistance etc., can be applied to all trades and professions.There are many method for preparing silicon nitride ceramic material, there is the burnings such as hot pressing, normal pressure, reaction Knot method, wherein normal atmosphere sintering method are simple and practicable, and energy consumption is few.Since silicon nitride is covalent key compound, self-diffusion coefficient is low, Itself it is difficult to be sintered directly into porcelain, therefore often adds in some oxides etc. and be sintered as sintering aid.It is common to have Al2O3、Y2O3、MgO2Deng.These additives form liquid phase in sintering process and promote silicon nitride ceramics densified sintering product, to reach material Expect the requirement of high intensity, high rigidity.
Due to Si3N4The performance of ceramic high intensity itself and high rigidity so that post-production is difficult, often with diamond cutter into Row cutting, but the method processing efficiency of traditional diamond processing is low and expensive.At low cost, efficient electric discharge (electrical fire Flower) processing technology be successfully used for metal product processing, if can be used to process Si3N4It is ceramic then can greatly improve processing efficiency and Processing cost is reduced, but can use the material of electro-discharge machining that there must be certain electric conductivity, resistivity requirement is down to 100Ω· Cm magnitudes and following, but Si3N4Ceramics belong to insulator, and resistivity is about 1015Ω cm magnitudes are impossible to use electric discharge side What method was processed.So it is thought that add in Si with the good material of another electric conductivity3N4In be prepared into Si3N4Base Composite conductive material makes its resistivity drop to the degree that can be used for electrical discharge machining.Make in the patent of CN1272283C With metal Ti and Ta, so that the composite nitride silicon resistivity being finally sintered drops to 100Ω cm magnitudes, have just reached electric discharge The requirement of processing, and its hardness and fracture toughness are poor compared with the silicon nitride ceramics of conductive auxiliary agent is not added.
The content of the invention：
Present invention seek to address that the above problem, a kind of low resistivity, hardness and a kind of excellent Si of fracture toughness are provided3N4- TiZrN2- TiN composite conductive ceramics；Also provide a kind of Si simultaneously3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics.
A kind of Si3N4-TiZrN2- TiN composite conductive ceramics, synthesizing the raw material of the composite conductive ceramic includes： Si3N4、 ZrN、TiN、Y2O3、La2O3、AlN；Include Si in the final product of the composite conductive ceramic3N4Phase, TiN phases and nitride metal The solid solution TiZrN of object2Phase.Wherein, the addition of AlN can avoid adding in Al in usual manner2O3Caused low temperature volatilization, and And adding in AlN can make the surface ratio of final products add in Al2O3It is smooth.
Due to being the composite conductive ceramic material made of sintering process, the thermal expansion system in each material sintering process Number is vital, if coefficient of thermal expansion differs greatly, is unfavorable for being sintered, and can influence density, the hardness of final finished And fracture toughness, therefore selected conductive auxiliary agent is low except wanting resistivity, and coefficient of thermal expansion is also wanted to be differed not with silicon nitride Greatly.In addition, if it is then even more ideal also to have other good mechanical performances concurrently.Titanium nitride and zirconium nitride have high conductivity, the two Resistivity all 10-4Ω cm magnitudes, ZrN are lower (TiN than TiN：2.07×10-4Ω·cm；ZrN：1.4×10-4Ω· cm)；Coefficient of thermal expansion and silicon nitride are about 10 in an order of magnitude-6K-1, and ZrN is closer to silicon nitride (Si3N4：3.64× 10-6K-1；ZrN： 7.3×10-6K-1；TiN：9.35×10-6K-1)；In addition the hardness of TiN, ZrN all in itself is all higher than silicon nitride Very much, wherein, than TiN titanium carbide highers, ZrN plays the role of enhancing toughness as additive the hardness of ZrN.
Preferably, Si3N4∶TiN∶Y2O3∶La2O3: AlN=(9~11): (5.4~6.6): (0.8~1.2): (0.8~ 1.2): (1.3~1.66), the addition of ZrN is 8~15w.t%.
A kind of Si3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics, comprises the following steps：
(1) dispensing mixes：By Si3N4、TiN、Y2O3、La2O3, AlN is with (9~11): (5.4~6.6): (0.8~1.2): (0.8~1.2): the ratio mixing of (1.3~1.66), the addition of ZrN is 8~15w.t%, adds in wine in mortar afterwards It is dry after 1~3h of smooth grinding；Wherein, Si3N4α phases content higher than 70%, purity is higher than 97%, and granularity is 0.6~0.8 μm, TiN granularities are 18~22nm, and ZrN granularities are 16~21nm；
(2) it is molded and is sintered：Dried mixture is put into sintering furnace after isostatic cool pressing again with mold is dry-pressing formed In in N2It being sintered in protective atmosphere, sintering temperature is 1760 ± 25 DEG C, soaking time is set to 1 according to the big I of sample~ 3h。
The present invention has the beneficial effect that：
1. resistivity is low；The composite conductive ceramic of the present invention is 10 with SX1944 four-point probe test samples resistance-2 Ω cm magnitudes, far below similar product.
2. high mechanical strength；The composite conductive ceramic of the present invention is 10kg with load, and pressing time is the conditioned measurement of 5s The Vickers hardness of sample is 14.7GPa；Using indentation hardness four corners extension crack length calculate sample fracture toughness be 7.8MPa.m0.5, reached the original high rigidity of silicon nitride ceramics and high-fracture toughness.
Specific embodiment：
A kind of Si3N4-TiZrN2- TiN composite conductive ceramics, synthesizing the raw material of the composite conductive ceramic includes： Si3N4、 ZrN、TiN、Y2O3、La2O3、AlN；Include Si in the final product of the composite conductive ceramic3N4Phase, TiN phases and nitride metal The solid solution TiZrN of object2Phase.
In the present embodiment, Si3N4∶TiN∶Y2O3∶La2O3: AlN=(9~11): (5.4~6.6): (0.8~1.2): (0.8~1.2): (1.3~1.66), the addition of ZrN is 8~15w.t%.
A kind of Si3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics, Si3N4α phases content is selected to be higher than 70% powder Material, purity are higher than 97%, 0.7 μm of particle mean size；Y2O3、La2O3It is commercially available with AlN, chemistry is pure；TiN is purchased from Hefei Kai Er nanometers Energy science and technology limited company, purity 99.2%, particle mean size 20nm；ZrN is purchased from Jinzhou Jin Xin limited companies； By each ingredient in (9~11): (): (5.4~6.6): (0.8~1.2): (0.8~1.2): the ratio of (1.3~1.66) weighs Dispensing when adding in alcohol by the material prepared mix grinding 2 is small in agate mortar or adds in alcohol and ZrO2Ball ball in polyurethane cylinder Grind 1 it is small when be placed on air drying；Again by dried mixture with the dry-pressing of stainless steel grinding tool into being put into sintering furnace after square In in N2It is sintered in protective atmosphere, sintering temperature is 1760 DEG C ± 25 DEG C, and soaking time is set to according to the big I of sample 1-3h。
The material phase analysis of sample is carried out to sintering using Rigaku D/MAX-RB types X-ray diffractometer, it was demonstrated that in sample Solid solution TiZrN containing metal nitride2。

Claims (2)

1. a kind of Si3N4-TiZrN2- TiN composite conductive ceramics, it is characterised in that：Synthesize the raw material bag of the composite conductive ceramic It includes：Si3N4、ZrN、TiN、Y2O3、La2O3、AlN；Include Si in the final product of the composite conductive ceramic3N4Phase, TiN phases and gold Belong to the solid solution TiZrN of nitride2Phase；
Si3N4∶TiN∶Y2O3∶La2O3: AlN=(9~11): (5.4~6.6): (0.8~1.2): (0.8~1.2): (1.3~ 1.66), the addition of ZrN is 8~15w.t%.
2. a kind of Si3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics, it is characterised in that：Comprise the following steps：
(1) dispensing mixes：By Si3N4、TiN、Y2O3、La2O3, AlN is with (9~11): (5.4~6.6): (0.8~1.2): (0.8 ~1.2): the ratio mixing of (1.3~1.66), the addition of ZrN is 8~15w.t%, adds in alcohol grinding in mortar afterwards It is dry after 1~3h；Wherein, Si3N4α phases content higher than 70%, purity is higher than 97%, and granularity is 0.6~0.8 μm, TiN granularities For 18~22nm, ZrN granularities are 16~21nm；
(2) it is molded and is sintered：Dried mixture is put into sintering furnace in N after isostatic cool pressing again with mold is dry-pressing formed2 It is sintered in protective atmosphere, sintering temperature is 1760 ± 25 DEG C, and soaking time is 1~3h.
CN201610178439.2A 2016-03-18 2016-03-18 A kind of Si3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics Expired - Fee Related CN105884375B (en)

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CN113121245A (en) * 2019-12-31 2021-07-16 辽宁省轻工科学研究院有限公司 Silicon nitride-based composite conductive ceramic capable of being subjected to discharge machining and preparation method thereof
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CN102170716A (en) * 2010-12-09 2011-08-31 江苏华盛精细陶瓷科技有限公司 Method for manufacturing silicon nitride heating body
CN103096528A (en) * 2010-12-09 2013-05-08 江苏华盛精细陶瓷科技有限公司 Preparation method for silicon nitride heating body
CN103764595A (en) * 2011-06-21 2014-04-30 戴蒙得创新股份有限公司 Composite compacts formed of ceramics and low-volume cubic boron nitride and method of manufacture

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CN102170716A (en) * 2010-12-09 2011-08-31 江苏华盛精细陶瓷科技有限公司 Method for manufacturing silicon nitride heating body
CN103096528A (en) * 2010-12-09 2013-05-08 江苏华盛精细陶瓷科技有限公司 Preparation method for silicon nitride heating body
CN103764595A (en) * 2011-06-21 2014-04-30 戴蒙得创新股份有限公司 Composite compacts formed of ceramics and low-volume cubic boron nitride and method of manufacture

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