CN1724467A - Process for synthesizing tin titanium carbide ceramic powder under atmospheric pressure - Google Patents

Process for synthesizing tin titanium carbide ceramic powder under atmospheric pressure Download PDF

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Publication number
CN1724467A
CN1724467A CN 200510011931 CN200510011931A CN1724467A CN 1724467 A CN1724467 A CN 1724467A CN 200510011931 CN200510011931 CN 200510011931 CN 200510011931 A CN200510011931 A CN 200510011931A CN 1724467 A CN1724467 A CN 1724467A
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powder
snc
ceramic powder
tic
titanium carbide
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CN1278991C (en
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李世波
翟洪祥
贝国平
周洋
张志力
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Beijing Jiaotong University
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Beijing Jiaotong University
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Abstract

An ordinary-pressure synthesizing process of Ti2SnC ceramic powder includes such steps as providing powdered Ti, Sn and TiC in the mole ration of 1:(0.6-1):(0.7-1),ball grounding, pressing under 10-100 MPa to become blocks, and calcining at 1050-1250 deg. C for 5-60 min in vacuum or argon gas.

Description

A kind of atmospheric synthesizing method of tin titanium carbide ceramic powder
Technical field
The present invention relates to a kind of preparation method of ceramic powder, particularly a kind of normal pressure is synthesis of high purity carbonization tin titanium Ti in batches 2The preparation method of SnC.
Background technology
Ti 2The SnC material combines pottery and the advantage of metallic substance, and like pottery is the same, has high strength, high-modulus, resistance to chemical attack; As metal, has high conductivity, lower hardness; Particularly the image-stone China ink equally has workability and self lubricity.Ti 2SnC is with a wide range of applications novel, as can be used as and flowed friction means, substitute graphite as brush material of new generation, all kinds of anti-attrition member, corrosion-resistant parts etc.In addition, Ti 2The SnC powder also can be used as the second phase toughener, not only can improve the intensity and the modulus of matrix material, and again can its conductivity of corresponding raising.Therefore synthetic Ti 2The SnC powder has crucial scientific research meaning.
Ti 2SnC is synthesized by people such as W.Jeitschko in 1963 first, and has determined its crystalline structure.Its spacer is P6 3/ mmc, lattice parameter is a=0.3618nm, (W.Jeitschko waits .Monatsh chem.1963,94:672.) to c=1.363nm.Henceforth, the research of this material is reported seldom.With Ti, Sn and C were raw material, utilize hot isostatic pressing technique 1250 ℃ of temperature up to people such as M.W.Barsoum in 1997, under the 40MPa pressure, and insulation 4h, argon shield atmosphere has been synthesized fine and close block Ti 2SnC, and measure corresponding performance.This material has lower Vickers' hardness (3.5GPa) and higher electric conductivity (14 * 10 6(Ω m) -1) (M.W.Barsoum waits .Scrip.Mater.1997, and 37 (10): 1583.).Recently, people such as Zhou are with Ti, and Sn and C are raw material, utilize the solid-liquid reaction method 1250 ℃ of temperature, under the 30MPa pressure, and insulation 2h, argon shield atmosphere has been synthesized Ti 2SnC.(Y.Zhou waits .Mat.Res.Innovat.2002,6:219-225.).(H.Vincent waits .Mater.Sci.Eng.A 1998 to people such as H.Vincent, and 256:83-91.) also with Ti, Sn and C are raw material, and in reduction furnace, at 1200 ℃, insulation 6h has synthesized Ti 2SnC.
But aforesaid method is with Ti, and Sn and C are the synthetic Ti of raw material 2The existing problem of SnC is: 1) have tin (Sn), titanium carbide (TiC) or other tin titanium compound in the product, as Ti 6Sn 5, Ti 5Sn 3Deng the impurity phase.Especially the existence of TiC impurity phase has not only influenced Ti 2The synthetic purity of SnC, and to Ti 2The high conductivity of SnC material, self-lubricating and excellent specific property such as can process disadvantageous effect is all arranged; 2) agglomerating plant costliness, the generated time of Cai Yonging is long, the corresponding preparation cost that improves powder.From the angle of suitability for industrialized production, should not adopt hot pressing or hot isostatic pressing technique, atmospheric synthesizing method should be adopted, and generated time, raising Ti must be shortened 2The purity of SnC powder reduces Ti 2The cost of SnC powder.
Summary of the invention
Technical problem to be solved by this invention is, changes traditionally with Ti, and Sn and C are the synthetic Ti of initial batching 2The existing impurity phase of SnC problem directly adopts Ti, and Sn and TiC are raw material; Substitute expensive hot pressing or hot isostatic pressing technique with normal pressure-sintered technology, at 1050~1250 ℃ of synthesis of high purity Ti 2SnC solves agglomerating plant costliness in the prior art, long, the Ti of preparation time 2Problems such as the purity of SnC and cost height realize being produced on a large scale high purity Ti 2The SnC powder.
Technical scheme of the present invention is:
A kind of atmospheric synthesizing method of tin titanium carbide ceramic powder:
(1) is raw material with titanium (Ti), tin (Sn) and titanium carbide (TiC) powder, presses Ti: Sn: TiC=1: (0.6~1): the molar ratio ingredient of (0.7~1);
(2) above-mentioned batching being put into Plastic Bottle, is grinding medium with the agate ball, does on ball mill and mixes 5~10 hours;
(3) with above-mentioned batch mixing briquetting under 10~100MPa pressure;
(4) above-mentioned briquetting is placed High Temperature Furnaces Heating Apparatus, vacuum or argon shield atmosphere rise to 1050~1250 ℃ with the temperature rise rate of 10~40 ℃/min with furnace temperature, and soaking time is 5~60min; Obtain high purity Ti 2The SnC ceramic powder.
The present invention compares the beneficial effect that is had with prior art and is:
1) adopting Ti, Sn and TiC powder alternative traditional Ti, Sn and C is initial batching, and sale is all arranged on the raw materials used market;
2) technical process of the present invention is simple, in the vacuum oven of routine, can be under vacuum or argon shield atmosphere, and the short period of time, be lower than synthesis of high purity Ti under 1250 ℃ of temperature 2The SnC powder has shortened generated time, has reduced the preparation cost of powder.
3) product purity height, impurity such as no TiC exists mutually in X-ray diffracting spectrum, and the particle of acquisition is tiny evenly.
4) the present invention is applicable to large-scale production, and is easy to operate, and equipment used is simple, less investment, and the synthetic powder cost is low.
Description of drawings
Fig. 1 is the normal pressure-sintered synthetic Ti of the present invention 2The X-ray diffraction of SnC (XRD) collection of illustrative plates;
Fig. 2 is the normal pressure-sintered synthetic Ti of the present invention 2The scanning electron microscope of SnC (SEM) photo.
Embodiment
Embodiment one:
Press Ti: Sn: TiC=1: 0.8: 0.9 molar ratio ingredient, take by weighing Ti powder 24.4 grams, Sn powder 48.4 grams, TiC powder 27.2 grams, put into Plastic Bottle, be grinding medium with the agate ball, on ball mill, do and mixed 5 hours.Then in mould, be pressed into block through the pressure of 50MPa, put into High Temperature Furnaces Heating Apparatus, vacuum atmosphere rises to 1150 ℃ with the temperature rise rate of 20 ℃/min with furnace temperature, and soaking time is 30 minutes, promptly makes high purity Ti 2The SnC powder.
Embodiment two:
Press Ti: Sn: TiC=1: 0.7: 0.8 molar ratio ingredient, take by weighing Ti powder 26.8 grams, Sn powder 46.5 grams, TiC powder 26.7 grams, be grinding medium with the agate ball, on ball mill, do and mixed 5 hours.Then in mould, be pressed into block through the pressure of 20MPa, put into High Temperature Furnaces Heating Apparatus, vacuum atmosphere rises to 1150 ℃ with the temperature rise rate of 10 ℃/min with furnace temperature, and soaking time is 15 minutes, promptly makes high purity Ti 2The SnC powder.
Embodiment three:
Press Ti: Sn: TiC=1: 0.8: 0.9 molar ratio ingredient, take by weighing Ti powder 24.4 grams, Sn powder 48.4 grams, TiC powder 27.2 grams, be grinding medium with the agate ball, on ball mill, do and mixed 5 hours.Then in mould, be pressed into block through the pressure of 20MPa, put into High Temperature Furnaces Heating Apparatus, vacuum atmosphere rises to 1200 ℃ with the temperature rise rate of 15 ℃/min with furnace temperature, and soaking time is 15 minutes, promptly makes high purity Ti 2The SnC powder.
Prepared Ti 2The XRD figure spectrum of SnC powder is seen accompanying drawing 1.As seen from the figure, the product purity height, impurity such as no TiC exists mutually in XRD figure spectrum.Ti 2The SnC morphology microstructure is seen accompanying drawing 2.As seen from the figure, particle is the sheet crystalline substance, and particle size is less than 4 μ m.

Claims (1)

1. the atmospheric synthesizing method of a tin titanium carbide ceramic powder is characterized in that:
(1) is raw material with Ti, Sn and TiC powder, presses Ti: Sn: TiC=1: (0.6~1): the molar ratio ingredient of (0.7~1);
(2) above-mentioned batching being put into Plastic Bottle, is grinding medium with the agate ball, does on ball mill and mixes 5~10 hours;
(3) with above-mentioned batch mixing briquetting under 10~100MPa pressure;
(4) above-mentioned briquetting is placed High Temperature Furnaces Heating Apparatus, vacuum or argon shield atmosphere rise to 1050~1250 ℃ with the temperature rise rate of 10~40 ℃/min with furnace temperature, and soaking time is 5~60min; Obtain high purity Ti 2The SnC ceramic powder.
CN 200510011931 2005-06-15 2005-06-15 Process for synthesizing tin titanium carbide ceramic powder under atmospheric pressure Expired - Fee Related CN1278991C (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331759C (en) * 2006-03-21 2007-08-15 北京交通大学 Method for synthesizing tin-titanium carbide at low temperature
CN102320835A (en) * 2011-07-28 2012-01-18 攀枝花学院 Ti2SnC-based electrical contact material as well as preparation method and application thereof
CN103701004A (en) * 2013-11-29 2014-04-02 武汉工程大学 Carbon brush for motor and preparation method thereof
CN104557045A (en) * 2015-02-05 2015-04-29 安徽工程大学 Normal-pressure low-temperature preparation method of titanium tin carbide material
CN105777127A (en) * 2016-02-29 2016-07-20 东南大学 Preparation method of high-purity Ti2SnC powder
CN106220181A (en) * 2016-07-13 2016-12-14 东南大学 One utilizes powder metallurgy means to prepare Ti2the method of PbC pottery
CN106278272A (en) * 2016-07-20 2017-01-04 哈尔滨师范大学 A kind of Ti2the preparation method of SnC ceramic powder
CN106882965A (en) * 2017-03-10 2017-06-23 东南大学 A kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two
CN106957175A (en) * 2017-03-17 2017-07-18 东南大学 A kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two
CN110183229A (en) * 2018-06-11 2019-08-30 中铭瓷(苏州)纳米粉体技术有限公司 A kind of Ti with low-temperature cracks self-healing capability2Al(1-x)SnxC ceramics repair phase raw powder's production technology
CN116217231A (en) * 2023-01-30 2023-06-06 辽宁大学 High-purity Ti 2 Preparation method of SnC powdery ceramic material

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331759C (en) * 2006-03-21 2007-08-15 北京交通大学 Method for synthesizing tin-titanium carbide at low temperature
CN102320835A (en) * 2011-07-28 2012-01-18 攀枝花学院 Ti2SnC-based electrical contact material as well as preparation method and application thereof
CN103701004A (en) * 2013-11-29 2014-04-02 武汉工程大学 Carbon brush for motor and preparation method thereof
CN103701004B (en) * 2013-11-29 2016-01-06 武汉工程大学 A kind of carbon brush used for electric engine and preparation method thereof
CN104557045A (en) * 2015-02-05 2015-04-29 安徽工程大学 Normal-pressure low-temperature preparation method of titanium tin carbide material
CN105777127A (en) * 2016-02-29 2016-07-20 东南大学 Preparation method of high-purity Ti2SnC powder
CN106220181A (en) * 2016-07-13 2016-12-14 东南大学 One utilizes powder metallurgy means to prepare Ti2the method of PbC pottery
CN106278272A (en) * 2016-07-20 2017-01-04 哈尔滨师范大学 A kind of Ti2the preparation method of SnC ceramic powder
CN106882965A (en) * 2017-03-10 2017-06-23 东南大学 A kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two
CN106957175A (en) * 2017-03-17 2017-07-18 东南大学 A kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two
CN110183229A (en) * 2018-06-11 2019-08-30 中铭瓷(苏州)纳米粉体技术有限公司 A kind of Ti with low-temperature cracks self-healing capability2Al(1-x)SnxC ceramics repair phase raw powder's production technology
CN116217231A (en) * 2023-01-30 2023-06-06 辽宁大学 High-purity Ti 2 Preparation method of SnC powdery ceramic material

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