CN1108392C - Method for preparing titanium aluminium carbon block material by in-situ hot pressing/solid-liquid phase reaction - Google Patents

Method for preparing titanium aluminium carbon block material by in-situ hot pressing/solid-liquid phase reaction Download PDF

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Publication number
CN1108392C
CN1108392C CN 00123203 CN00123203A CN1108392C CN 1108392 C CN1108392 C CN 1108392C CN 00123203 CN00123203 CN 00123203 CN 00123203 A CN00123203 A CN 00123203A CN 1108392 C CN1108392 C CN 1108392C
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powder
solid
liquid phase
hot pressing
phase reaction
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CN 00123203
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CN1352317A (en
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周延春
王晓辉
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The present invention relates to a method for preparing a Ti-Al-C block material by in-situ hot-pressing/solid-liquid phase reaction. The method is characterized in that Ti powder, Al powder and C powder in the atomic ratio of 3: (1.0 to 1.1): (1.8 to 2.0) are used as raw materials; the raw materials are processed through ball milling for 5 to 15 hours and pressed into a cake shape under the pressure of 8 to 12MPa; the raw material cakes are put in a graphite mold, the temperature is increased to 1200 DEG C to 1500 DEG C at the heating rate of 5 to 30 DEG C/min in a hot-pressing furnace in the presence of Ar gas as protective atmosphere, and the in-situ hot-pressing /solid-liquid phase reaction is carried for 0.5 to 4 hours, and the pressure of hot pressing is from 10 to 50MPa. The method can be carried out at a low temperature in a short period of time.

Description

A kind of in-situ hot pressing/solid-liquid phase reaction prepares the method for titanium aluminium carbon block material
The present invention relates to intermetallic compound, provide a kind of in-situ hot pressing/solid-liquid phase reaction to prepare Ti especially 3AlC 2The method of block materials.
Ti 3AlC 2It is a kind of novel tertiary lamellar compound.It had both had the plurality of advantages of stupalith, as high-melting-point, and high-modulus (Young's modulus 297GPa, shearing modulus 124GPa), high strength etc.; Some characteristics that have metallic substance again, as high conductivity, high thermal conductivity, but destruction there are strong resistibility and mechanical workout etc.In addition, because Ti 3AlC 2Low (the 4.2g/cm of density 3), be a kind of a kind of novel texture/function integration material that gets a good chance of being applied in high-tech sectors such as Aeronautics and Astronautics, nuclear industry and electronic information.Though Ti 3AlC 2Have excellent comprehensive performance and application prospects.But because the preparation difficulty of this material makes his fundamental research and application be restricted.As document 1.J.Am.Ceram.Soc.83, No.4,2000.With Ti, graphite and Al 4C 3Be raw material, at 1400 ℃, 70MPa hot pressing 16 hours synthesizes the Ti of non-stoichiometric 3AlC 2The block polycrystalline material.Because Al in the raw material 4C 3Water-absorbent very strong, Al 4C 3The moisture that absorbs is difficult to Ex-all, and causing has Al in product 2O 3Impurity exist mutually ( )。Al 2O 3Be the brittle oxide pottery, it is at Ti 3AlC 2Existence in the polycrystalline bulk material influences Ti 3AlC 2Mechanical property and conductivity.
Having the object of the present invention is to provide a kind of is raw material with Ti powder, Al powder and C powder, carries out in-situ hot pressing/solid-liquid phase reaction in lesser temps, short period of time and obtains Ti 3AlC 2The preparation method of block materials.
The invention provides a kind of in-situ hot pressing/solid-liquid phase reaction and prepare the method for titanium aluminium carbon block material, Ti 3AlC 2The chemical ingredients of block materials is pressed atomic ratio, Ti: Al: C :=3: 1: 2, it is characterized in that:
1) raw material is formed and composition range:
With the Ti powder, Al powder and C powder are raw material; The Ti powder, the atomic ratio Ti of Al powder and C powder: Al: C=3: (1.0-1.1): (1.8-2.0);
2) technology:
Raw material ball milling 5~15 hours; depress to pie at 8~12MPa pressure; put into graphite jig and rose to 1200 ℃ of-1500 ℃ of in-situ hot pressings/solid-liquid phase reaction 0.5-4 hour, hot pressing pressure 10-50MPa being connected with hot pressing furnace that Ar gas does protective atmosphere temperature rise rate with 5-30 ℃/min.
Characteristics of the present invention are: 1. select for use starting material simple, they are Ti powder, Al powder and C powder; 2. make full use of Ti and Al, the thermopositive reaction between Ti and the C promotes Ti 3AlC 2Synthetic, therefore, hot pressing temperature is low, below 1500 ℃, the reaction times is short, generally at 2 hours with interior synthetic finishing; 3. by in-situ hot pressing/solid-liquid phase reaction, reaction and one step of sintering finish, and have obtained single mutually fine and close Ti 3AlC 2Block materials.Its reaction process can be described as:
Below by embodiment in detail the present invention is described in detail.
Accompanying drawing 1 is the X-ray diffraction of reaction product;
Embodiment 1.
Ti powder 71.82 grams; Al powder 13.49 grams; C powder 12.01 grams; ball milling 10 hours; depress to pie at 10MPa pressure; put into graphite jig and rose to 1450 ℃ of in-situ hot pressings/solid-liquid phase reaction 2 hours, hot pressing pressure 20MPa being connected with hot pressing furnace that Ar gas does protective atmosphere temperature rise rate with 10 ℃/min.The reaction product that obtains is Ti through the X-ray diffraction analysis 3AlC 2Ti 3AlC 2X-ray diffraction pattern see accompanying drawing 1.Surveying its density with Archimedes's method is 4.22g/cm 3(theoretical density is 4.25g/cm 3).
Example 2.
Ti powder 71.82 grams, Al powder 14.84 grams, C powder 10.81 grams; ball milling 10 hours; depress to pie at 10MPa pressure, put into graphite jig and rise to 1500 ℃ of solid-liquid phase reactions 1 hour, hot pressing pressure 20MPa being connected with hot pressing furnace that Ar gas does protective atmosphere temperature rise rate with 20 ℃/min.It is 4.2g/cm that block is surveyed its density with Archimedes's method 3The reaction product that obtains is Ti through the X-ray diffraction analysis 3AlC 2

Claims (1)

1、一种原位热压/固-液相反应制备钛铝碳块体材料的方法,Ti3AlC2块体材料的化学成分按原子比,Ti∶Al∶C∶=3∶1∶2,其特征在于:1. A method for preparing titanium-aluminum-carbon bulk material by in-situ hot pressing/solid-liquid phase reaction, the chemical composition of Ti 3 AlC 2 bulk material is atomic ratio, Ti:Al:C:=3:1:2 , characterized by: 1)原料组成及成分范围:1) Raw material composition and ingredient range: 以Ti粉,Al粉和C粉为原料;Ti粉,Al粉和C粉的原子比Ti∶Al∶C=3∶(1.0-1.1)∶(1.8-2.0);Using Ti powder, Al powder and C powder as raw materials; the atomic ratio of Ti powder, Al powder and C powder Ti: Al: C=3: (1.0-1.1): (1.8-2.0); 2)工艺:2) Process: 原料球磨5~15小时,在8~12MPa压力下压成饼状,放入石墨模具中在通有Ar气做保护气氛的热压炉中以5-30℃/min的升温速率升至1200℃-1500℃原位热压/固-液相反应0.5-4小时,热压压力10-50MPa。Ball mill the raw material for 5-15 hours, press it into a cake shape under a pressure of 8-12MPa, put it into a graphite mold, and heat it up to 1200°C at a rate of 5-30°C/min in a hot-press furnace with Ar gas as a protective atmosphere In-situ hot pressing at -1500°C/solid-liquid phase reaction for 0.5-4 hours, hot pressing pressure 10-50MPa.
CN 00123203 2000-11-06 2000-11-06 Method for preparing titanium aluminium carbon block material by in-situ hot pressing/solid-liquid phase reaction Expired - Fee Related CN1108392C (en)

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Families Citing this family (8)

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Publication number Priority date Publication date Assignee Title
CN100519477C (en) * 2006-02-17 2009-07-29 中国科学院金属研究所 Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction
CN100519478C (en) * 2006-02-22 2009-07-29 中国科学院金属研究所 Method for preparing zirconium-aluminium-carbon ceramic cube material by in-situ reaction heat-pressing
CN100396650C (en) * 2006-10-30 2008-06-25 陕西科技大学 Method for preparing Ti2AlC ceramic material
CN103208735A (en) * 2012-01-12 2013-07-17 郑州大学 Heat sink with adjustable thermal expansion coefficients for large-power semiconductor laser array
CN104016345B (en) * 2014-06-03 2016-04-27 河海大学 The preparation method of one kind Graphene two-dimensional layer titanium carbide nanometer sheet
CN106396683B (en) * 2016-08-29 2019-03-01 华北电力大学(保定) A kind of titanium aluminium carbon and titanium carbide composite hydrogen storage material and preparation method thereof
CN109231988B (en) * 2018-11-01 2020-09-22 燕山大学 Large-vacancy non-metered specific activity Ti3AlC2Method for preparing ceramic material
CN110627507B (en) * 2019-09-18 2022-02-25 广东工业大学 A kind of low temperature silicon carbide ceramic and its preparation method and application

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