CN102825259B - Method for preparing TiAl inter-metallic compound powder by using titanium hydride powder - Google Patents

Method for preparing TiAl inter-metallic compound powder by using titanium hydride powder Download PDF

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CN102825259B
CN102825259B CN201210354102.4A CN201210354102A CN102825259B CN 102825259 B CN102825259 B CN 102825259B CN 201210354102 A CN201210354102 A CN 201210354102A CN 102825259 B CN102825259 B CN 102825259B
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powder
metallic compound
titanium hydride
hydride powder
hydride
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CN102825259A (en
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邵慧萍
王志
林涛
郭志猛
叶青
王军
孙森
吕绍元
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Jiangsu Jinwu New Material Co Ltd
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University of Science and Technology Beijing USTB
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Abstract

The invention belongs to the technical field of powder metallurgy, and relates to a method for preparing TiAl inter-metallic compound powder by using titanium hydride powder. The method comprises the following preparation steps of: weighing titanium hydride powder and aluminum powder according to an atom ratio of Ti to Al being 1: 1, and uniformly mixing the powders through ball milling of a high-energy ball milling machine, wherein toluene is added as a controlling agent in a ball milling process, so as to prevent oxidation; then sintering the powders by using a certain process in a rapid warming tube type electric furnace with a vacuum degree of 4.0*10<-2> to 4.0*10<-3> Pa, and cooling along with the furnace to obtain the TiAl inter-metallic compound. The method provided by the invention is simple in technique process; the cheap titanium hydride powder is used as a raw material, and is simply milled after diffusing and sintering in a low temperature condition, so as to obtain the TiAl inter-metallic compound powder with very high purity; and the TiAl inter-metallic compound is subjected to follow-up machining, such as molding, through a powder metallurgy normal method.

Description

A kind of hydride powder prepares the method for TiAl intermetallic compound powder
Technical field
The invention belongs to powder metallurgical technology, relate to a kind of method that hydride powder prepares TiAl intermetallic compound powder.
Background technology
Along with developing rapidly of the field such as space flight and aviation and automobile, Intermatallic Ti-Al compound becomes the following high-temperature structural material having development potentiality most due to the performance of its excellence, apply widely in fields such as Aero-Space, as the various parts in space flight engine, the engine component etc. in Gran turismo.
The technique that powder metallurgy prepares TiAl-base alloy can be divided into element powders method and pre-alloyed powder method by material powder.Take element powders as raw material, cost is lower, but due to Kirkendall effect, significantly volumetric expansion can be produced in reaction-sintered, thus adopt pressureless sintering to be difficult to obtain high dense material, simultaneously also because of its oxygen and impurity content higher, sintering character is poor, the performance of alloy product is slackened, and make material obtain higher-density although the technique such as hot pressing or high temperature insostatic pressing (HIP) can obtain, cost is more expensive; The homogeneity of ingredients of pre-alloyed powder method is good, oxygen and impurity content low, mechanical property is good, but at present the method for production TiAl intermetallic compound generally adopts the method such as mechanical alloying, vacuum metling to produce.In these methods, mechanical alloying easily produces various being mingled with; There is component segregation in vacuum metling, operation difficulties is large, easily produces the various shortcoming such as to be mingled with.Therefore the necessary method to preparing alloyed powder is inquired into, and develops new technique to carry out the production of alloyed powder, and make the alloyed powder cost produced lower, be mingled with less, purity is higher, and preparation technology is simpler.
The titanium valve that Wang Jun etc. utilize titantium hydride Oxidative Dehydrogenation to obtain and aluminium powder are raw material, after mechanical mixture, in tube furnace, carry out diffusion reaction obtain TiAl alloy powder, but comparatively titantium hydride is expensive in price for the titanium valve obtained with titantium hydride Oxidative Dehydrogenation, and add that titanium valve is large compared with the activity of hydride powder, oxygen etc. in titanium valve is caused to be mingled with content higher, very unfavorable to further processing below.
Summary of the invention
A kind of hydride powder is the object of the present invention is to provide to prepare the method for TiAl intermetallic compound powder.
Hydride powder has lower price relative to titanium valve, and when sintering temperature is not very high, sintering obtains TiAl alloy powder, finally sinter the alloyed powder obtained and have very high purity, and the operating process of the method is very simple.Therefore, can be used as a kind of method preparing high-purity Ti Al alloyed powder.
Hydride powder prepares a method for TiAl intermetallic compound powder, it is characterized in that:
1) be that 1:1 weighs hydride powder and aluminium powder according to Ti, Al atomic ratio, in high energy ball mill, carry out homogenising; It is the anti-oxidation of controlling agent that its process adds toluene;
2) material after above-mentioned mixing being put into vacuum is≤4.0 × 10 -2pa is rapidly heated in electric tube furnace, is diffusion reaction temperature at 100-650 DEG C, and heating rate is 2 ~ 4 DEG C/min, and temperature retention time is 10min ~ 4 hour; Low rate intensification diffusion reaction object is the dehydrogenation of diffusion reaction in order to aluminium powder and hydride powder.Sintering temperature is 750-1000 DEG C, and heating rate is 4 ~ 8 DEG C/min, and temperature retention time is 1-5 hour, and higher temperature insulation is in order to the alloying between titanium and aluminium.
3) heating cools with stove after terminating, and through grinding and obtain TiAl intermetallic compound powder, particle mean size is 10-50 μm.
Because first period carries out the dehydrogenation of titantium hydride in low-temperature insulation stage or temperature-rise period, the various defect of the mixed powder after vibratory milling is made to reduce and portion of energy is discharged, and Ti, the sensitiveness of the diffusion couple temperature retention time of Al mixed powder is more much lower to the sensitiveness of temperature than it, therefore simple prolongation still can not obtain purer TiAl alloy powder in several hours, so the Ti after dehydrogenation, Al powder cannot carry out sufficient alloying in lower temperature range, only be heated to uniform temperature, to Ti, the diffusion of Al powder provides enough energy, just can obtain very pure TiAl alloy powder.Meanwhile, the titanium valve obtained compared with titantium hydride Oxidative Dehydrogenation in price due to hydride powder is cheaply more, well below the fringe cost produced due to intensification.Therefore, the present invention has distinct practical significance.
Advantage of the present invention is: it is then that titanium valve used is again obtain with titantium hydride Oxidative Dehydrogenation, and thus price is higher with titanium valve and aluminium powder for raw material that routine produces TiAl intermetallic compound powder; The present invention is then be directly raw material with titanium hydride powders and aluminium powder, under a high vacuum and temperature is lower when sinter, not only cost is low, and it is also little that the TiAl intermetallic compound powder of gained contains impurity; The technical process of said method is extremely simple.
Detailed description of the invention
embodiment 1:
Step 1: take the hydride powder 240g that particle mean size is 30 μm, particle mean size is the aluminium powder 135g of 8 μm, mixes 1 hour in high energy ball mill, and wherein adding toluene is the anti-oxidation of controlling agent;
Step 2: be 3 × 10 in vacuum by mixed-powder -3heat in the electric tube furnace that is rapidly heated of Pa, heating process is: be heated to 120 DEG C with the firing rate of 3 DEG C/min, at 120 DEG C of insulation 10min, 500 DEG C are warming up to the firing rate of 3 DEG C/min from 120 DEG C, carry out insulation 2 hours, then be warmed up to 750 DEG C with the firing rate of 6 DEG C/min, then be incubated 2 hours;
Step 3: the powder after heating is cooled with stove, carries out simple grinding and namely obtain the TiAl intermetallic compound powder that particle mean size is 10 μm.
embodiment 2:
Step 1: take the hydride powder 240g that particle mean size is 50 μm, particle mean size is the aluminium powder 135g of 15 μm, mixes 20 hours in high energy ball mill, and wherein adding toluene is the anti-oxidation of controlling agent;
Step 2: be 3 × 10 in vacuum by mixed-powder -2heat in the electric tube furnace that is rapidly heated of Pa, heating process is: be heated to 120 DEG C with the firing rate of 3 DEG C/min, at 120 DEG C of insulation 10min, is warmed up to 1000 DEG C from 120 DEG C with the programming rate of 6 DEG C/min, then 1000 DEG C of insulations 3 hours;
Step 3: the powder after heating is cooled with stove, carries out simple grinding and namely obtain the TiAl intermetallic compound powder that particle mean size is 30 μm.

Claims (1)

1. prepare a method for TiAl intermetallic compound powder with hydride powder, it is characterized in that:
1) be that 1:1 weighs hydride powder and aluminium powder according to Ti, Al atomic ratio, within ball milling 1-24 hour in high energy ball mill, carry out homogenising; It is the anti-oxidation of controlling agent that its process adds toluene;
The particle mean size of raw materials used hydride powder is 20-65 μm, and the particle mean size of aluminium powder is 5-20 μm;
2) material after above-mentioned mixing being put into vacuum is≤4.0 × 10 -2pa is rapidly heated in electric tube furnace, carries out Dehydroepiandrosterone derivative at 100-500 DEG C, and heating rate is 2-4 DEG C/min, and temperature retention time is 10min-4 hour; Then be directly heated to high temperature, carry out carrying out alloying in insulation 1-5 hour at 1000 DEG C; Low rate intensification diffusion reaction object is the dehydrogenation of diffusion reaction in order to aluminium powder and hydride powder, and higher temperature insulation is in order to the alloying between titanium and aluminium;
3) heating cools, through grinding and obtain TiAl intermetallic compound powder with stove after terminating;
After grinding, the particle mean size of TiAl intermetallic compound powder is 10-50 μm.
CN201210354102.4A 2012-09-21 2012-09-21 Method for preparing TiAl inter-metallic compound powder by using titanium hydride powder Active CN102825259B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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RU2758372C1 (en) * 2020-10-26 2021-10-28 Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский авиационный институт (национальный исследовательский университет)" METHOD FOR PRODUCING POWDERS FROM INTERMETALLIC TITANIUM ALLOYS BASED ON Ti2AlNb (VARIANTS)

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CN104325150A (en) * 2014-11-10 2015-02-04 中国核动力研究设计院 Preparation process for metal hydride powder
CN104550963A (en) * 2014-12-16 2015-04-29 中国航空工业集团公司北京航空材料研究院 Method for realizing forming of titanium alloy powder by utilizing titanium hydride alloy powder
CN105499576B (en) * 2016-01-11 2018-01-16 北京科技大学 A kind of method that powder metallurgy prepares porous titanium-aluminium alloy
CN110369734A (en) * 2019-06-25 2019-10-25 西安宝德九土新材料有限公司 A kind of preparation method of titanium-aluminium alloy powder
CN111545743B (en) * 2020-04-21 2021-08-31 北京科技大学 Method for preparing high-performance powder metallurgy titanium-aluminum intermetallic compound
CN111545742B (en) * 2020-04-21 2021-08-31 北京科技大学 Method for preparing high-performance powder metallurgy Ti6Al4V alloy
CN112453384B (en) * 2020-11-10 2022-04-15 中南大学 Preparation method of diffusion bonding titanium powder
CN114309621B (en) * 2021-12-28 2023-11-10 云航时代(重庆)科技有限公司 Preparation method of fine TiAl alloy spherical powder containing refractory metal elements

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JPH04210401A (en) * 1990-12-13 1992-07-31 Honda Motor Co Ltd Production of structural member made of tial intermetallic compound
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2758372C1 (en) * 2020-10-26 2021-10-28 Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский авиационный институт (национальный исследовательский университет)" METHOD FOR PRODUCING POWDERS FROM INTERMETALLIC TITANIUM ALLOYS BASED ON Ti2AlNb (VARIANTS)

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