CN110777275A - Titanium-aluminum three-dimensional through hole structure material and preparation method thereof - Google Patents

Titanium-aluminum three-dimensional through hole structure material and preparation method thereof Download PDF

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Publication number
CN110777275A
CN110777275A CN201910957920.5A CN201910957920A CN110777275A CN 110777275 A CN110777275 A CN 110777275A CN 201910957920 A CN201910957920 A CN 201910957920A CN 110777275 A CN110777275 A CN 110777275A
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Prior art keywords
camphene
titanium
aluminum
dimensional
powder
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张树志
冯弘
侯赵平
张长江
韩富银
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

A method for preparing a titanium-aluminum three-dimensional through hole intermetallic compound belongs to the technical field of intermetallic compounds, and relates to a method for preparing an intermetallic compound porous material. The method comprises the following steps: (1) uniformly mixing titanium powder and aluminum powder in proportion to obtain mixed metal powder; (2) melting camphene crystals in a water bath and adding 1 wt.% polystyrene; (3) adding the mixed metal powder into the camphene, and continuously stirring and mixing to prevent titanium particles from settling; (4) after fully stirring, sealing the mixture by using a preservative film, taking out the mixture, and rotationally cooling the mixture to room temperature to obtain a blank material; (5) and placing the blank in a ventilation place until the embedding alkene volatilizes completely, and then sintering in vacuum at 1300 ℃ to obtain the three-dimensional through hole material. The titanium-aluminum alloy with the three-dimensional through hole structure is prepared by utilizing the low melting point (51 ℃) and volatility of the camphene, has the advantages of high porosity, large specific surface area, simple process, energy conservation and environmental protection, and provides a good foundation for further application in the chemical industry.

Description

Titanium-aluminum three-dimensional through hole structure material and preparation method thereof
Technical Field
The invention belongs to the technical field of intermetallic compounds, and relates to a titanium-aluminum three-dimensional through hole structure material and a preparation method thereof, in particular to a titanium-aluminum three-dimensional through hole material obtained by sintering titanium powder and aluminum powder after embedding and fixing and a preparation method thereof.
Background
The intermetallic compound porous material is a novel high-temperature alloy which is currently developed, has the advantages of both ceramics and metals, has excellent performances such as low density, high thermal conductivity, high specific strength and specific stiffness, high-temperature oxidation resistance, acid/alkali corrosion resistance (the heat difference is more than 600 ℃) and the like due to the fact that the intermetallic compound has metal bonds and covalent bonds, has attracted more and more attention, and is a novel porous material with great development potential. Currently, research on porous intermetallic compounds has mainly focused on intermetallic compounds containing Al, mainly including three types of Ti-Al, Fe-Al system, and Ni-Al system. The key and difficulty in preparing porous materials is to form a uniform porous structure, and how to improve the porosity and control the shape and distribution of the pore diameter according to different performance requirements is realized by controlling different parameters by using different preparation processes and knowing the formation and evolution mechanisms of the pores. The titanium-aluminum-based intermetallic compound is a novel high-temperature structural material which is researched more at present, has excellent high-temperature performance compared with a titanium-based alloy, has lower density compared with a nickel-based alloy, is only 50 percent of the density of the titanium-aluminum-based intermetallic compound, and has wide application prospect. The titanium-aluminum porous material effectively solves the technical problems of poor high-temperature oxidation resistance and corrosion resistance, difficult welding assembly of the ceramic porous material, low strength and the like. Compared with other porous materials, the titanium-aluminum porous material has the advantages of simple preparation process, low cost, energy conservation and environmental protection, and has important theoretical significance in further application in the chemical industry.
According to the new results, the method for preparing the titanium-aluminum three-dimensional through hole material and the method for fixing the titanium-aluminum blank by using the embedding alkene slurry have no other related reports at home and abroad.
Disclosure of Invention
The invention aims to provide a titanium-aluminum three-dimensional through hole structure material and a preparation method thereof, and the titanium-aluminum three-dimensional through hole material can be prepared more conveniently and rapidly by adopting the method.
The technical scheme of the invention is as follows: a preparation method of a titanium-aluminum three-dimensional through hole structure material is characterized by comprising the following steps: the method comprises the following steps:
(1) titanium powder and aluminum powder are mixed according to the mass ratio of Ti: al =1:1, uniformly mixing to obtain mixed metal powder;
(2) weighing camphene crystals, placing the camphene crystals in a container, placing the container in a water bath at 60 ℃ for heat preservation to melt the camphene crystals, and adding a binder polystyrene into the molten camphene to obtain camphene slurry; then, embedding the alkene slurry: mixed metal powder = 4: 1, pouring the mixed metal powder into a container containing the camphene slurry, and continuously stirring to prevent Ti particles from settling;
(3) after the slurry and the mixed metal powder are uniformly stirred, the container is quickly taken out, a preservative film is used for sealing (the prepared slurry is required to fill the container because of the volume shrinkage of the camphene crystal), the container is fixed on a self-made rotary auxiliary tool, and the container is cooled in a rotary mode. After the camphene is solidified, demoulding the blank, taking out, placing in a ventilated place, and periodically weighing until the weight is not reduced any more, namely all the camphene volatilizes to obtain a porous blank;
(4) vacuum sintering the porous blank in a tubular vacuum furnace with the vacuum degree of 6.0 × 10 -3Pa~1.6×10 -2Pa, heating at a rate of 4 ℃/min, sintering at a temperature of 1300 ℃, sintering for 310min, and cooling at a rate of 10 ℃/min to obtain the intermetallic compound of the titanium-aluminum three-dimensional through hole structure.
The method for preparing the titanium-aluminum three-dimensional through hole structure material according to claim 1, wherein the method comprises the following steps: the initial material titanium powder and aluminum powder are 500 meshes of 99.5 percent titanium with purity and 99.85 percent aluminum powder with purity.
The method for preparing the titanium-aluminum three-dimensional through hole structure material according to claim 1, wherein the method comprises the following steps: the stirred mixture contained 80 vol% of camphene slurry and 20 vol% of mixed metal powder.
The method for preparing the titanium-aluminum three-dimensional through hole structure material according to claim 1, wherein the method comprises the following steps: the camphene slurry consists of camphene and binder polystyrene, wherein the addition amount of the polystyrene is 1 wt.%.
A titanium-aluminum three-dimensional through-hole structure material prepared according to any one of the preparation methods of claims 1 to 4.
The titanium-aluminum three-dimensional through hole material prepared by the invention has the advantages of small density, high oxidation resistance and corrosion resistance and the like, meets the special requirements of certain heat resistance and corrosion resistance for filtration in the chemical industry, and improves the service life and the service range of the porous material.
The prepared titanium-aluminum three-dimensional through hole material framework has the traditional gamma-TiAl and α of titanium-aluminum alloy 2-Ti 3An Al two-phase structure. The porous titanium-aluminum framework with the dendritic three-dimensional through holes is prepared by volatilization of the camphene slurry, the operation is simple and convenient, and the communicated pores provide a good matrix for application.
In the cooling process, the uniformity of the camphene slurry and the mixed metal powder is ensured by adopting a rotary cooling mode, the porosity is high, and the pore distribution is uniform.
Drawings
FIG. 1 shows the surface morphology of a titanium-aluminum three-dimensional via material; FIG. 2 is a hole morphology of a titanium aluminum three-dimensional via material; FIG. 3 is an XRD pattern of a titanium aluminum three-dimensional via intermetallic compound; fig. 4 is a diagram of a vacuum sintering process.
Detailed Description
The volume of the porous material is 50cm 3According to 20 vol.% of metal powder, titanium powder: and (3) calculating the mass of the required powder by the atomic ratio of the aluminum powder =1: 1. Weighing corresponding metal powder, mixing the titanium powder and the aluminum powder in an atomic ratio of 1:1, and uniformly stirring. The required mass of camphene is converted according to 80 vol.%, the weighed camphene is placed in a mould, the water temperature in a water bath kettle is kept at 60 ℃, and the mould is placed in the water bath kettle for heating. After the camphene in the mould is melted, adding 1 wt.% of polystyrene as a binder to prepare a camphene melt, transferring the mixed metal powder into the mould to be dissolved in the camphene melt, and uniformly stirring. And taking the mold out of the water bath and fixing the mold on a prepared bracket. To prevent the slurry from settling during the setting process, resulting in uneven material, the support is rotated horizontally, causing the mold to rotate in the horizontal direction. And (4) demolding the porous blank after the slurry is solidified, and placing the porous blank in a ventilated place for drying to volatilize the camphene. And placing the dried porous blank body in a hot-pressing sintering furnace for sintering. The sintering process curve is shown in FIG. 4, the sintering temperature rise rate is 4 ℃/min, the low-temperature reaction sintering is respectively carried out at 400 ℃ and 600 ℃ for 60min and 120min, the high-temperature sintering is carried out at 1300 ℃ for 130min, and after the reaction is finished, the cooling rate is controlled at 10 ℃/min. The prepared surface appearance is shown in figure 1, the pore appearance is shown in figure 2, the pore diameter ranges from 10 to 45 mu m, and the porosity is 56.788%. The XRD pattern of the titanium-aluminum three-dimensional through hole material is shown in figure 3.

Claims (5)

1. A preparation method of a titanium-aluminum three-dimensional through hole structure material is characterized by comprising the following steps: the method comprises the following steps:
(1) titanium powder and aluminum powder are mixed according to the mass ratio of Ti: al =1:1, uniformly mixing to obtain mixed metal powder;
(2) weighing camphene crystals, placing the camphene crystals in a container, placing the container in a water bath at 60 ℃ for heat preservation to melt the camphene crystals, and adding a binder polystyrene into the molten camphene to obtain camphene slurry; then, embedding the alkene slurry: mixed metal powder = 4: 1, pouring the mixed metal powder into a container containing the camphene slurry, and continuously stirring to prevent Ti particles from settling;
(3) after the slurry and the mixed metal powder are uniformly stirred, quickly taking out the container, sealing the container by using a preservative film (the prepared slurry is required to fill the container because of the volume shrinkage of the camphene crystal), fixing the container on a self-made rotary auxiliary tool, and carrying out rotary cooling;
after the camphene is solidified, demoulding the blank, taking out, placing in a ventilated place, and periodically weighing until the weight is not reduced any more, namely all the camphene volatilizes to obtain a porous blank;
(4) vacuum sintering the porous blank in a tubular vacuum furnace with the vacuum degree of 6.0 × 10 -3Pa~1.6×10 -2Pa, heating at a rate of 4 ℃/min, sintering at a temperature of 1300 ℃, sintering for 310min, and cooling at a rate of 10 ℃/min to obtain the intermetallic compound of the titanium-aluminum three-dimensional through hole structure.
2. The method for preparing the titanium-aluminum three-dimensional through hole structure material according to claim 1, wherein the method comprises the following steps: the initial material titanium powder and aluminum powder are 500 meshes of 99.5 percent titanium with purity and 99.85 percent aluminum powder with purity.
3. The method for preparing the titanium-aluminum three-dimensional through hole structure material according to claim 1, wherein the method comprises the following steps: the stirred mixture contained 80 vol% of camphene slurry and 20 vol% of mixed metal powder.
4. The method for preparing the titanium-aluminum three-dimensional through hole structure material according to claim 1, wherein the method comprises the following steps: the camphene slurry consists of camphene and binder polystyrene, wherein the addition amount of the polystyrene is 1 wt.%.
5. A titanium-aluminum three-dimensional through-hole structure material prepared according to any one of the preparation methods of claims 1 to 4.
CN201910957920.5A 2019-10-10 2019-10-10 Titanium-aluminum three-dimensional through hole structure material and preparation method thereof Pending CN110777275A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102008017547A1 (en) * 2008-03-07 2009-09-10 Autogastechnik Triptis Gmbh Filter unit for insertion in fuel supply line of liquid petroleum gas combustion engine, has filter housing and filter insert, where filter insert is carried from housing
CN102071333A (en) * 2010-12-20 2011-05-25 中南大学 Method for preparing foamed TiAl intermetallic compound
CN102718541A (en) * 2012-02-21 2012-10-10 山东科技大学 Porous material with whiskers or rod crystals in apertures and preparation method thereof
CN106978550A (en) * 2017-03-22 2017-07-25 西安建筑科技大学 A kind of Ti porous materials and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102008017547A1 (en) * 2008-03-07 2009-09-10 Autogastechnik Triptis Gmbh Filter unit for insertion in fuel supply line of liquid petroleum gas combustion engine, has filter housing and filter insert, where filter insert is carried from housing
CN102071333A (en) * 2010-12-20 2011-05-25 中南大学 Method for preparing foamed TiAl intermetallic compound
CN102718541A (en) * 2012-02-21 2012-10-10 山东科技大学 Porous material with whiskers or rod crystals in apertures and preparation method thereof
CN106978550A (en) * 2017-03-22 2017-07-25 西安建筑科技大学 A kind of Ti porous materials and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JUNG HYUN-DO ET AL.: "Dynamic freeze casting for the production of porous titanium (Ti) scaffolds", 《MATERIALS SCIENCE & ENGINEERING. C》 *

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