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CN101108291A - A kind of preparation method of FeAl intermetallic compound filter material - Google Patents

A kind of preparation method of FeAl intermetallic compound filter material Download PDF

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Publication number
CN101108291A
CN101108291A CNA2007100354063A CN200710035406A CN101108291A CN 101108291 A CN101108291 A CN 101108291A CN A2007100354063 A CNA2007100354063 A CN A2007100354063A CN 200710035406 A CN200710035406 A CN 200710035406A CN 101108291 A CN101108291 A CN 101108291A
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China
Prior art keywords
powder
filter material
minutes
intermetallic compound
sintering
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CNA2007100354063A
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Chinese (zh)
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贺跃辉
江垚
高海燕
沈培智
徐南平
黄伯云
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Central South University
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Central South University
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Abstract

本发明公开了一种FeAl金属间化合物过滤材料的制备方法。A.选取粒径为100~1μm的Fe粉和粒径为100~1μm的Al粉,其成分配比为75~25at.%Fe和25~75at.%Al;B.采用模压成形制备片状成形坯,压制压力控制在100~300MPa,或采用冷等静压制备管状成形坯,等静压力控制在50~200MPa;C.反应合成采用无压烧结工艺,首先在120~150℃温度下保温30~60分钟,随后以1~10℃/min的速率升至1000~1200℃,保温30~60分钟;烧结气氛为氢气或分解氨,或者采用真空烧结,真空度为1×10-1~1×10-3Pa;冷却阶段,控制降温速度为10~50℃/min。采用这种元素粉末反应合成工艺来制备过滤材料,有利于控制过滤材料的孔结构性能,制备过程不需要添加造孔剂,降低了能耗,几乎无污染。The invention discloses a preparation method of a FeAl intermetallic compound filter material. A. Select Fe powder with a particle size of 100-1 μm and Al powder with a particle size of 100-1 μm, the composition ratio of which is 75-25 at.% Fe and 25-75 at.% Al; B. Prepare flakes by molding Formed blanks, the pressing pressure is controlled at 100-300MPa, or cold isostatic pressing is used to prepare tubular shaped blanks, and the isostatic pressure is controlled at 50-200MPa; C. The reaction synthesis adopts a pressureless sintering process, and firstly, it is kept at a temperature of 120-150°C 30-60 minutes, then increase to 1000-1200°C at a rate of 1-10°C/min, and keep warm for 30-60 minutes; the sintering atmosphere is hydrogen or decomposed ammonia, or vacuum sintering, the vacuum degree is 1×10 -1 ~ 1×10 -3 Pa; in the cooling stage, the cooling rate is controlled to be 10-50°C/min. The use of this element powder reaction synthesis process to prepare the filter material is beneficial to control the pore structure performance of the filter material. The preparation process does not need to add a pore-forming agent, which reduces energy consumption and is almost pollution-free.

Description

A kind of preparation method of FeAl intermetallic compound filter material
Technical field
The present invention relates to the technology of preparing of filtering material, be specifically related to adopt a kind of preparation method of Fe, the synthetic FeAl intermetallic compound filter material of Al element powders reaction.
Background technology
Filtering material is separated dispersed microparticles by means of its porous structure that has from the fluid of disperse, thereby reaches purposes such as Separation of Solid and Liquid, solid and gas separation, purification and purification, is widely used in fields such as chemical industry, metallurgy, medicine and environmental protection.Filtering material can be divided into inorganic material and organic material two classes by the preparation material, and wherein inorganic material more and more comes into one's own owing to have high heat endurance, chemical stability and mechanical stability.Present used inorganic material mainly contains ceramic body, as aluminium oxide and glass, and metals such as copper, nickel and stainless steel, the technology of preparing that is adopted mainly is the solid particles sintering process.This preparation technology need add pore creating material usually in powder stock, brought certain environmental pollution in sintering process subsequently.Ceramic filter material need carry out sintering usually under high temperature more than 1600 ℃ simultaneously, and energy consumption is big, has improved production cost.The antiacid caustic corrosion performance and the high temperature oxidation resistance of common metal material are relatively poor.
Summary of the invention
Technical problem to be solved by this invention is to introduce the FeAl intermetallic compound in inorganic filter material, the new technology of a kind of Fe of employing, the synthetic preparation of Al element powders reaction FeAl intermetallic compound filter material is provided, with high temperature oxidation resistance and the corrosion resistance that increases substantially inorganic filter material, enlarge the use field of filtering material, cut down the consumption of energy simultaneously, reduce and pollute.
In order to solve the problems of the technologies described above, employing Fe provided by the invention, the synthetic method for preparing FeAl intermetallic compound filter membrane material of Al element powders reaction, its concrete process route is: element powders composition, grain size proportion → batch mixing → shaping → reaction are synthesized, it is characterized in that: A, to choose Fe powder and the particle diameter that particle diameter is 100~1 μ m be the Al powder of 100~1 μ m, and its composition proportion is 75~25at.%Fe and 25~75at.%Al (at. is an atomic percent); B, employing die forming prepare sheet-like formed base, and pressing pressure is controlled at 100~300MPa, or adopt isostatic cool pressing to prepare tubulose shaping base, and isostatic pressure is controlled at 50~200MPa; C, the synthetic non-pressure sintering technology that adopts of reaction at first are incubated 30~60 minutes under 120~150 ℃ of temperature, the speed with 1~10 ℃/min rises to 1000~1200 ℃ subsequently, is incubated 30~60 minutes; Sintering atmosphere is hydrogen or cracked ammonium, perhaps adopts vacuum-sintering, and vacuum is 1 * 10 -1~1 * 10 -3Pa; Cooling stage, the control cooling rate is 10~50 ℃/min.
Compared with prior art, the present invention has the following advantages:
1. because the FeAl intermetallic compound has good antiacid caustic corrosion performance, anti-curability and high temperature oxidation resistance, adopt the FeAl intermetallic compound to prepare inorganic filter material, improve the antioxygenic property of filtering material, anti-curability and corrosion resistance significantly, enlarged the use field of filtering material.
2.Fe, in the synthetic preparation of the Al element powders reaction FeAl intermetallic compound filter material process, do not need to add pore creating material and can obtain 30 ~ 50% porosity, avoided removing the pore creating material link in the traditional handicraft, reduced energy consumption, almost pollution-free.
In sum, the present invention is the new technology of a kind of Fe of employing, the synthetic preparation of Al element powders reaction FeAl intermetallic compound filter material, with high temperature oxidation resistance and the corrosion resistance that increases substantially inorganic filter material, enlarge the use field of filtering material, cut down the consumption of energy simultaneously, reduce and pollute.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1:
Adopting particle mean size is that Fe powder and the granularity of 5 μ m is the mixed-powder of the following Al powder of 50 μ m, carries out batch mixing by the composition proportion of Fe-40at.%Al, die forming under the pressure of 220MPa subsequently, and making diameter is 32mm, the sheet of thick 1~2mm is filtered base.The synthetic non-pressure sintering technology that adopts of reaction at first is incubated 30 minutes under 120 ℃ of temperature, the speed with 5 ℃/min rises to 1000 ℃ subsequently, is incubated 60 minutes; Sintering atmosphere is a hydrogen; Cooling stage, the control cooling rate is 50 ℃/min.Zhi Bei FeAl intermetallic compound sheet filtering material thus, porosity is 31%, the maximum diameter of hole is 1.7 μ m.
Embodiment 2:
The employing particle mean size is that Fe powder and the granularity of 3 μ m is the mixed-powder of the following Al powder of 20 μ m, composition proportion by Fe-30at.%Al is carried out batch mixing, adopt cold isostatic compaction tubulose base subsequently, isostatic pressure is 150MPa, making external diameter is 30mm, internal diameter is 28~29mm, and height is the tubulose shaping base of 200mm.The synthetic non-pressure sintering technology that adopts of reaction at first is incubated 60 minutes under 140 ℃ of temperature, the speed with 8 ℃/min rises to 1200 ℃ subsequently, is incubated 30 minutes; Sintering atmosphere is a vacuum, and vacuum is 1 * 10 -1~1 * 10 -3Pa; Cooling stage, the control cooling rate is 20 ℃/min.Zhi Bei FeAl intermetallic compound tubular filter material thus, porosity is 35%, the maximum diameter of hole is 1.1 μ m.
Embodiment 3:
Adopting particle mean size is that Fe powder and the granularity of 1 μ m is the mixed-powder of the following Al powder of 50 μ m, carries out batch mixing by the composition proportion of Fe-25at.%Al, die forming under the pressure of 100MPa subsequently, and making diameter is 32mm, the sheet of thick 1~2mm is filtered base.The synthetic non-pressure sintering technology that adopts of reaction at first is incubated 30 minutes under 120 ℃ of temperature, the speed with 1 ℃/min rises to 1000 ℃ subsequently, is incubated 60 minutes; Sintering atmosphere is a hydrogen; Cooling stage, the control cooling rate is 50 ℃/min.Zhi Bei FeAl intermetallic compound sheet filtering material thus, porosity is 31%, the maximum diameter of hole is 0.9 μ m.
Embodiment 4:
The employing particle mean size is that Fe powder and the granularity of 3 μ m is the mixed-powder of the following Al powder of 20 μ m, composition proportion by Fe-30at.%Al is carried out batch mixing, adopt cold isostatic compaction tubulose base subsequently, isostatic pressure is 50MPa, making external diameter is 30mm, internal diameter is 28~29mm, and height is the tubulose shaping base of 200mm.The synthetic non-pressure sintering technology that adopts of reaction at first is incubated 60 minutes under 150 ℃ of temperature, the speed with 10 ℃/min rises to 1200 ℃ subsequently, is incubated 30 minutes; Sintering atmosphere is a vacuum, and vacuum is 1 * 10 -1~1 * 10 -3Pa; Cooling stage, the control cooling rate is 10 ℃/min.Zhi Bei FeAl intermetallic compound tubular filter material thus, porosity is 36%, the maximum diameter of hole is 1.4 μ m.
Embodiment 5:
Adopting particle mean size is that Fe powder and the granularity of 5 μ m is the mixed-powder of the following Al powder of 100 μ m, carries out batch mixing by the composition proportion of Fe-75at.%Al, die forming under the pressure of 300MPa subsequently, and making diameter is 32mm, the sheet of thick 1~2mm is filtered base.The synthetic non-pressure sintering technology that adopts of reaction at first is incubated 30 minutes under 120 ℃ of temperature, the speed with 5 ℃/min rises to 1000 ℃ subsequently, is incubated 60 minutes; Sintering atmosphere is a hydrogen; Cooling stage, the control cooling rate is 50 ℃/min.Zhi Bei FeAl intermetallic compound sheet filtering material thus, porosity is 30%, the maximum diameter of hole is 1.6 μ m.
Embodiment 6:
The employing particle mean size is that Fe powder and the granularity of 100 μ m is the mixed-powder of the following Al powder of 20 μ m, composition proportion by Fe-30at.%Al is carried out batch mixing, adopt cold isostatic compaction tubulose base subsequently, isostatic pressure is 200MPa, making external diameter is 30mm, internal diameter is 28~29mm, and height is the tubulose shaping base of 200mm.The synthetic non-pressure sintering technology that adopts of reaction at first is incubated 60 minutes under 140 ℃ of temperature, the speed with 8 ℃/min rises to 1200 ℃ subsequently, is incubated 30 minutes; Sintering atmosphere is a vacuum, and vacuum is 1 * 10 -1~1 * 10 -3Pa; Cooling stage, the control cooling rate is 20 ℃/min.Zhi Bei FeAl intermetallic compound tubular filter material thus, porosity is 37%, the maximum diameter of hole is 1.9 μ m.

Claims (1)

1.一种FeAl金属间化合物过滤材料的制备方法,其具体工艺路线为:元素粉末成分、粒度配比→混料→成形→反应合成,其特征在于:A、选取粒径为100~1μm的Fe粉和粒径为100~1μm的Al粉,其成分配比为75~25at.%Fe和25~75at.%Al;B、采用模压成形制备片状成形坯,压制压力控制在100~300MPa,或采用冷等静压制备管状成形坯,等静压力控制在50~200MPa;C、反应合成采用无压烧结工艺,首先在120~150℃温度下保温30~60分钟,随后以1~10℃/min的速率升至1000~1200℃,保温30~60分钟;烧结气氛为氢气或分解氨,或者采用真空烧结,真空度为1×10-1~1×10-3Pa;冷却阶段,控制降温速度为10~50℃/min。1. A preparation method of FeAl intermetallic compound filter material, its specific process route is: element powder composition, particle size ratio→mixing→forming→reaction synthesis, characterized in that: A, the selected particle size is 100~1μm Fe powder and Al powder with a particle size of 100-1 μm, the composition ratio of which is 75-25 at.% Fe and 25-75 at.% Al; B. The sheet-shaped blank is prepared by compression molding, and the pressing pressure is controlled at 100-300 MPa , or use cold isostatic pressing to prepare tubular shaped blanks, and the isostatic pressure is controlled at 50-200MPa; C. The reaction synthesis adopts a pressureless sintering process, firstly at a temperature of 120-150°C for 30-60 minutes, and then with 1-10 The rate of ℃/min is increased to 1000-1200 ℃, and the temperature is kept for 30-60 minutes; the sintering atmosphere is hydrogen or decomposed ammonia, or vacuum sintering is used, and the vacuum degree is 1×10 -1 to 1×10 -3 Pa; in the cooling stage, Control the cooling rate to 10-50°C/min.
CNA2007100354063A 2007-07-20 2007-07-20 A kind of preparation method of FeAl intermetallic compound filter material Pending CN101108291A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102580404A (en) * 2012-02-06 2012-07-18 江苏云才材料有限公司 Method for preparing asymmetric stainless steel filter disc
CN103361505A (en) * 2012-12-27 2013-10-23 华东理工大学 Preparation method of FeAl-based porous material
TWI551451B (en) * 2014-11-05 2016-10-01 The method of making high permeability materials
CN106191492A (en) * 2016-07-12 2016-12-07 东南大学 A kind of preparation method of high-purity FeGa3 intermetallic compound
CN109454231A (en) * 2018-12-18 2019-03-12 湖北汽车工业学院 A kind of preparation method of iron aluminium copper micropore filter material
CN111230118A (en) * 2020-01-14 2020-06-05 中南大学 A kind of FeAlSi intermetallic compound porous material and its preparation method and application
CN113584402A (en) * 2021-08-03 2021-11-02 西部宝德科技股份有限公司 Preparation method of iron-aluminum-chromium filtering material

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102580404A (en) * 2012-02-06 2012-07-18 江苏云才材料有限公司 Method for preparing asymmetric stainless steel filter disc
CN102580404B (en) * 2012-02-06 2014-05-28 江苏云才材料有限公司 Method for preparing asymmetric stainless steel filter disc
CN103361505A (en) * 2012-12-27 2013-10-23 华东理工大学 Preparation method of FeAl-based porous material
TWI551451B (en) * 2014-11-05 2016-10-01 The method of making high permeability materials
CN106191492A (en) * 2016-07-12 2016-12-07 东南大学 A kind of preparation method of high-purity FeGa3 intermetallic compound
CN109454231A (en) * 2018-12-18 2019-03-12 湖北汽车工业学院 A kind of preparation method of iron aluminium copper micropore filter material
CN109454231B (en) * 2018-12-18 2021-02-05 湖北汽车工业学院 A kind of preparation method of iron-aluminum-copper alloy microporous filter material
CN111230118A (en) * 2020-01-14 2020-06-05 中南大学 A kind of FeAlSi intermetallic compound porous material and its preparation method and application
CN113584402A (en) * 2021-08-03 2021-11-02 西部宝德科技股份有限公司 Preparation method of iron-aluminum-chromium filtering material
CN113584402B (en) * 2021-08-03 2022-11-08 西部宝德科技股份有限公司 A kind of preparation method of iron-aluminum-chromium filter material

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Open date: 20080123