CN109454231A - A kind of preparation method of iron aluminium copper micropore filter material - Google Patents

A kind of preparation method of iron aluminium copper micropore filter material Download PDF

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Publication number
CN109454231A
CN109454231A CN201811546122.5A CN201811546122A CN109454231A CN 109454231 A CN109454231 A CN 109454231A CN 201811546122 A CN201811546122 A CN 201811546122A CN 109454231 A CN109454231 A CN 109454231A
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powder
iron
copper
aluminium
temperature
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CN109454231B (en
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沈培智
罗成
赵红利
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Hubei University of Automotive Technology
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Hubei University of Automotive Technology
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    • 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
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027—Metallic material
    • 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
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • 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
    • B22F3/1017—Multiple heating or additional steps
    • 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
    • B22F3/1103—Making porous workpieces or articles with particular physical characteristics
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
    • B22F5/106—Tube or ring forms
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper

Abstract

The invention discloses a kind of preparation methods of iron aluminium copper micropore filter material, step includes: that (1) to choose average grain diameter be that 1~100 micron of iron powder, aluminium powder and copper powder mixes by mass percentage, wherein Cu is 4~20%, and the 80~69% of surplus are Fe, 20~31% are Al；(2) green compact are made using molding or cold isostatic compaction, 100~300MPa of pressure are controlled, within dwell time 10min；(3) powder metallurgical sintering process is used, sintering atmosphere is hydrogen or inert atmosphere or vacuum-sintering, first 120~150OC keeps the temperature 30~60 minutes, then with 1~10OC/min speed rises to 580~620OC, and 60~120 minutes are kept the temperature at such a temperature, then with 1~10OC/min speed rises to 1000~1200O,C keeps the temperature 30~120 minutes；Cooling stage is higher than 500OIt is 5~20 that rate of temperature fall is controlled when COC/min.This method is not required to addition pore creating material, and pollution-free, product strength is high, and high temperature oxidation resistance and excellent in sour resistance, filtering material pore structure is controllable and strainability is good, and running resistance is low, easily recoil regeneration.

Description

A kind of preparation method of iron aluminium copper micropore filter material
Technical field
The present invention relates to the technologies of preparing of filtering material, and in particular to a kind of preparation of iron aluminium copper micropore filter material Method.
Background technique
In the modern industrial production process, the solid gas or solid-liquid that filtering material is usually used in mixing multiple groups part separate, Classification, purification and enrichment, have energy-efficient, simple process, and small investment pollutes the advantages that small, is widely used in chemical industry, cure Medicine, the fields such as environmental protection.With the continuous improvement of environmental protection requirement, temperature Gas Dedusting Technologies are had attracted much attention, core It is high-performance filtration material.Bad for thermal shock resistance existing for ceramic filter material, the problems such as reliability is not high enough, the world is each State has carried out the research and development of advanced metal porous filtering material, and wherein ferro-aluminum alloy porous material is with its excellent oxygen resistant to high temperatures Change and resistance to vulcanization corrosive nature is suitble to work under high-temperature corrosion environment.Preparation method has following two:
(1) method that ferro-aluminum alloy porous material is prepared as raw material sintering using ferroaluminium powder is taken, there are alloy powders Price is high and powder shape, ingredient and granularity selection range are small, needs to add pore creating material, lubricant, bonding agent in mixing process Wait the problems such as auxiliary elements and sintering process temperature are high, the time is long, exhaust emission is more serious.
(2) ferro-aluminum alloy porous material is synthetically prepared using iron, aluminium element powdered reaction, due to iron in high-temperature sintering process Powder and aluminium powder easily occur to react from climing combustion, it is prominent to lead to material problem on deformation, and material temperature-room type plasticity is not high, and brittleness is larger, cause Make its with post-processing be assembled into filter element and filter element performance in terms of there are problems.
The adverse effect caused by product shape is reacted in order to reduce from climing combustion, has researcher to propose (1) in the fusing point of aluminium Under carry out long-time heat preservation, using solid phase reaction substep generate intermediate product, reduce a large amount of iron powders and aluminium powder directly generate iron The amount of heat generated when aluminium alloy avoids occurring from climing combustion, but this method sintering time is long, and the requirement to equipment and technique is very It is high；(2) inert powders such as a certain proportion of silica or silicon carbide are added in element powders, are reduced between iron powder, aluminium powder Contact area, weakened and slowing down the speed chemically reacted under high temperature from climing combustion react be inclined to.This method can alleviate production The problem on deformation of object, but to the microcellular structure and high-temperature oxidation resistance of porous material without improvement result.
Therefore it develops a kind of novel problem on deformation that can not only improve iron Lu porous material but also can to improve its again micro- The new material of pore structure and high-temperature oxidation resistance has great importance.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of preparation methods of iron aluminium copper micropore filter material, should Preparation method can greatly improve green compact near-net forming during the sintering process and gas permeability, high temperature oxidation resistance of filter material etc. Performance, so that filter efficiency is high in the process of running for filter elements, running resistance is low, and process stabilizing is easy to the cleaning and regeneration that recoils.
For this purpose, the technical solution of the present invention is as follows: a kind of preparation method of iron aluminium copper micropore filter material, specific to prepare Steps are as follows:
(1) powder is prepared: being chosen iron powder, aluminium powder and copper powder that average grain diameter is 1~100 micron, is carried out by mass percentage Proportion: Cu is 4~20%, and Fe is 80~69% in remaining content, Al is 20~31%；
(2) compression moulding: sheet or tubulose green compact are made using molding or cold isostatic compaction, in which: pressure is controlled 100 ~300MPa, dwell time control within 10min；
(3) green sintering: sintering atmosphere is hydrogen or inert atmosphere or vacuum state, in which: vacuum when using vacuum-sintering Degree is less than 1 × 10-2Pa；Specific sintering process are as follows: first by green compact obtained in (2) 120~150O30~60 points are kept the temperature under C Clock, then with 1~10OThe heating rate of C/min rises to 580~620OC, and 60~120 minutes are kept the temperature at such a temperature, then with 1 ~10OThe heating rate of C/min rises to 1000~1200O,C keeps the temperature 30~120 minutes；Cooling stage is finally entered, is higher than 500OIt is 5~20 that cooling rate is controlled when COC/min is to get the iron aluminium copper micropore filter material.
Preferably, selecting average particle size is 3~5 μm of copper powder, 3~5 μm of iron powder and 10 μm of aluminium powder, by quality hundred Point ratio is matched, wherein Cu be 4%, Fe 76%, Al 20%.
Preferably, selecting average particle size is 10 μm of copper powder, 3~5 μm of iron powder and 20 μm of aluminium powder, by quality percentage Than being matched, wherein Cu be 8%, Fe 70%, Al 22%.
Preferably, selecting average particle size for 38 μm of copper powder, 38 μm of iron powder and 38 μm of aluminium powder, by mass percentage Matched, wherein Cu be 12%, Fe 67%, Al 21%.
Preferably, selecting average particle size for 74 μm of copper powder, 74 μm of iron powder and 38 μm of aluminium powder, by mass percentage Matched, wherein Cu be 16%, Fe 64%, Al 20%.
Preferably, selecting average particle size for 74 μm of copper powder, 74 μm of iron powder and 74 μm of aluminium powder, by mass percentage Matched, wherein Cu be 20%, Fe 61%, Al 19%.
The utility model has the advantages that the present invention prepares the new process of iron aluminium copper filtering material using iron aluminum bronze element powders, it can be big Width improves the high temperature oxidation resistance and corrosion resistance of inorganic filter material, almost pollution-free.Compared with prior art, this hair It is bright to have the advantage that
1, FeAl alloy has excellent resistance to high temperature oxidation, curability, is suitable for being prepared into inorganic filter material.The present invention can Significantly improve as iron, aluminium element powder at high temperature from climing combustion reaction and caused by deformation of products cracking phenomena (see Fig. 1 (a) shown in), the FeAlCu porous material shapes prepared stablize (see shown in Fig. 1 (b)).
2, the addition of copper is so that the even pore distribution of iron aluminium copper porous filter material is further changed It is kind, additive is not needed in preparation process, product microcellular structure is easy to regulate and control, porosity be up to 30%~40%(see Fig. 2 (a b C d) shown in).
3, iron aluminium copper porous filter material and FeAl porous filter material phase are synthetically prepared using element powders reaction Than, high-temperature oxidation resistance is improved (as shown in Figure 3), and it is high-efficient that product can carry out being machined etc. post-processing filtering, Running resistance is low, is easy to blowback.
Detailed description of the invention
Fig. 1 (a) is existing using iron and aluminium powder as raw material, occurs to react from climing combustion, the iron Lu porous material of preparation.
Fig. 1 (b) is of the invention using the powder of iron, aluminium and copper as raw material, reaction front and back green compact and iron aluminum bronze porous material Comparison diagram.
Fig. 2 (a) is the microscopic appearance figure of iron aluminium copper porous material prepared by the embodiment of the present invention 2.
Fig. 2 (b) is the microscopic appearance figure of iron aluminium copper porous material prepared by the embodiment of the present invention 3.
Fig. 2 (c) is the microscopic appearance figure of iron aluminium copper porous material prepared by the embodiment of the present invention 4.
Fig. 2 (d) is the microscopic appearance figure of iron aluminium copper porous material prepared by the embodiment of the present invention 5.
Fig. 3 is the oxygen of the different Cu content sample of iron aluminium copper porous material of the invention when temperature reaches 600 DEG C Change weight gain curve.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.
Below with reference to specific implementation example, the invention will be further described.
Embodiment 1:
Using 3~5 μm of copper powder of average particle size, 3~5 μm of iron powder and 10 μm of aluminium powder, Cu:Fe:Al=4 by mass percentage: 76:20 composition proportion carries out mixing, is then pressed and molded under the pressure of 200MPa, diameter 32mm is made, 1~2mm's of thickness Sheet green compact；Green compact use non-pressure sintering technology, keep the temperature 30 minutes at 120 DEG C, then rise to 580 with the heating rate of 5 DEG C/min DEG C and keep the temperature 60min, then rise to 1000 DEG C with the heating rate of 5 DEG C/min, keep the temperature 120 minutes, sintering atmosphere is hydrogen, with Furnace cooling, the iron aluminum bronze sheet-like filter material thus prepared, porosity 30%, maximum diameter of hole are 1.5 μm.
Embodiment 2:
Using 10 μm of copper powder of average particle size, 3~5 μm of iron powder and 20 μm of aluminium powder, Cu:Fe:Al=8 by mass percentage: 70:22 composition proportion carries out mixing, then under the pressure of 150MPa, using compression molding, is made diameter 32mm, and thickness 1~ The sheet green compact of 2mm；Green compact use non-pressure sintering technology, keep the temperature 30 minutes at 120 DEG C, then with the heating rate liter of 5 DEG C/min To 600 DEG C and 60min is kept the temperature, then rises to 1050 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 90 minutes, sintering atmosphere is hydrogen Gas cools down with furnace, the iron aluminum bronze sheet-like filter material thus prepared, porosity 32%, and maximum diameter of hole is 2.1 μm.
Embodiment 3:
Using 38 μm of copper powder of average particle size, 38 μm of iron powder and 38 μm of aluminium powder, Cu:Fe:Al=12:67 by mass percentage: 21 composition proportions carry out mixing, are then pressed and molded under the pressure of 200MPa, diameter 32mm, the sheet of 1~2mm of thickness is made Green compact；Green compact use non-pressure sintering technology, keep the temperature 30 minutes at 120 DEG C, then rise to 620 DEG C simultaneously with the heating rate of 5 DEG C/min 80min is kept the temperature, then rises to 1100 DEG C with the heating rate of 8 DEG C/min, keeps the temperature 60 minutes, sintering atmosphere is hydrogen, is dropped with furnace Temperature, the iron aluminum bronze sheet-like filter material thus prepared, porosity 35%, maximum diameter of hole are 4.1 μm.
Embodiment 4:
Using 74 μm of copper powder of average particle size, 74 μm of iron powder and 38 μm of aluminium powder, Cu:Fe:Al=16:64 by mass percentage: 20 composition proportions carry out mixing, are then pressed and molded under the pressure of 250MPa, diameter 32mm, the sheet of 1~2mm of thickness is made Green compact；Green compact use vacuum sintering technology, and vacuum degree is 1 × 10-2Pa keeps the temperature 30 minutes at 120 DEG C, then with the liter of 5 DEG C/min Warm speed rises to 620 DEG C and keeps the temperature 120min, then rises to 1050 DEG C with the heating rate of 8 DEG C/min, 40min is kept the temperature, with furnace Cooling, the iron aluminum bronze sheet-like filter material thus prepared, porosity 38%, maximum diameter of hole are 6.3 μm.
Embodiment 5:
Use average particle size for 74 μm of copper powders, 74 μm of iron powder and 74 μm of aluminium powder, by mass percentage Cu:Fe:Al=20:61: 19 composition proportions carry out mixing, are then pressed and molded under the pressure of 300MPa, diameter 32mm, the sheet of 1~2mm of thickness is made Green compact；Green compact use vacuum sintering technology, and control vacuum degree is 1 × 10-2Pa keeps the temperature 30 minutes at a temperature of 120 DEG C, then with 5 DEG C/heating rate of min rises to 620 DEG C and keeps the temperature 120min, 1200 DEG C then are risen to the heating rate of 5 DEG C/min, heat preservation After forty minutes, with 20 DEG C/min cooling, the iron aluminum bronze sheet-like filter material thus prepared, porosity 39%, maximum diameter of hole is 8.5 μ m。
Core of the invention is: iron powder, aluminium powder and copper powder that average grain diameter is 1~100 micron is chosen, by quality hundred Divide than carrying out ingredient, in which: Cu is 4~20%, and Fe, by cold-press moulding, reburns containing 80~69%, Al containing 20~31% in surplus Knot sizing, a kind of iron aluminium copper micropore filter material obtained；
Addition pore creating material is not needed using the preparation method, preparation process is pollution-free, compared with prior art, product tool obtained There is intensity high, high temperature oxidation resistance and excellent in sour resistance, the pore structure of filtering material is controllable, and strainability is good, running resistance It is low, it is easy to the advantages of regenerating of recoiling.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Made any modification, improvement etc., should all be included in the protection scope of the present invention within principle.

Claims (6)

1. a kind of preparation method of iron aluminium copper micropore filter material, specific preparation process is as follows:
(1) powder is prepared: being chosen iron powder, aluminium powder and copper powder that average grain diameter is 1~100 micron, is carried out by mass percentage Proportion: Cu is 4~20%, and Fe is 80~69% in remaining content, Al is 20~31%；
(2) compression moulding: sheet or tubulose green compact are made using molding or cold isostatic compaction, in which: pressure is controlled 100 ~300MPa, dwell time control within 10min；
(3) green sintering: sintering atmosphere is hydrogen or inert atmosphere or vacuum state, in which: vacuum when using vacuum-sintering Degree is less than 1 × 10-2Pa；Specific sintering process are as follows: first by green compact obtained in (2) 120~150O30~60 points are kept the temperature under C Clock, then with 1~10OThe heating rate of C/min rises to 580~620OC, and 60~120 minutes are kept the temperature at such a temperature, then with 1 ~10OThe heating rate of C/min rises to 1000~1200O,C keeps the temperature 30~120 minutes；Cooling stage is finally entered, is higher than 500OIt is 5~20 that cooling rate is controlled when COC/min is to get the iron aluminium copper micropore filter material.
2. a kind of preparation method of iron aluminium copper micropore filter material according to claim 1, it is characterised in that: select Average particle size is 3~5 μm of copper powder, 3~5 μm of iron powder and 10 μm of aluminium powder, is matched by mass percentage, wherein Cu is 4%, Fe 76%, Al 20%.
3. a kind of preparation method of iron aluminium copper micropore filter material according to claim 1, it is characterised in that: select Average particle size is 10 μm of copper powder, 3~5 μm of iron powder and 20 μm of aluminium powder, is matched by mass percentage, wherein Cu is 8%, Fe 70%, Al 22%.
4. a kind of preparation method of iron aluminium copper micropore filter material according to claim 1, it is characterised in that: select Average particle size be 38 μm of copper powder, 38 μm of iron powder and 38 μm of aluminium powder, matched by mass percentage, wherein Cu be 12%, Fe is 67%, Al 21%.
5. a kind of preparation method of iron aluminium copper micropore filter material according to claim 1, it is characterised in that: select Average particle size be 74 μm of copper powder, 74 μm of iron powder and 38 μm of aluminium powder, matched by mass percentage, wherein Cu be 16%, Fe is 64%, Al 20%.
6. a kind of preparation method of iron aluminium copper micropore filter material according to claim 1, it is characterised in that: select Average particle size be 74 μm of copper powder, 74 μm of iron powder and 74 μm of aluminium powder, matched by mass percentage, wherein Cu be 20%, Fe is 61%, Al 19%.
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Cited By (3)

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CN111230118A (en) * 2020-01-14 2020-06-05 中南大学 FeAlSi intermetallic compound porous material and preparation method and application thereof
CN113427002A (en) * 2021-06-25 2021-09-24 哈尔滨工业大学 Pressureless sintering preparation method of three-dimensional porous structure
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

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CN111230118A (en) * 2020-01-14 2020-06-05 中南大学 FeAlSi intermetallic compound porous material and preparation method and application thereof
CN113427002A (en) * 2021-06-25 2021-09-24 哈尔滨工业大学 Pressureless sintering preparation method of three-dimensional porous structure
CN113427002B (en) * 2021-06-25 2022-06-21 哈尔滨工业大学 Pressureless sintering preparation method of three-dimensional porous structure
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 Preparation method of iron-aluminum-chromium filtering material

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