CN104451344A - Large-aperture high-porosity porous iron and preparation method thereof - Google Patents
Large-aperture high-porosity porous iron and preparation method thereof Download PDFInfo
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- CN104451344A CN104451344A CN201410667837.1A CN201410667837A CN104451344A CN 104451344 A CN104451344 A CN 104451344A CN 201410667837 A CN201410667837 A CN 201410667837A CN 104451344 A CN104451344 A CN 104451344A
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Abstract
The invention discloses large-aperture high-porosity porous iron and a preparation method thereof, belonging to the technical field of preparation of porous materials. According to the technical scheme adopted by the invention, the preparation method of the large-aperture high-porosity porous iron comprises the following steps: 1) uniformly mixing a pore-forming agent with iron powder to obtain a material mixture, pressing and molding the material mixture, thereby obtaining a pre-pressed preform body; 2) treating the pre-pressed preform body with a diluted acid solution, then, cleaning the diluted acid solution with clear water, and finally putting the cleaned diluted acid solution in absolute ethyl alcohol to remove the pore-forming agent, thereby preparing a preform body; and 3) after sintering the preform body treated in the step 2), cooling, thereby preparing large-aperture high-porosity porous iron. The porous iron prepared by the preparation method disclosed by the invention is uniform in distribution, has density lower than 4g/cm<3>, porosity over 65%, a macroscopic macroporous dimension of 0.5mm-1.5mm, and certain strength (20-110MPa). Moreover, the preparation process of the material is simple, the equipment requirements are low, the cost is low, the practicability is strong, and the industrial production can be realized.
Description
Technical field
The invention belongs to porous metal material preparing technical field, be specifically related to a kind of wide aperture high porosity porous iron and preparation method thereof.
Background technology
Porous metal material is a kind of new metallic material with structure and function double attribute developed rapidly in the later stage eighties 20th century, is widely used in a lot of engineering field.Porous metal material is the metallic substance containing a certain amount of quantity, aperture and porosity in a kind of metallic matrix.Relative to compact metal material, porous metal have the characteristic of many excellences, as little in density, specific surface area is large, energy-absorbing damping performance is good, good penetrability, high temperature resistant, can regenerate, the feature such as can to process, be widely used in, in the techniques such as the filtration of the industries such as aerospace, nuclear power, electrochemistry, petrochemical complex, metallurgy, machinery, medicine, environmental protection, separation, noise reduction, catalysis, heat exchange, in aeroamphibious weaponry, communication, lightweight etc., also having potential purposes.
Iron is the essential substance in the earth's core, be also people know the most a kind of metal ([1] Liu Peisheng, porous material draws opinion [M]. Beijing: press of Tsing-Hua University, 2004).Iron has high-melting-point, density is large, the physicals of ductility and magnetic.As porous metal, porous iron has following several typical application: the hole that (1) is a large amount of because porous iron exists, and all plays an important role in damping antifriction field and in oil bearing etc.; (2) because the anti-compression properties of porous iron, energy absorption and resistance to elevated temperatures etc. are all better than the low melting point porous metal materials such as porous aluminum, more wide application prospect is all had in fields such as automobile making, shipbuilding, Highrise buildings, bridge and communications and transportation; ([2] wangdan. the present Research [J] of iron-based porous metal material. heat processing technique, 2011,40 (8): 75-83.) (3) filtering and purifying of preparing with porous iron, be separated field of purification at vehicle exhaust etc. and have application, it had both overcome porous polymer non-refractory, to isolate selectively shortcoming, compensate for again porous ceramics fragility high, deficiency ([3] Wu Wei of poor rigidity, the preparation of foamed iron material and the research [D] of performance thereof. University On The Mountain Of Swallows's Master's thesis, 2012).
The preparation method of current porous metal is mostly for the porous metal of low melting point, and the fusing point of iron is 1535 DEG C, and relatively high, preparation process is wayward, and preparation method is relatively less.But porous iron material has cheap relative to other porous metal materials, operating procedure is simple, and environmental pollution is little, the more high advantage of specific rigidity, is therefore have very much economic implications and social effect in the long run.
Summary of the invention
The object of the present invention is to provide a kind of wide aperture high porosity porous iron and preparation method thereof, the method is simple to operate, practical, and the porosity of the porous iron obtained through the method reaches 85%, even pore distribution, and density is little, and intensity is high.
The present invention is achieved through the following technical solutions:
A preparation method for wide aperture high porosity porous iron, comprises the following steps:
1) by pore-forming material and iron powder according to (1 ~ 3): the mass ratio of (9 ~ 7), fully mixes, and obtains mixture, by mixture compression moulding, obtains precompressed base substrate;
2) by precompressed base substrate first with after dilute acid soln process, then clean dilute acid soln with clear water, be finally statically placed in dehydrated alcohol to dissolve and remove pore-forming material, obtained base substrate;
3) will through step 2) after blank sintering after process, cooling, obtained wide aperture high porosity porous iron.
Described pore-forming material is CO (NH
2)
2particle, and this CO (NH
2)
2the particle diameter of particle is 1mm ~ 2mm.
Described iron powder is that fineness is less than 40 object straight iron powders.
Described iron powder is through pre-treatment before mixing with pore-forming material, and concrete operations are: by iron powder first with dilute acid soln cleaning, then after fully cleaning with clear water, under nitrogen protection atmosphere, carry out drying, finally soak with dehydrated alcohol.
Step 1) described in compression moulding be mixture is placed in punching block under pressing machine, be pressed into cylindrical precompressed base substrate, and adopt pressure be 300MPa ~ 600MPa.
Described punching block first removes punching block oxide on surface through dilute acid soln cleaning before use, then in basic solution and the dilute acid soln of punching block remained on surface, with lubricator lubricated steel die after finally being cleaned up by punching block with dehydrated alcohol.
Described dilute acid soln to be massfraction be 5% ~ 30% hydrochloric acid soln.
Step 3) described in sintering carry out in two stages, the first stage by base substrate by room temperature to 200 ~ 300 DEG C, insulation 1 ~ 3h; Subordinate phase is after base substrate being continued be warming up to 1000 ~ 1200 DEG C, sintering 1 ~ 4h.
Described sintering base substrate is placed in hot hole formula atmosphere protection resistance furnace, sinters under nitrogen protection atmosphere.
The density of this wide aperture high porosity porous iron is less than 4g/cm3, and porosity is 65% ~ 85%, and aperture is 0.5mm ~ 1.5mm, and intensity is 20 ~ 110MPa.
Compared with prior art, the present invention has following useful technique effect:
The preparation method of wide aperture disclosed by the invention high porosity porous iron, selects CO (NH
2)
2particle, as pore-forming material, can obtain the porous iron material that porosity reaches 85%.The present invention chooses CO (NH
2)
2particle is pore-forming material, is first because CO (NH
2)
2the very easily water-soluble and dehydrated alcohol of particle, is easy to molten and removes; Secondly due to CO (NH
2)
2particle fusing point is low, and heat treatment process easily removes residual CO (NH
2)
2; Last CO (NH
2)
2this can play the effect of lubrication in pressing process, is conducive to the density of raising pressed compact and is easy to move back mould.And if adopt the CO (NH of different mass mark
2)
2particle then can realize the controllability preparation of wide aperture high porosity porous iron.The inventive method technique is simple, low for equipment requirements, and raw material sources are extensive, environmental friendliness, is applicable to industrialization scale operation.
The density of the porous iron obtained through the inventive method is less than 4g/cm
3, porosity is 65% ~ 85%, and aperture is 0.5mm ~ 1.5mm, and intensity is 20 ~ 110MPa.
Accompanying drawing explanation
Fig. 1 is the macrostructure figure of porous iron prepared by the embodiment of the present invention 1;
Fig. 2 is the stress-strain diagram of porous iron prepared by the embodiment of the present invention 1.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
The technical solution adopted in the present invention is:
Adopt powder sintering to prepare a method for wide aperture high porosity porous iron, comprise the steps:
Step 1: the pre-treatment of iron powder;
Iron powder is first with the diluted acid cleaning of certain mass mark; to remove the oxide compound on iron powder surface, then with dry in nitrogen protection loft drier after the abundant washes clean of clear water, finally add a certain amount of dehydrated alcohol and soak; dehydrated alcohol is as caking agent herein, is convenient to iron powder and CO (NH
2)
2particle mixes.
This CO (NH
2)
2the particle diameter of particle is 1mm ~ 2mm, and iron powder is that fineness is less than 40 object straight iron powders.
Step 2: with CO (NH
2)
2particle is pore-forming material, the material that pore-forming material and step 1 are obtained be in mass ratio 1 ~ 3:9 ~ 7 ratio together be placed in planetary mixer and fully mix;
Choose CO (NH
2)
2particle is pore-forming material is because CO (NH on the one hand
2)
2the very easily water-soluble and dehydrated alcohol of particle, is easy to molten and removes; Secondly CO (NH
2)
2particle fusing point is low, and heat treatment process easily removes residual CO (NH
2)
2; CO (NH in addition
2)
2this can play the effect of lubrication in pressing process, is conducive to the density of raising pressed compact and is easy to move back mould.
Step 3: the mixture obtained in step 2 is placed in punching block is pressed into cylindrical preformed compact under pressing machine, the pressure selected is 300MPa ~ 600MPa;
Pressed compact front mold needs first with diluted acid cleaning, removing die surface oxide compound, then with diluted acid residual with die surface in basic solution, is finally totally lubricated afterwards by mold clean with dehydrated alcohol.
Step 4: the preformed compact that suppresses is left standstill 5 ~ 10 minutes in diluted acid, the removing preformed compact oxide compound that surface produces in pressing process, cleans up diluted acid with clear water afterwards, then puts into dehydrated alcohol and dissolve part pore-forming material;
Step 5: step 4 gained material is put into hot hole formula atmosphere protection resistance furnace (employing nitrogen protection) and sinter, i.e. obtained porous iron.
Sintering is divided into two stages, and the first stage be by blank by room temperature to 200 DEG C ~ 300 DEG C, insulation 1 ~ 3h, the urea that removing remains; Subordinate phase is warming up to 1000 DEG C ~ 1200 DEG C sintering 1 ~ 4h for being continued by blank, finally takes out sample and is chilled to room temperature.
Specific embodiment
Embodiment 1
A preparation method for wide aperture high porosity porous iron, comprises the following steps:
(1) CO (NH that mass ratio is 1 ~ 2:9 ~ 8 is chosen
2)
2particle and iron powder (iron powder is less than 40 orders), iron powder first with diluted acid cleaning, then with dry in nitrogen protection loft drier after the abundant washes clean of clear water, finally add a certain amount of dehydrated alcohol and soaks.
(2) by CO (NH
2)
2particle and iron powder are placed in planetary mixer and carry out batch mixing.
(3) by mould first with diluted acid cleaning, then with basic solution cleaning, lubricated dies after finally mold clean is clean with dehydrated alcohol.
(4) mixed material is placed in mould and is pressed into preformed compact under 500 ~ 600MPa.
(5) preformed compact that suppresses first leaves standstill 5 ~ 10 minutes in diluted acid, is rinsed well by diluted acid afterwards with clear water, then puts into dehydrated alcohol and dissolve part pore-forming material, obtained base substrate.
(6) base substrate is placed in hot hole formula atmosphere protection resistance furnace, adopts nitrogen protection, point two stages sinter, and the first stage be by blank by room temperature to 200 DEG C ~ 300 DEG C, insulation 1 ~ 3h, the urea that removing remains; Subordinate phase is warming up to 1000 DEG C ~ 1200 DEG C sintering 1 ~ 4h for being continued by blank, finally takes out sample and is chilled to room temperature, obtained wide aperture high porosity porous iron.
The density of the wide aperture high porosity porous iron of gained is 3.948g/cm
3; Fig. 1 is the macrostructure figure of the wide aperture high porosity porous iron that the present embodiment obtains, in figure, white portion is the sample hole that white chalk dust is filled, black part is divided into metallic iron powder, the mean sizes measuring this porous iron macroporosity with IPP analysis software is about 0.63mm, by calculating white (hole) part area occupied ratio, show that mean porosities is 68.8%; Compressive strength is 109.4MPa, Fig. 2 is the stress-strain diagram that the present embodiment obtains porous iron, and vertex is compressive strength maximum, and its value is 109.4MPa.
Embodiment 2
A preparation method for wide aperture high porosity porous iron, comprises the following steps:
(1) CO (NH that mass ratio is 2 ~ 3:8 ~ 7 is chosen
2)
2particle and iron powder (<40 order), iron powder first with diluted acid cleaning, then with dry in nitrogen protection loft drier after the abundant washes clean of clear water, finally add a certain amount of dehydrated alcohol and soaks.
(2) by CO (NH
2)
2particle and iron powder are placed in planetary mixer and carry out batch mixing.
(3) by mould first with diluted acid cleaning, then with basic solution cleaning, lubricated dies after finally mold clean is clean with dehydrated alcohol.
(4) mixed material is placed in mould and is pressed into preformed compact under 300 ~ 400MPa.
(5) preformed compact that suppresses first leaves standstill 5 ~ 10 minutes in diluted acid, is rinsed well by diluted acid afterwards with clear water, then puts into dehydrated alcohol and dissolve part pore-forming material, obtained base substrate.
(6) base substrate is placed in hot hole formula atmosphere protection resistance furnace, adopts nitrogen protection, point two stages sinter, and the first stage be by blank by room temperature to 200 DEG C ~ 300 DEG C, insulation 1 ~ 3h, the urea that removing remains; Subordinate phase is warming up to 1000 DEG C ~ 1200 DEG C sintering 1 ~ 4h for being continued by blank, finally takes out sample and is chilled to room temperature, obtained wide aperture high porosity porous iron.
The porous iron density of the present embodiment gained is 1.991g/cm
3, the mean sizes of macroporosity is about 1.43mm, and porosity is 84.3%, and compressive strength is 21.3MPa.
Embodiment 3
A preparation method for wide aperture high porosity porous iron, comprises the following steps:
(1) CO (NH that mass ratio is 2:8 is chosen
2)
2particle and iron powder (<40 order), iron powder is first 10% hydrochloric acid soln cleaning with massfraction, then with dry in nitrogen protection loft drier after the abundant washes clean of clear water, finally add a certain amount of dehydrated alcohol and soak.
(2) by CO (NH
2)
2particle and iron powder are placed in planetary mixer and carry out batch mixing.
(3) be first 10% hydrochloric acid cleaning with massfraction by mould, then with basic solution cleaning, lubricated dies after finally mold clean is clean with dehydrated alcohol.
(4) mixed material is placed in mould and is pressed into preformed compact under 300MPa.
(5) preformed compact that suppresses is first leave standstill 5 minutes in 10% hydrochloric acid soln at massfraction, is rinsed well by diluted acid afterwards with clear water, then puts into dehydrated alcohol and dissolve part pore-forming material, obtained base substrate.
(6) base substrate is placed in hot hole formula atmosphere protection resistance furnace, adopts nitrogen protection, point two stages sinter, and the first stage is by blank by room temperature to 200 DEG C, insulation 1h, the urea that removing is residual; Subordinate phase is warming up to 1000 DEG C of sintering 4h for being continued by blank, finally takes out sample and is chilled to room temperature, obtained wide aperture high porosity porous iron.
The porous iron density of the present embodiment gained is 2.582g/cm
3, the mean sizes of macroporosity is about 0.72mm, and porosity is 79.6%, and compressive strength is 71.1MPa.
Embodiment 4
A preparation method for wide aperture high porosity porous iron, comprises the following steps:
(1) CO (NH that mass ratio is 1:9 is chosen
2)
2particle and iron powder (<40 order), iron powder is first 20% hydrochloric acid soln cleaning with massfraction, then with dry in nitrogen protection loft drier after the abundant washes clean of clear water, finally add a certain amount of dehydrated alcohol and soak.
(2) by CO (NH
2)
2particle and iron powder are placed in planetary mixer and carry out batch mixing.
(3) be first 20% hydrochloric acid cleaning with massfraction by mould, then with basic solution cleaning, lubricated dies after finally mold clean is clean with dehydrated alcohol.
(4) mixed material is placed in mould and is pressed into preformed compact under 500MPa.
(5) preformed compact that suppresses is first leave standstill 5 minutes in 20% hydrochloric acid soln at massfraction, is rinsed well by diluted acid afterwards with clear water, then puts into dehydrated alcohol and dissolve part pore-forming material, obtained base substrate.
(6) base substrate is placed in hot hole formula atmosphere protection resistance furnace, adopts nitrogen protection, point two stages sinter, and the first stage is by blank by room temperature to 260 DEG C, insulation 1h, the urea that removing is residual; Subordinate phase is warming up to 1100 DEG C of sintering 3h for being continued by blank, finally takes out sample and is chilled to room temperature, obtained wide aperture high porosity porous iron.
The porous iron density of the present embodiment gained is 3.525g/cm
3, the mean sizes of macroporosity is about 0.82mm, and porosity is 72.2%, and compressive strength is 93.4MPa.
Embodiment 5
A preparation method for wide aperture high porosity porous iron, comprises the following steps:
(1) CO (NH that mass ratio is 3:7 is chosen
2)
2particle and iron powder (<40 order), iron powder is first 30% hydrochloric acid soln cleaning with massfraction, then with dry in nitrogen protection loft drier after the abundant washes clean of clear water, finally add a certain amount of dehydrated alcohol and soak.
(2) by CO (NH
2)
2particle and iron powder are placed in planetary mixer and carry out batch mixing.
(3) be first 30% hydrochloric acid cleaning with massfraction by mould, then with basic solution cleaning, lubricated dies after finally mold clean is clean with dehydrated alcohol.
(4) mixed material is placed in mould and is pressed into preformed compact under 600MPa.
(5) preformed compact that suppresses is first leave standstill 5 minutes in 30% hydrochloric acid soln at massfraction, is rinsed well by diluted acid afterwards with clear water, then puts into dehydrated alcohol and dissolve part pore-forming material, obtained base substrate.
(6) base substrate is placed in hot hole formula atmosphere protection resistance furnace, adopts nitrogen protection, point two stages sinter, and the first stage is by blank by room temperature to 300 DEG C, insulation 1h, the urea that removing is residual; Subordinate phase is warming up to 1200 DEG C of sintering 2h for being continued by blank, finally takes out sample and is chilled to room temperature, obtained wide aperture high porosity porous iron.
The porous iron density of the present embodiment gained is 2.414g/cm
3, the mean sizes of macroporosity is about 1.25mm, and porosity is 80.9%, and compressive strength is 31.8MPa.
Claims (10)
1. a preparation method for wide aperture high porosity porous iron, is characterized in that, comprises the following steps:
1) by pore-forming material and iron powder according to (1 ~ 3): the mass ratio of (9 ~ 7), fully mixes, and obtains mixture, by mixture compression moulding, obtains precompressed base substrate;
2) by precompressed base substrate first with after dilute acid soln process, then clean dilute acid soln with clear water, be finally statically placed in dehydrated alcohol to dissolve and remove pore-forming material, obtained base substrate;
3) will through step 2) after blank sintering after process, cooling, obtained wide aperture high porosity porous iron.
2. the preparation method of a kind of wide aperture according to claim 1 high porosity porous iron, it is characterized in that, described pore-forming material is CO (NH
2)
2particle, and this CO (NH
2)
2the particle diameter of particle is 1mm ~ 2mm.
3. the preparation method of a kind of wide aperture according to claim 1 high porosity porous iron, is characterized in that, described iron powder is that fineness is less than 40 object straight iron powders.
4. the preparation method of a kind of wide aperture according to claim 1 high porosity porous iron; it is characterized in that; described iron powder before mixing with pore-forming material through pre-treatment; concrete operations are: first cleaned with dilute acid soln by iron powder; after fully cleaning with clear water again; under nitrogen protection atmosphere, carry out drying, finally soak with dehydrated alcohol.
5. the preparation method of a kind of wide aperture according to claim 1 high porosity porous iron, it is characterized in that, step 1) described in compression moulding be mixture is placed in punching block under pressing machine, be pressed into cylindrical precompressed base substrate, and adopt pressure be 300MPa ~ 600MPa.
6. the preparation method of a kind of wide aperture according to claim 5 high porosity porous iron, it is characterized in that, described punching block first removes punching block oxide on surface through dilute acid soln cleaning before use, again in basic solution and the dilute acid soln of punching block remained on surface, with lubricator lubricated steel die after finally punching block being cleaned up with dehydrated alcohol.
7. the preparation method of a kind of wide aperture high porosity porous iron according to claim 1 or 4 or 6, is characterized in that, described dilute acid soln to be massfraction be 5% ~ 30% hydrochloric acid soln.
8. the preparation method of a kind of wide aperture according to claim 1 high porosity porous iron, is characterized in that, step 3) described in sintering carry out in two stages, the first stage by base substrate by room temperature to 200 ~ 300 DEG C, insulation 1 ~ 3h; Subordinate phase is after base substrate being continued be warming up to 1000 ~ 1200 DEG C, sintering 1 ~ 4h.
9. the preparation method of a kind of wide aperture high porosity porous iron according to claim 1 or 8, is characterized in that, described sintering base substrate is placed in hot hole formula atmosphere protection resistance furnace, sinters under nitrogen protection atmosphere.
10. adopt the wide aperture high porosity porous iron that the method in claim 1 ~ 9 described in any one is obtained, it is characterized in that, the density of this wide aperture high porosity porous iron is less than 4g/cm
3, porosity is 65% ~ 85%, and aperture is 0.5mm ~ 1.5mm, and intensity is 20 ~ 110MPa.
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Cited By (1)
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| CN105803298A (en) * | 2016-04-22 | 2016-07-27 | 西安建筑科技大学 | Method for preparing blister steel from pore forming agent |
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| CN104451344B (en) | 2016-08-31 |
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