CN111230118A - FeAlSi intermetallic compound porous material and preparation method and application thereof - Google Patents
FeAlSi intermetallic compound porous material and preparation method and application thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
- B22F3/1039—Sintering only by reaction
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- 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
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- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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Abstract
The invention relates to a FeAlSi intermetallic compound porous material and a preparation method and application thereof, wherein the porous material comprises the following components in percentage by mass: fe71.25-74.25 wt%; al23.75-24.75 wt.%; si 1-5 wt.%; the porosity of the porous material is 40-60%, the porous material has sufficient porosity and can be used for filtering materials, the porous material has excellent mechanical properties, high temperature resistance and corrosion resistance, and compared with a FeAl intermetallic compound porous material, the preparation method of the FeAlSi intermetallic compound porous material provided by the invention can prepare the FeAl (Si) porous material only by element mixing, die forming and a solid-state partial diffusion-reaction synthesis method.
Description
Technical Field
The invention relates to a FeAlSi intermetallic compound porous material and a preparation method and application thereof, belonging to the technical field of porous material preparation.
Background
The FeAl intermetallic compound porous material has the advantages of low cost, low density, good mechanical property and machining property, high-temperature oxidation resistance, vulcanization resistance and the like, and is considered to be a high-temperature filter material with high competitiveness. However, in the preparation process of the FeAl porous material, the Fe and the liquid Al generate violent exothermic reaction to initiate self-propagating reaction, so that the near-net shape of the material is seriously damaged, the pore structure is difficult to control, and the mechanical property is damaged. The existing method adopts slow temperature rise to prolong the low-temperature heat preservation time, so that Al element is consumed to form a diffusion layer with a certain thickness to inhibit the occurrence of violent self-propagating reaction. However, the product produced by the method still has the possibility of cracking deformation, and needs long-time heat preservation, thereby causing waste of energy and time.
At present, a diluent method is mainly adopted to control the self-propagating reaction in the element powder reaction process, external element powder is added into mixed powder to inhibit the self-propagating process, Si element is an important material for preparing metal ceramics, and the metal ceramic composite material prepared by the Si element inherits the respective advantages of metal and ceramic and makes up the defects of the metal and ceramic.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a FeAlSi intermetallic compound porous material and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a FeAlSi intermetallic compound porous material, which comprises the following components in percentage by mass: fe 71.25-74.25 wt%; 23.75-24.75 wt.% Al; si 1-5 wt.%; the porosity of the porous material is 40-60%.
In a preferred scheme, the porous material comprises the following components in percentage by mass: fe72.75-74.25 wt%; 24.25-24.75 wt.% Al; si 1-3 wt.%.
The FeAlSi intermetallic compound porous material provided by the invention has sufficient porosity for filtering materials, and also has excellent mechanical properties, high temperature resistance and corrosion resistance.
The invention relates to a FeAlSi intermetallic compound porous material, which comprises the following steps: the preparation method comprises the following steps of mixing iron powder, aluminum powder and silicon powder according to a designed proportion to obtain mixed powder, pressing and molding the mixed powder, and sintering to obtain the FeAlSi intermetallic compound porous material, wherein the sintering process comprises the following steps: heating to 120 ℃ at the speed of 3-7 ℃/min, preserving heat for 0.5-1h, then heating to 620 ℃ at the speed of 3-7 ℃/min, preserving heat for 0.5-1h, heating to 1120 ℃ to 1180 ℃ at the speed of 3-7 ℃/min, and preserving heat for 1-2 h.
In the preferred scheme, the iron powder is reduced iron powder, the particle size of the reduced iron powder is 250-400 meshes, and the purity of the reduced iron powder is more than or equal to 99.9%.
In a preferred scheme, the aluminum powder is atomized aluminum powder, the particle size of the atomized aluminum powder is 300-400 meshes, and the purity of the atomized aluminum powder is more than or equal to 99.9 percent.
In the preferable scheme, the particle size of the silicon powder is 600-800 meshes, and the purity is more than or equal to 99.9%.
In a preferred embodiment, the mixed powder comprises the following components in percentage by mass: 71.25-74.25 wt% of Fe powder; 23.75-24.75 wt.% of Al powder; 1-5 wt.% of Si powder
In the invention, the raw materials meeting the particle size requirement of the invention are prepared according to the range of the raw materials, and then the pressing pressure and the sintering procedure of the invention are combined, so that the FeAlSi intermetallic compound porous material which has high bonding strength, high porosity and uniform distribution can be obtained.
It can be seen that the FeAlSi intermetallic compound porous material with the required porosity can be obtained without pore-forming agents, and the FeAlSi intermetallic compound porous material does not need to be mixed again and degreased because the pore-forming agents do not need to be added, so that the process flow of the porous material is greatly simplified compared with that of the common porous material.
In a preferable scheme, the mixing is carried out in a mixer, the mixing rotating speed is 60-100rpm, and the mixing time is 12-24 h.
Preferably, the pressure for compression molding is 100-150 MPa.
In the actual operation process, the uniformly mixed powder raw materials are pressed into a required blank body by an oil press.
In a preferred embodiment, the sintering is performed in a vacuum environment.
And after sintering, cooling to room temperature along with the furnace.
The invention relates to an application of a FeAlSi intermetallic compound porous material, which is applied to a filter material. Especially applied to the field of high-temperature filtration and separation.
The invention has the beneficial effects that:
(1) the invention innovatively provides a method for preparing a FeAl (Si) porous material by adding Si element to inhibit the self-propagating reaction, and selecting element mixing, die pressing forming and solid partial diffusion-reaction synthesis.
(2) The preparation method of the FeAlSi intermetallic compound porous material provided by the invention is simple and easy to implement, and has low cost, and the prepared FeAlSi intermetallic compound porous material has the advantages of high porosity, light weight, high strength, good high-temperature oxidation resistance and corrosion resistance, and the like.
(3) The FeAlSi intermetallic compound porous material prepared by the invention uses the Kerkdall effect to form pores, and the pore structure is optimally regulated and controlled by adding the components, the particle size, the pressing pressure and the sintering temperature
(4) The FeAlSi intermetallic compound porous material prepared by the method has excellent high-temperature mechanical property, good corrosion resistance and high-temperature oxidation resistance, and can be applied to the field of high-temperature filtration and separation.
Drawings
FIG. 1 is a graph showing the appearance and morphology of FeAlSi intermetallic compound porous materials obtained in examples 1-4 and comparative example 1 of the present invention.
It can be seen from the figure that the products prepared by the examples 1-4 of the present invention have no deformation and crack, and are well formed and have no deformation. While comparative example 1, in which no Si element was added, was severely deformed and even cracked under the same production conditions.
Fig. 2 is a scanning electron micrograph of the FeAlSi intermetallic compound porous material prepared according to example 1 of the present invention.
Fig. 3 is a pore size distribution diagram of the FeAlSi intermetallic compound porous material prepared in example 1 of the present invention.
Detailed Description
The following will describe the specific embodiments of the present invention in detail with reference to examples, but the present invention is not limited to the examples:
in the following examples, the iron powder used is reduced iron powder with a particle size of 250-400 mesh and a purity of not less than 99.9%; the used aluminum powder is atomized aluminum powder with the particle size of 300-400 meshes and the purity of more than or equal to 99.9 percent, and the used silicon powder with the particle size of 600-800 meshes and the purity of more than or equal to 99.9 percent.
Example 1
The preparation method of the FeAlSi intermetallic compound porous material comprises the following steps:
first, iron powder, aluminum powder, and silicon powder were mixed in a mass ratio of 73.8 wt% Fe (73.8g), 24.6 wt.% Al (24.6g), and 1.6 wt.% Si (1.6g), and placed in a closed container.
Secondly, the mixed powder is put into a V-shaped mixer, the mixing is started, the rotating speed is set to be about 60rpm, the mixing time is 24h,
then, taking out the uniformly mixed powder, adopting a molding method of mold one-way pressurization to perform compression molding, wherein the inner diameter of the mold is phi 30mm, the loading pressure is 110MPa, preparing a round pressed blank with phi 30mm and thickness of 3mm, and finally putting the obtained pressed blank into a vacuum sintering furnace to enter into the vacuum sintering furnaceVacuum pressureless sintering is carried out, wherein a sintering furnace is firstly vacuumized to 1 multiplied by 10-3Pa, the heating rate is 5 ℃/min, the sintering procedure is 120 ℃ multiplied by 0.5h +600 ℃ multiplied by 1h +1150 ℃ multiplied by 2h, and the mixture is cooled to the room temperature along with the furnace.
The porosity of the FeAlSi intermetallic compound porous material is 49.2 percent, and the intermediate pore diameter is 17.7um
Example 2
The preparation method of the FeAlSi intermetallic compound porous material comprises the following steps:
first, iron powder, aluminum powder, and silicon powder were mixed in a mass ratio of 74.25 wt% Fe (74.25g), 24.75 wt.% Al (24.75g), and 1 wt.% Si (1g), and placed in a closed container.
Secondly, the mixed powder is put into a V-shaped mixer, the mixing is started, the rotating speed is set to be about 60rpm, and the mixing time is 24h
Then, the uniformly mixed powder is taken out, and is pressed and molded by adopting a molding method of unidirectional pressurization of a mold, the inner diameter of the mold is phi 30mm, the loading pressure is 110MPa, and a round green compact with phi 30mm and thickness of 3mm is prepared.
Finally, the obtained pressed compact is placed into a vacuum sintering furnace for vacuum pressureless sintering, and the sintering furnace is firstly vacuumized to 1 multiplied by 10-3Pa, the heating rate is 5 ℃/min, the sintering procedure is 120 ℃ multiplied by 0.5h +600 ℃ multiplied by 1h +1150 ℃ multiplied by 2h, and the mixture is cooled to the room temperature along with the furnace.
The porosity of the FeAlSi intermetallic compound porous material is 48.1 percent, and the intermediate pore diameter is 17.2um
Example 3
The preparation method of the FeAlSi intermetallic compound porous material comprises the following steps:
first, iron powder, aluminum powder, and silicon powder were mixed in a mass ratio of 73.5 wt% Fe (73.5g), 24.5 wt.% Al (24.5g), and 2 wt.% Si (2g), and placed in a closed container.
Secondly, the mixed powder is put into a V-shaped mixer, the mixing is started, the rotating speed is set to be about 60rpm, and the mixing time is 24h
Then, the uniformly mixed powder is taken out, and is pressed and molded by adopting a molding method of unidirectional pressurization of a mold, the inner diameter of the mold is phi 30mm, the loading pressure is 110MPa, and a round green compact with phi 30mm and thickness of 3mm is prepared.
Finally, the obtained pressed compact is placed into a vacuum sintering furnace for vacuum pressureless sintering, and the sintering furnace is firstly vacuumized to 1 multiplied by 10-3Pa, the heating rate is 5 ℃/min, the sintering procedure is 120 ℃ multiplied by 0.5h +600 ℃ multiplied by 1h +1150 ℃ multiplied by 2h, and the mixture is cooled to the room temperature along with the furnace.
The porosity of the FeAlSi intermetallic compound porous material is 49.8 percent, and the intermediate pore diameter is 18.1um
Example 4
The preparation method of the FeAlSi intermetallic compound porous material comprises the following steps:
first, iron powder, aluminum powder, and silicon powder were mixed in a mass ratio of 72.75 wt% Fe (72.75g), 24.25 wt.% Al (24.25g), and 3 wt.% Si (3g), and placed in a closed container.
Secondly, the mixed powder is put into a V-shaped mixer, the mixing is started, the rotating speed is set to be about 60rpm, and the mixing time is 24h
Then, the uniformly mixed powder is taken out, and is pressed and molded by adopting a molding method of unidirectional pressurization of a mold, the inner diameter of the mold is phi 30mm, the loading pressure is 110MPa, and a round green compact with phi 30mm and thickness of 3mm is prepared.
Finally, the obtained pressed compact is placed into a vacuum sintering furnace for vacuum pressureless sintering, and the sintering furnace is firstly vacuumized to 1 multiplied by 10-3Pa, the heating rate is 5 ℃/min, the sintering procedure is 120 ℃ multiplied by 0.5h +600 ℃ multiplied by 1h +1150 ℃ multiplied by 2h, and the mixture is cooled to the room temperature along with the furnace.
The porosity of the FeAlSi intermetallic compound porous material is 56.1%, and the intermediate pore diameter is 19.7um
Comparative example 1
A preparation method of a FeAl intermetallic compound porous material comprises the following steps:
first, iron powder and aluminum powder were mixed in a mass ratio of 75 wt% Fe (75g) and 25 wt.% Al (25g), and the mixture was placed in a closed container.
Secondly, the mixed powder is put into a V-shaped mixer, the mixing is started, the rotating speed is set to be about 60rpm, and the mixing time is 24h
Then, the uniformly mixed powder is taken out, and is pressed and molded by adopting a molding method of unidirectional pressurization of a mold, the inner diameter of the mold is phi 30mm, the loading pressure is 110MPa, and a round green compact with phi 30mm and thickness of 3mm is prepared.
And finally, putting the obtained pressed compact into a vacuum sintering furnace for vacuum pressureless sintering, vacuumizing the sintering furnace to 1 x 10 < -3 > Pa, raising the temperature at 5 ℃/min, performing the sintering procedure of 0.5h at 120 ℃, 1h at 600 ℃, 1h at 1150 ℃ and 2h, and cooling to room temperature along with the furnace.
The porosity of the FeAlSi intermetallic compound porous material is 42.4%, the intermediate pore diameter is 16.7um, a sample is easy to deform and crack, and the structure components are not uniform.
Comparative example 2
The preparation method of the FeAlSi intermetallic compound porous material comprises the following steps:
first, iron powder, aluminum powder, and silicon powder were mixed in a mass ratio of 67.5 wt% Fe (67.5g), 22.5 wt.% Al (22.5g), and 10 wt.% Si (10g), and placed in a closed container.
Secondly, the mixed powder is put into a V-shaped mixer, the mixing is started, the rotating speed is set to be about 60rpm, the mixing time is 24h,
then, the uniformly mixed powder is taken out, and is pressed and molded by adopting a molding method of unidirectional pressurization of a mold, the inner diameter of the mold is phi 30mm, the loading pressure is 110MPa, and a round green compact with phi 30mm and thickness of 3mm is prepared.
Finally, the obtained pressed compact is placed into a vacuum sintering furnace for vacuum pressureless sintering, and the sintering furnace is firstly vacuumized to 1 multiplied by 10-3Pa, the heating rate is 5 ℃/min, the sintering procedure is 120 ℃ multiplied by 0.5h +600 ℃ multiplied by 1h +1150 ℃ multiplied by 2h, and the mixture is cooled to the room temperature along with the furnace.
It was found during the test that the samples were not easily shaped and easily cracked and delaminated during the pressing. The porosity of the FeAlSi intermetallic compound porous material is 57.26 percent, and the intermediate pore diameter is 25.2um
Comparative example 3
The preparation method of the FeAlSi intermetallic compound porous material comprises the following steps:
first, iron powder, aluminum powder, and silicon powder were mixed in a mass ratio of 83.64 wt% Fe (83.64g), 14.76 wt.% Al (14.76g), and 1.6 wt.% Si (1.6g), and placed in a closed container.
Secondly, the mixed powder is put into a V-shaped mixer, the mixing is started, the rotating speed is set to be about 60rpm, and the mixing time is 24h
Then, the uniformly mixed powder is taken out, and is pressed and molded by adopting a molding method of unidirectional pressurization of a mold, the inner diameter of the mold is phi 30mm, the loading pressure is 110MPa, and a round green compact with phi 30mm and thickness of 3mm is prepared.
Finally, the obtained pressed compact is placed into a vacuum sintering furnace for vacuum pressureless sintering, and the sintering furnace is firstly vacuumized to 1 multiplied by 10-3Pa, the heating rate is 5 ℃/min, the sintering procedure is 120 ℃ multiplied by 0.5h +600 ℃ multiplied by 1h +1150 ℃ multiplied by 2h, and the mixture is cooled to the room temperature along with the furnace.
During the test, it was found that the sintered sample was brittle and the compressive strength of the sample was reduced.
Comparative example 4
The preparation method of the FeAlSi intermetallic compound porous material comprises the following steps:
first, iron powder, aluminum powder, and silicon powder were mixed in a mass ratio of 73.8 wt% Fe (73.8g), 24.6 wt.% Al (24.6g), and 1.6 wt.% Si (1.6g), and placed in a closed container.
Secondly, the mixed powder is put into a V-shaped mixer, the mixing is started, the rotating speed is set to be about 60rpm, and the mixing time is 24h
Then, taking out the uniformly mixed powder, adopting a molding method of mold one-way pressurization to perform compression molding, wherein the inner diameter of the mold is phi 30mm, the loading pressure is 110MPa, preparing a round pressed blank with phi 30mm and thickness of 3mm, finally, putting the obtained pressed blank into a vacuum sintering furnace to perform vacuum pressureless sintering, and firstly, vacuumizing the sintering furnace to 1 x 10-3Pa, the heating rate is 10 ℃/min, the sintering procedure is that the temperature is firstly raised to 120 ℃ for 0.5h, then the temperature is directly raised to 1150 x 2h, and the temperature is cooled to the room temperature along with the furnace.
During the test, it was found that the sample had undergone severe deformation and cracking, and the sample became oval and had many fine cracks around it.
Claims (9)
1. A FeAlSi intermetallic porous material characterized by: the porous material comprises the following components in percentage by mass: fe 71.25-74.25 wt%; 23.75-24.75 wt.% Al; si 1-5 wt.%; the porosity of the porous material is 40-60%.
2. A FeAlSi intermetallic porous material according to claim 1 characterized by: the porous material comprises the following components in percentage by mass: fe72.75-74.25 wt%; 24.25-24.75 wt.% Al; si 1-3 wt.%.
3. A method of preparing a FeAlSi intermetallic porous material according to claim 1 or 2, characterized in that: the method comprises the following steps: the preparation method comprises the following steps of mixing iron powder, aluminum powder and silicon powder according to a designed proportion to obtain mixed powder, pressing and molding the mixed powder, and sintering to obtain the FeAlSi intermetallic compound porous material, wherein the sintering process comprises the following steps: heating to 120 ℃ at the speed of 3-7 ℃/min, preserving heat for 0.5-1h, then heating to 620 ℃ at the speed of 3-7 ℃/min, preserving heat for 0.5-1h, heating to 1120 ℃ to 1180 ℃ at the speed of 3-7 ℃/min, and preserving heat for 1-2 h.
4. A method for preparing a FeAlSi intermetallic porous material according to claim 3, characterized in that: the iron powder is reduced iron powder, and the particle size of the reduced iron powder is 250-400 meshes.
5. A method for preparing a FeAlSi intermetallic porous material according to claim 3, characterized in that: the aluminum powder is atomized aluminum powder with the particle size of 300-400 meshes; the particle size of the silicon powder is 600-800.
6. A method for preparing a FeAlSi intermetallic porous material according to claim 3, characterized in that: the mixing is carried out in a mixer, the mixing speed is 60-100rpm, and the mixing time is 12-24 h.
7. A method for preparing a FeAlSi intermetallic porous material according to claim 3, characterized in that: the pressure of the compression molding is 100-150 MPa.
8. A method for preparing a FeAlSi intermetallic porous material according to claim 3, characterized in that: and during sintering, sintering is carried out in a vacuum environment.
9. Use of a FeAlSi intermetallic porous material according to claim 1 or 2, characterized in that: the porous FeAlSi intermetallic compound porous material is applied to a filter material.
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| CN112077321A (en) * | 2020-08-24 | 2020-12-15 | 向双清 | Method for preparing FeAl intermetallic compound flexible film by element mixed powder reaction synthesis |
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| 高海燕, 干庆展, 贺跃辉, 江垚, 冯路利: "FeAl(Si)多孔材料的制备及高温力学性能", 《功能材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647741A (en) * | 2020-06-12 | 2020-09-11 | 山东煜龙环保科技股份有限公司 | Method for producing ferro-silico-aluminum alloy by using red mud iron powder |
| CN112077321A (en) * | 2020-08-24 | 2020-12-15 | 向双清 | Method for preparing FeAl intermetallic compound flexible film by element mixed powder reaction synthesis |
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