CN111940746B - Method for preparing FeAl intermetallic compound flexible film by prealloyed powder activation sintering - Google Patents
Method for preparing FeAl intermetallic compound flexible film by prealloyed powder activation sintering Download PDFInfo
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
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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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses a method for preparing a FeAl intermetallic compound flexible membrane by activated sintering of prealloyed powder. The method comprises the following steps: a. powder preparation: adding gas atomized FeAl-based alloy powder, adding a wet grinding medium, a bonding agent and a sintering activator, and uniformly mixing to obtain powder slurry; b. ball milling: carrying out mechanical ball milling on the powder slurry; c. sizing: spraying the powder slurry subjected to ball milling on a wire mesh by taking a 310S stainless wire mesh as a substrate, and fully drying to obtain a powder/wire mesh composite; d. and (3) sintering: and placing the powder/silk screen composite body in a sintering furnace for low-temperature degreasing and high-temperature sintering, and then cooling to obtain the FeAl intermetallic compound flexible film. The prepared FeAl intermetallic compound flexible membrane has uniform components, high porosity, good high-temperature oxidation resistance and vulcanization resistance, and good mechanical property and filtering property.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic porous membrane materials, and particularly relates to a method for preparing a FeAl intermetallic compound flexible membrane by activation sintering of prealloy powder.
Background
The high-temperature filtration is to use the specific pore structure of the membrane material to filter and separate high-temperature gas, has the advantages of high efficiency, energy conservation, simplicity, convenience, small pollution and the like, and is widely applied to various industrial fields, in particular to the purification treatment of industrial high-temperature flue gas such as steel, coal chemical industry, thermal power, waste incineration and the like. At present, the high-temperature filter material is mainly a metal membrane material and a ceramic membrane material, wherein the metal porous membrane material has the defects of poor high-temperature resistance and corrosion resistance, and the ceramic porous membrane material is easy to break in use due to the problems of high brittleness, poor thermal shock resistance and the like, so that the application environment is limited.
The FeAl-based alloy filter material has excellent performances of room high-temperature strength, high-temperature oxidation resistance, sulfuration resistance, molten salt corrosion resistance and the like, particularly benefits from the component characteristics of high Al content, has superior sulfur corrosion resistance to expensive stainless steel and nickel-based alloy filter materials such as Inconel 600 and Hastelloy X, and has unique performance and economic advantages in the field of filtration of sulfur-containing high-temperature gas in petrochemical industry and coal gasification, which has the widest application prospect. Practice proves that the upper limit of the use temperature of the sintered metal FeAl-based filter material in a coal gasification environment can reach 800-1000 ℃. In addition, the main components of the FeAl-based filter material are composed of Fe, al and part of alloy elements, the price is relatively low, and the FeAl-based filter material meets the requirements of modern industry on high-temperature filter materials. At present, commercial FeAl-based filter materials comprise various sintered metals, metal fiber felts, sintered metal wire meshes and the like, and have various size specifications, thereby meeting the requirement of domestic high-temperature filtration to a certain extent. However, for the working conditions that the flue gas flow is large and the system pressure drop is required to be low, such as the key industries of catalytic cracking FCC, coal-fired power plants, steel and the like, the high-temperature membrane filtration has not been widely applied, because of the lack of high-temperature resistance, corrosion resistance, large flux, low membrane resistance and high-precision filter materials. The thickness of a traditional sintered metal filter element is usually more than 2.0mm, and the stable pressure difference of a filter unit exceeds 5.0KPa under the condition that the economic filter wind speed is 1.2-1.4 m/s, so that the energy consumption of a system is increased, and the normal operation of a front-end process is limited to a great extent. Therefore, a large number of key industries such as coal-fired power plants, steel, FCC (fluid catalytic cracking) and the like have to select a low-temperature end treatment mode, so that the waste heat recovery efficiency, the desulfurization and denitrification efficiency are reduced, and the environmental protection investment is increased. In order to realize the treatment of industrial high-temperature corrosive dusty gas in a wider range, a new high-performance metal porous material/filter material needs to be developed urgently.
Disclosure of Invention
The invention aims to overcome the defects that the existing metal high-temperature filtering material is insufficient in high-temperature resistance and corrosion resistance, the ceramic filtering material is insufficient in toughness and thermal shock resistance, and the common tubular filtering material is large in thickness, high in filtering resistance and the like.
The invention aims to:
(1) The flexible FeAl intermetallic compound porous material with high temperature resistance, corrosion resistance, high strength and toughness and low filtration resistance is provided;
(2) The problems of weak binding force and easy cracking between a film layer and a silk screen matrix in the direct spraying and sintering of the traditional FeAl prealloy powder are greatly improved.
In order to achieve the above object, the method for preparing a flexible film of a FeAl intermetallic compound by activation sintering of prealloyed powder of the present invention comprises the following steps:
a. powder preparation: adding gas atomized FeAl-based alloy powder, adding a wet grinding medium, a bonding agent and a sintering activator, and uniformly mixing to obtain powder slurry;
b. ball milling: mechanically ball-milling the powder slurry obtained in the step a;
c. sizing: spraying the powder slurry subjected to ball milling on a wire mesh by taking a 310S stainless wire mesh as a substrate, and fully drying to obtain a powder/wire mesh composite;
d. and (3) sintering: and placing the powder/silk screen composite in a sintering furnace for degreasing and high-temperature sintering, and then cooling to obtain the FeAl intermetallic compound flexible film.
The gas atomized FeAl-based alloy powder can be atomized by adopting nitrogen or argon. Since high aluminum alloys are subject to irreversible oxidation by exposure to air or water, the atomization process needs to be carried out under inert gas shielding. The nitrogen and the argon do not react with the FeAl-based alloy in the atomization process, so that the passivation of the surface of the powder can be avoided.
Preferably, the FeAl-based alloy is a FeAl alloy or a FeCrAl alloy; the aluminum content in the FeAl alloy is 10-25% by mass, and the balance is Fe; the content of Cr in the FeCrAl alloy is 10-20% by mass, the content of Al is 5-12% by mass, and the balance is Fe. Too high Al content or both Al and Cr content may lead to embrittlement of the FeAl-based alloy.
Preferably, the particle size of the FeAl-based alloy powder is-200 meshes, and the median diameter D50 is less than 300 meshes.
Preferably, the wet grinding medium is ethanol, and the addition amount of the ethanol is 30-40% of the mass of the FeAl-based alloy.
The addition amount of ethanol is too high or too low, which is not favorable for achieving good ball milling efficiency, and when the addition amount is too high, the powder slurry is too thin and is difficult to form a slurry film, so that the ball milling efficiency is reduced; when the amount of the additive is insufficient, the powder slurry is too thick to be easily dispersed, and insufficient or uneven ball milling is likely to occur. In addition, ethanol is used as a wet grinding medium, so that the powder can be prevented from being oxidized in the high-energy ball milling process.
Preferably, the binder is one or a composition of more than two of thermoplastic phenolic resin, PEG, PVA, PVB and PAA, and the addition amount of the binder is 5-10% of the mass of the FeAl-based alloy.
Preferably, the sintering activator is one or a composition of more than two of elementary boron, boron iron powder, metal yttrium and yttrium boride, and the main elements of the sintering activator are boron (B) and yttrium (Y). The addition amount of the sintering activator is 0.5-1.0 percent of the mass of the FeAl-based alloy.
Preferably, the mechanical ball milling ball material ratio is 3-1 to 1, and the ball milling time is 24-36 h; it can be carried out on a tumbling ball mill, a planetary ball mill or an agitated ball mill.
The main purpose of the ball milling process is to fully mix the sintering activator and the FeAl-based alloy powder, and embed the sintering activator on the surface of the powder, thereby being beneficial to surface diffusion in the later sintering process. Meanwhile, in the ball milling process, gas atomized spherical powder is converted into irregular powder in the modes of extrusion, impact and the like, a large amount of yield deformation is generated macroscopically, the specific surface area of the powder is increased, and a large amount of lattice deformation and dislocation are generated microscopically, so that energy storage activation is realized.
Preferably, the aperture of the 310S stainless steel wire mesh is 60-80 meshes; the 310S material has good high-temperature resistance, and meanwhile, the aperture specification of 60-80 meshes is adopted, so that the base material has good mechanical property and the smooth macroscopic form of the flexible membrane can be kept after high-temperature sintering.
Preferably, the spraying amount of the sizing agent powder sizing agent is 250-350 g/m in terms of the mass of the FeAl-based alloy 2 The drying temperature is 80-100 ℃.
If the sizing amount is too small, a continuous and compact film layer is difficult to form, so that the filtering precision of the flexible film is low; if the sizing amount is too large, the thickness of the film layer is too large, and the resistance of the film layer is too high. The drying process is carried out at this relatively low temperature, which reduces the oxidation rate of the powder. Meanwhile, the solvent ethanol can be recovered according to the requirement.
Further, the high-temperature sintering process may be performed in a vacuum furnace or a hydrogen furnace. The vacuum sintering and the hydrogen sintering can prevent the powder and the substrate silk screen from being oxidized as much as possible, and generate certain activation effect to promote the sintering process.
Preferably, the step d of sintering comprises the following steps:
the powder/screen composite was placed in a sintering furnace at 1X 10 -2 ～1×10 -3 Keeping the temperature for 1-2 h at 400-500 ℃ under the Pa condition, then raising the temperature to 950-1050 ℃ at the temperature raising speed of 5-10 ℃/min, keeping the temperature for 30-60 min, finally raising the temperature to 1250-1300 ℃ at the temperature raising speed of 5-10 ℃/min, and keeping the temperature for 90-120 min; then cooling to 800-850 ℃ at the cooling rate of 3-5 ℃/min, preserving the heat at 800-850 ℃ for 60min, and finally cooling to room temperature at the cooling rate of 5-8 ℃/min to obtain the FeAl intermetallic compound flexible film.
Namely, the high-temperature sintering process can be divided into a heating process and a cooling process. The temperature rise process of the high-temperature sintering process is set with three sections of sintering platforms, the temperature of the first section is 400-500 ℃, and the time is 1-2 hours; the temperature of the second section is 950-1050 ℃, and the time is 30-60 min; the third section is 1250-1300 ℃ and the sintering temperature is 90-120 min.
The first stage sintering is to remove organic matters; the second stage sintering process aims to make the sintering active agent mixed in the powder produce diffusion reaction with the powder and the silk screen matrix. The B element in the sintering activator can be diffused with the film layer powder and the silk screen matrix to form an Fe-B phase with a lower melting point, thereby promoting the growth of a sintering neck. The purpose of three-stage sintering is to ensure the homogenization of components, the sufficient development of sintering necks among powders and between powders and a matrix wire mesh, the sufficient formation of a pore structure and the obtainment of good mechanical properties. In the added sintering activator, the B element is easily segregated in the grain boundary after diffusion, thereby strengthening the grain boundary. The added element Y can be dissolved into the alloy matrix in a solid solution mode in the three-stage high-temperature sintering process, excessive growth of crystal grains is inhibited to a certain extent, solid solution strengthening is generated, and the high-temperature resistance of the FeAl-based alloy is improved.
The temperature reduction process is also divided into two-section temperature reduction and one-section heat preservation, wherein the first-section temperature reduction is that the furnace is cooled to 800-850 ℃ after the three-section sintering heat preservation is finished, the first-section heat preservation is that the furnace is kept at 800-850 ℃ for 60min, and the second-section temperature reduction is that the furnace is cooled to room temperature at 800-850 ℃. Wherein the first-stage cooling rate is 3-5 ℃/min, and the second-stage cooling rate is 5-8 ℃/min. The first stage of cooling is furnace cooling, and the second stage of cooling is accelerated cooling of gas circulation cooling.
The heat preservation at 800-850 ℃ in the cooling process is equivalent to the annealing process, so that the sintering stress can be eliminated, and the toughness of the flexible membrane material is improved; the two-stage accelerated cooling process can avoid the brittleness generation temperature section, namely the FeAl alloy or the FeAlCr alloy generates amplitude modulation decomposition in the process of 450-500 ℃, thereby inducing brittleness behavior. Therefore, the control of the cooling process can effectively improve the obdurability of the FeAl-based alloy flexible film.
The invention has the beneficial effects that:
(1) The invention adopts gas atomized FeAl-based pre-alloyed powder as a raw material, the powder has good component uniformity and strong corrosion resistance, and the prepared FeAl intermetallic compound flexible film has good high-temperature oxidation resistance and corrosion resistance and long service life.
(2) The invention adopts mechanical ball milling and sintering activator addition to carry out mechanical energy storage activation and chemical activation on the powder sintering process, thereby improving the sintering activity of the pre-alloy powder; compared with the process of directly spraying and atomizing alloy powder, the process of the activated sintering can ensure that the flexible film obtains better mechanical property and fatigue resistance.
(3) The added sintering active agent B and Y elements can induce the FeAl material to quickly form alpha-type alumina in the high-temperature oxidation process, so that the high-temperature resistance and the corrosion resistance of the FeAl-based flexible film can be further improved.
Drawings
Fig. 1 is a tensile strength result for FeAl intermetallic flexible films.
Fig. 2 shows that the mechanical properties of the flexible membrane added with B and Y are significantly improved.
FIG. 3 shows the morphology of FeAl flexible films formed by coating and sintering.
FIG. 4 shows that a good metallurgical bond is formed between the film and the substrate after activation sintering.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof.
The FeAl or FeCrAl alloy powders used in the following examples had a particle size of-200 mesh and a median diameter D50 of less than 300 mesh.
Example 1
A method for preparing a FeAl intermetallic compound flexible membrane by a pre-alloy powder sintering method comprises the following steps:
1. powder preparation: adding 5g of thermoplastic phenolic resin into 30mL of ethanol, then adding 100g of FeAl gas atomized spherical alloy powder (wherein the aluminum content is 10wt.%, and the balance is Fe), and then adding a sintering activator (0.5 g of boron is contained according to elements, and the addition form is simple substance boron and ferroboron powder); and preparing uniform suspended particle slurry by mechanical stirring.
2. Ball milling: and (2) placing the suspension particle slurry prepared in the step (1) in a planetary ball mill for mechanical ball milling, wherein the ball-to-material ratio is 3 to 1, and the ball milling time is 24 hours, so as to obtain irregular energy storage powder uniformly compounded by an activator and FeAl-based alloy powder.
3. Sizing: a layer of uniform FeAl pre-alloy powder composite slurry is sprayed on a 310S stainless steel net (the net aperture is 60 meshes), and the slurry loading amount is 250g/m calculated by the mass of FeAl-based alloy 2 And drying at 80 ℃ to form a film layer.
4. And (3) sintering: in a vacuum furnace at a vacuum degree of 1X 10 -2 Under the condition of Pa, firstly preserving heat for 1h at 400 ℃, then raising the temperature to 950 ℃ at the temperature raising speed of 5 ℃/min and preserving heat for 30min, finally raising the temperature to 1150 ℃ at the temperature raising speed of 5 ℃/min and preserving heat for 90min. Then the temperature is reduced to 800 ℃ at the cooling rate of 3 ℃/min, the temperature is preserved for 60min at 800 ℃, and finally the temperature is reduced to room temperature at the cooling rate of 5 ℃/min. Thus preparing the FeAl intermetallic compound flexible film.
The FeAl intermetallic compound flexible film prepared by the embodiment forms metallurgical bonding with the surface of the stainless steel mesh (fig. 3 and 4), and the surface has rich smooth pore structure.
Example 2
A method for preparing a FeAl intermetallic compound flexible film by a pre-alloy powder sintering method comprises the following steps:
1. powder preparation: adding 8g of thermoplastic phenolic resin into 35mL of ethanol, adding 100g of FeAl gas atomized spherical alloy powder (wherein the aluminum content is 20wt.%, and the balance is Fe), and adding a sintering activator (0.2 g of boron and 0.3g of yttrium according to elements, wherein the addition forms are metal yttrium and yttrium boride); and preparing uniform suspended particle slurry by mechanical stirring.
2. Ball milling: and (2) placing the suspension particle slurry prepared in the step (1) in a planetary ball mill for mechanical ball milling, wherein the ball-to-material ratio is 3 to 1, and the ball milling time is 30h, so as to obtain irregular energy storage powder uniformly compounded by an activator and FeAl-based alloy powder.
3. Sizing: a layer of uniform FeAl pre-alloy powder composite slurry is sprayed on a 310S stainless steel net (the net aperture is 80 meshes), and the slurry loading amount is 300g/m calculated by the mass of FeAl-based alloy 2 And drying at 100 ℃ to form a film layer.
4. And (3) sintering: in a vacuum furnace at a vacuum degree of 1X 10 -3 Under the condition of Pa, firstly preserving heat for 1.5h at 450 ℃, then raising the temperature to 1000 ℃ at the temperature raising speed of 8 ℃/min and preserving heat for 45min, and finally raising the temperature to 1150 ℃ at the temperature raising speed of 8 ℃/min and preserving heat for 105min. Then cooling to 820 deg.C at a rate of 5 deg.C/min, maintaining at 820 deg.C for 60min, and finally cooling to room temperature at a rate of 8 deg.C/min. Thus preparing the FeAl intermetallic compound flexible film.
The FeAl intermetallic compound flexible film prepared by the embodiment forms metallurgical bonding with the surface of the stainless steel mesh, and the surface has rich smooth pore structures.
Example 3
A method for preparing a FeAl intermetallic compound flexible film by a pre-alloy powder sintering method comprises the following steps:
1. powder preparation: adding 10g of thermoplastic phenolic resin into 40mL of ethanol, adding 100g of FeAl gas atomized spherical alloy powder (wherein the aluminum content is 25wt.%, and the balance is Fe), and adding sintering activating agents (0.3 g of boron and 0.3g of yttrium according to elements, wherein the adding forms are ferroboron powder and yttrium boride); and preparing uniform suspended particle slurry by mechanical stirring.
2. Ball milling: and (3) placing the suspension particle slurry prepared in the step (1) into a planetary ball mill for mechanical ball milling, wherein the ball-to-material ratio is 3 and the ball milling time is 36h, so that irregular energy storage powder uniformly compounded by an activator and FeAl-based alloy powder is obtained.
3. Sizing: at 310S does notA layer of uniform FeAl pre-alloy powder composite slurry is sprayed on the rust steel mesh (the mesh aperture is 60 meshes), and the slurry feeding amount is 350g/m in terms of the mass of the FeAl-based alloy 2 And drying at 80 ℃ to form a film layer.
4. And (3) sintering: in a vacuum furnace at a vacuum degree of 1X 10 -2 Under the condition of Pa, firstly preserving heat for 2h at 500 ℃, then raising the temperature to 1050 ℃ at the heating rate of 10 ℃/min and preserving heat for 60min, finally raising the temperature to 1150 ℃ at the heating rate of 10 ℃/min and preserving heat for 120min. Then the temperature is reduced to 850 ℃ at the cooling rate of 3 ℃/min, the temperature is preserved for 60min at 850 ℃, and finally the temperature is reduced to the room temperature at the cooling rate of 5 ℃/min. Thus preparing the FeAl intermetallic compound flexible film.
The FeAl intermetallic compound flexible film prepared by the embodiment forms metallurgical bonding with the surface of the stainless steel mesh, and the surface has rich smooth pore structures.
Example 4
A method for preparing a FeAl intermetallic compound flexible film by a pre-alloy powder sintering method comprises the following steps:
1. powder preparation: adding 5g of thermoplastic phenolic resin into 30mL of ethanol, adding 100g of FeCrAl gas atomized spherical alloy powder (wherein the Cr content is 10wt.%, the Al content is 12wt.%, and the balance is Fe), and adding a sintering activator (according to elements, 0.3g of boron and 0.4g of yttrium are contained, and the addition forms are simple substance boron powder and yttrium boride); and preparing uniform suspended particle slurry by mechanical stirring.
2. Ball milling: and (2) placing the suspension particle slurry prepared in the step (1) in a planetary ball mill for mechanical ball milling, wherein the ball-to-material ratio is 5 to 1, and the ball milling time is 24 hours, so as to obtain irregular energy storage powder uniformly compounded by an activator and FeAl-based alloy powder.
3. Sizing: spraying a layer of uniform FeAl pre-alloy powder composite slurry on a 310S stainless steel net (the net aperture is 80 meshes), wherein the slurry loading amount is 250g/m in terms of the mass of FeAl-based alloy 2 And drying at 100 ℃ to form the film layer.
4. And (3) sintering: in a vacuum furnace at a vacuum degree of 1X 10 -3 Under the condition of Pa, firstly preserving heat for 1h at 400 ℃, then raising the temperature to 950 ℃ at the temperature-raising speed of 5 ℃/min and preserving heat for 30min, and finally raising the temperature at the temperature-raising speed of 5 ℃/minReach 1280 deg.c and maintaining for 90min. Then cooling to 800 ℃ at the cooling rate of 5 ℃/min, preserving the heat at 800 ℃ for 60min, and finally cooling to room temperature at the cooling rate of 8 ℃/min. Thus preparing the FeAl intermetallic compound flexible film.
The FeAl intermetallic compound flexible film prepared by the embodiment forms metallurgical bonding with the surface of the stainless steel mesh, and the surface has rich smooth pore structures.
Example 5
A method for preparing a FeAl intermetallic compound flexible film by a pre-alloy powder sintering method comprises the following steps:
1. powder preparation: adding 8g of thermoplastic phenolic resin into 35mL of ethanol, adding 100g of FeCrAl gas atomized spherical alloy powder (wherein the Cr content is 15wt.%, the Al content is 10wt.%, and the balance is Fe), and adding a sintering activator (according to elements, 0.2g of boron is contained, 0.6g of yttrium is contained, and the addition forms are metal yttrium and yttrium boride); and preparing uniform suspended particle slurry by mechanical stirring.
2. Ball milling: and (2) placing the suspension particle slurry prepared in the step (1) in a planetary ball mill for mechanical ball milling, wherein the ball-to-material ratio is 5 to 1, and the ball milling time is 30h, so as to obtain irregular energy storage powder uniformly compounded by an activator and FeAl-based alloy powder.
3. Sizing: spraying a layer of uniform FeAl pre-alloy powder composite slurry on a 310S stainless steel net (the mesh diameter is 60 meshes), wherein the slurry loading amount is 300g/m in terms of the mass of FeAl-based alloy 2 And drying at 80 ℃ to form a film layer.
4. And (3) sintering: in a vacuum furnace at a vacuum degree of 1X 10 -2 Under the condition of Pa, firstly preserving heat for 1.5h at 450 ℃, then raising the temperature to 1000 ℃ at the heating rate of 8 ℃/min and preserving heat for 45min, and finally raising the temperature to 1300 ℃ at the heating rate of 8 ℃/min and preserving heat for 105min. Then the temperature is reduced to 820 ℃ at the cooling rate of 3 ℃/min, the temperature is preserved for 60min at 820 ℃, and finally the temperature is reduced to the room temperature at the cooling rate of 5 ℃/min. Thus preparing the FeAl intermetallic compound flexible film.
The FeAl intermetallic compound flexible film prepared by the embodiment forms metallurgical bonding with the surface of the stainless steel mesh, and the surface smooth pore structure is rich.
Example 6
A method for preparing a FeAl intermetallic compound flexible film by a pre-alloy powder sintering method comprises the following steps:
1. powder preparation: adding 10g of thermoplastic phenolic resin into 40mL of ethanol, adding 100g of FeCrAl gas atomized spherical alloy powder (wherein the Cr content is 20wt.%, the Al content is 5wt.%, and the balance is Fe), and adding a sintering activator (according to elements, 0.4g of boron is contained, 0.6g of yttrium is contained, and the addition forms are metal yttrium and ferroboron powder); and preparing uniform suspended particle slurry by mechanical stirring.
2. Ball milling: and (3) placing the suspension particle slurry prepared in the step (1) into a planetary ball mill for mechanical ball milling, wherein the ball-material ratio is 5 to 1, and the ball milling time is 36h, so that irregular energy storage powder uniformly compounded by an activator and FeAl-based alloy powder is obtained.
3. Sizing: spraying a layer of uniform FeAl pre-alloy powder composite slurry on a 310S stainless steel net (the net aperture is 80 meshes), wherein the slurry amount is 350g/m in terms of the mass of FeAl-based alloy 2 And drying at 100 ℃ to form the film layer.
4. And (3) sintering: in a vacuum furnace at a vacuum degree of 1X 10 -3 Under the condition of Pa, firstly preserving heat for 2h at 500 ℃, then increasing the temperature to 1050 ℃ at the heating rate of 10 ℃/min and preserving heat for 60min, finally increasing the temperature to 1320 ℃ at the heating rate of 10 ℃/min and preserving heat for 120min. Then cooling to 850 deg.C at a rate of 5 deg.C/min, maintaining at 850 deg.C for 60min, and finally cooling to room temperature at a rate of 8 deg.C/min. Thus preparing the FeAl intermetallic compound flexible film.
The FeAl intermetallic compound flexible film prepared by the embodiment forms metallurgical bonding with the surface of the stainless steel mesh, and the surface smooth pore structure is rich.
Comparative example 1
The sample was sintered by the step 4 sintering method of the method of example 1 using a 310S stainless steel net having a mesh size of 80 mesh.
Comparative example 2
The method of example 1 was used, but without the addition of a sintering activator.
Performance testing and results:
FIG. 1 is the tensile strength results for FeAl intermetallic compound flexible films prepared in examples 1, 3-6. Fig. 2 is a mechanical property test of the FeAl intermetallic compound flexible films prepared in examples 1 and 4, and compared with comparative example 1, the mechanical property of the flexible film after B and Y are added in the preparation method of the example is significantly improved.
The performance tests were performed on the FeAl intermetallic compound flexible films prepared in examples 1 to 6 and the product obtained in comparative example 1, and the results are shown in table 1; wherein: the product obtained once prepared according to the corresponding example method is recorded as one repetition, 3 repetitions, and the results of the data in table 1 correspond to the mean values determined. Wherein, the aperture is tested by an aperture tester, and the average aperture is recorded. The oxidation weight gain and the vulcanization weight gain are respectively measured by cutting to obtain 2x2cm 2 The dimensionally flexible film samples were placed in 600 air and 600 ℃ nitrogen atmosphere with 10% partial pressure of sulfur and tested for percent weight gain after 100 hours. The internal standard method of the fatigue resistance test method company is as follows: and clamping the strip-shaped flexible film with the cut shape of 2cm multiplied by 10cm on a tensile testing machine, and testing in a pulling and pulling mode. The upper and lower limits of the tensile force are 10MPa and 30MPa, the testing period is 30000 times, the elongation of the sample is observed after the test is finished, and if the elongation does not exceed 1% or no mutation occurs, the test is regarded as passing.
TABLE 1 FeAl intermetallic Compound Flexible film Performance parameters
Claims (8)
1. A method for preparing a FeAl intermetallic compound flexible film by prealloyed powder activation sintering is characterized by comprising the following steps:
a. powder preparation: adding gas atomized FeAl-based alloy powder, adding a wet grinding medium, a bonding agent and a sintering activator, and uniformly mixing to obtain powder slurry;
the FeAl-based alloy is FeAl alloy or FeCrAl alloy, the aluminum content in the FeAl alloy is 10-25% by mass, the balance is Fe, the Cr content in the FeCrAl alloy is 10-20% by mass, the Al content is 5-12% by mass, and the balance is Fe; the binder is one or a composition of more than two of thermoplastic phenolic resin, PEG, PVA, PVB and PAA, and the sintering activator is one or a composition of more than two of simple substance boron, boron iron powder, metal yttrium and yttrium boride;
b. ball milling: mechanically ball-milling the powder slurry obtained in the step a;
c. sizing: spraying the powder slurry subjected to ball milling on a wire mesh by taking a 310S stainless wire mesh as a substrate, and fully drying to obtain a powder/wire mesh composite;
d. and (3) sintering: the powder/wire mesh composite was placed in a sintering furnace at 1X 10 -2 ～1×10 -3 Keeping the temperature for 1-2 h at 400-500 ℃ under the Pa condition, then raising the temperature to 950-1050 ℃ at the temperature raising speed of 5-10 ℃/min, keeping the temperature for 30-60 min, finally raising the temperature to 1250-1300 ℃ at the temperature raising speed of 5-10 ℃/min, and keeping the temperature for 90-120 min; then cooling to 800-850 ℃ at the cooling rate of 3-5 ℃/min, preserving the heat at 800-850 ℃ for 60min, and finally cooling to room temperature at the cooling rate of 5-8 ℃/min to obtain the FeAl intermetallic compound flexible film.
2. The method as claimed in claim 1, wherein the FeAl-based alloy powder has a particle size of-200 mesh and a median diameter D50 of less than 300 mesh.
3. The method of claim 1, wherein the wet milling medium is ethanol added in an amount of 30% to 40% by weight of the FeAl-based alloy.
4. The method according to claim 1, wherein the binder is added in an amount of 5 to 10% by mass based on the FeAl-based alloy.
5. The method according to claim 1, wherein the sintering activator is added in an amount of 0.5 to 1.0% by mass based on the FeAl-based alloy.
6. The method according to claim 1, wherein the mechanical ball milling ball-to-material ratio is 3 to 1 to 5, and the ball milling time is 24 to 36 hours.
7. The method of claim 1, wherein the 310S stainless steel wire mesh has a pore size of 60 to 80 mesh.
8. The method as claimed in claim 1, wherein the slurry is sprayed in an amount of 250 to 350g/m in terms of the mass of the FeAl-based alloy 2 The drying temperature is 80-100 ℃.
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