FE-AL-BASED METAL POROUS MEMBRANE AND PREPARATION METHOD THEREOF

Abstract

The present invention discloses a Fe—Al-based metal porous membrane and a preparation method thereof, which relate to the technical field of industrial gas-solid and liquid-solid separation and purification, and mainly address problems in the prior art, such as cracking-prone and peeling of a membrane layer of an existing Fe—Al-based metal porous membrane during its preparation and use. The preparation method of the present invention comprises the steps of: adding a Fe—Al-based metal powder and a metal fiber powder into an organic-additive-added water-based solvent, and mixing them into a slurry; tape casting the slurry, through a tape casting machine, to form a membrane green body on a metal substrate layer, and letting it dry; and placing the dried membrane green body in a sintering furnace, to remove organic substances and perform high-temperature sintering and predetermined-temperature reaction synthesis.

Claims

1. A method for preparing a Fe—Al-based metal porous membrane, wherein, the method comprises the steps of: adding a Fe—Al-based metal powder and a metal fiber powder into an organic-additive-added water-based solvent, and mixing them into a slurry; Tape casting the slurry, through a tape casting machine, to form a membrane green body on a metal substrate layer, and letting it dry; and placing the dried membrane green body in a sintering furnace, to remove organic substances and perform high-temperature sintering and predetermined-temperature reaction synthesis, thus generating a Fe—Al-based metal porous membrane removed off the organic additive and having a uniform pore structure.

2. The preparation method according to claim 1, wherein, the Fe—Al-based metal powder is one or two selected from a Fe.sub.3Al powder and a FeAl powder, and the metal fiber powder is one or more selected from 304L, 316L and 310S stainless steel fiber powders; the metal substrate layer is made of one material selected from 310S, 304L and 316L; and, the organic additive include one or more selected from polyvinyl alcohol, methyl cellulose, polyethylene glycol, propanetriol, and dibutyl phthalate.

3. The preparation method according to claim 2, wherein, a Al powder is further added into the Fe—Al-based metal powder.

4. The preparation method according to claim 3, wherein, a metal wire mesh is used as the metal substrate layer.

5. The preparation method according to claim 3, wherein, the Fe—Al-based metal powder is a Fe.sub.3Al powder, and a raw material ratio of the Fe—Al-based metal powder, the Al powder and the metal fiber powder is adjusted to 10:1:1; and during treatments in the sintering furnace, a first stage is heating up to 280-320° C. and then retaining temperature for 2 h, a second stage is heating up to below 450° C. and then retaining temperature for 2 h, a third stage is slow heating up to 650-730° C. and then retaining temperature for 1 h, and a fourth stage is continuing slow heating up to 1300° C.

6. The preparation method according to claim 3, wherein, the Fe—Al-based metal powder is a Fe.sub.3Al powder, and a raw material ratio of the Fe—Al-based metal powder, the Al powder and the metal fiber powder is adjusted to 30:1:1; and during treatments in the sintering furnace, a first stage is heating up to 280-320° C. and then retaining temperature for 2 h, a second stage is heating up to below 450° C. and then retaining temperature for 2 h, a third stage is slow heating up to 650-730° C. and then retaining temperature for 1 h, and a fourth stage is continuing slow heating up to 1300° C.

7. The preparation method according to claim 3, wherein, the Fe—Al-based metal powder is a FeAl powder, and a raw material ratio of the Fe—Al-based metal powder, the Al powder and the metal fiber powder is adjusted to 30:1:1; and during treatments in the sintering furnace, a first stage is heating up to 280-320° C. and then retaining temperature for 2 h, a second stage is heating up to below 450° C. and then retaining temperature for 2 h, a third stage is slow heating up to 650-730° C. and then retaining temperature for 1 h, and a fourth stage is continuing slow heating up to 1300° C.

8. A Fe—Al-based metal porous membrane, wherein characterized in that, the Fe—Al-based metal porous membrane comprises a sintered metal substrate layer (1), and a sintered hybrid membrane layer (2) composed of a Fe—Al-based metal powder and a metal fiber powder, wherein, the sintered hybrid membrane layer (2) composed of a Fe—Al-based metal powder and a metal fiber powder is disposed above the sintered metal substrate layer (1); and wherein, the sintered metal substrate layer (1) and the sintered hybrid membrane layer (2) composed of a Fe—Al-based metal powder and a metal fiber powder are obtained, by tape casting a water-based solution containing an organic additive, the Fe—Al-based metal powder and the metal fiber powder, through a tape casting machine, to form a membrane green body on a metal substrate layer (1), and drying, and thereafter removing organic substances and performing high-temperature sintering and predetermined-temperature reaction synthesis.

9. The Fe—Al-based metal porous membrane according to claim 8, wherein, the Fe—Al-based metal powder is one or two selected from a Fe.sub.3Al powder and a FeAl powder, and the metal fiber powder is one or more selected from 304L, 316L and 310S stainless steel fiber powders; the metal substrate layer is a metal wire mesh, and made of one material selected from 310S, 304L and 316L; and, the organic additive is a binder, a plasticizer and a dispersant, and includes one or more selected from polyvinyl alcohol, methyl cellulose, polyethylene glycol, propanetriol, and dibutyl phthalate.

10. The Fe—Al-based metal porous membrane according to claim 7, wherein, a Al powder is further added into the Fe—Al-based metal powder.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0021] FIG. 1 is a cross-sectional structure of a Fe—Al-based metal porous membrane in accordance with the present disclosure;

[0022] FIG. 2 is a flowchart of a method for preparing a Fe—Al-based metal porous membrane in accordance with the present disclosure;

[0023] FIG. 3 is a schematic diagram of a tape casting process equipment used in a preparation method of the present disclosure; and

[0024] FIG. 4 is a diagram of a sintering and heating process in a preparation method of the present disclosure.

DETAILED DESCRIPTION

[0025] Hereinafter, the present disclosure will be described in detail with reference to the accompanying drawings, in which same or similar reference numerals indicate same or similar components.

[0026] FIG. 1 is a cross-sectional structure of a Fe—Al-based metal porous membrane in accordance with the present disclosure. As shown in FIG. 1, the Fe—Al-based metal porous membrane of the present disclosure comprises a sintered metal substrate layer 1, and a sintered hybrid membrane layer 2 composed of a Fe—Al-based metal powder and a metal fiber powder, wherein, the sintered hybrid membrane layer 2 composed of a Fe—Al-based metal powder and a metal fiber powder is disposed above the sintered metal substrate layer 1.

[0027] In this embodiment, the metal substrate layer 1 may be in the form of a metal substrate membrane or a metal wire mesh; by tape casting a water-based solution containing an organic additive, a Fe—Al-based metal powder and a metal fiber powder, through a tape casting machine, to form a membrane green body on a metal substrate layer 1, and drying, and thereafter removing organic substances and performing high-temperature sintering and predetermined-temperature reaction synthesis on the dried membrane green body, thus generating a Fe—Al-based metal porous membrane removed off the organic additive and having a uniform pore structure, thereby the Fe—Al-based metal porous membrane of the present disclosure consisting of as-a-whole incorporated two layers, i.e. the sintered metal substrate layer 1 and the sintered hybrid membrane layer 2 composed of the Fe—Al-based metal powder and the metal fiber powder, is obtained.

[0028] In the present disclosure, the Fe—Al-based metal powder preferably is one or two selected from a Fe.sub.3A1 powder and a FeAl powder, and more preferably is added with a Al powder; the metal fiber powder preferably is one or more selected from 304L, 316L and 310S stainless steel fiber powders; the metal substrate membrane or metal wire mesh preferably is made of one material selected from 310S, 304L and 316L; and, the organic additive is a binder, a plasticizer and a dispersant, and preferably includes one or more selected from polyvinyl alcohol, methyl cellulose, polyethylene glycol, propanetriol, and dibutyl phthalate.

[0029] FIG. 2 is a flowchart of a method for preparing a Fe—Al-based metal porous membrane in accordance with the present disclosure. As shown in FIG. 2, the preparation method of the present disclosure comprises the following steps:

[0030] 1. adding a Fe—Al-based metal powder and a metal fiber powder into an organic-additive-added water-based solvent, stirring and mixing to prepare a uniform and stable slurry;

[0031] 2. tape casting the slurry, through a tape casting machine, to form a membrane green body on a metal substrate layer such as a metal substrate membrane or a metal wire mesh, and drying it at room temperature;

[0032] 3. placing the dried membrane green body in a sintering furnace, to remove organic substances and perform high-temperature sintering and predetermined-temperature reaction synthesis, thus generating a Fe—Al-based metal porous membrane removed off the organic additive and having a uniform pore structure.

[0033] In addition, in a case where the Fe—Al-based metal porous membrane needs to be made into a filter medium, the preparation method may further comprise the step of:

[0034] 4. Tube-forming and welding the Fe—Al-based metal porous membrane after completion of sintering, thus obtaining a filter medium with smooth surface, uniform pore distribution and superior toughness.

[0035] In this embodiment, the Fe—Al-based metal porous membrane of the present disclosure is a composite of a metal substrate layer (which may be a metal substrate membrane or a metal wire mesh) and a hybrid membrane layer composed of a Fe—Al-based metal powder and a metal fiber powder; the Fe—Al-based metal powder preferably is one or two selected from a FeAl powder and a Fe.sub.3Al powder, and more preferably is added with a Al powder; the metal fiber powder preferably is one or more selected from 304L, 310S and 316L stainless steel fiber powders; the metal substrate membrane or metal wire mesh preferably is made of one material selected from 304L, 310S and 316L; and, the organic additive is a binder, a plasticizer and a dispersant, and preferably includes one or more selected from polyvinyl alcohol, methyl cellulose, polyethylene glycol, propanetriol, and dibutyl phthalate.

[0036] The Fe—Al-based metal powder and the metal fiber powder are mixed to obtain a slurry as a raw material for preparing a Fe—Al-based metal porous membrane, then the slurry is cast, by using a cast molding method, on a metal substrate layer to form a molded green body having uniform pores, homogeneous performance and consistent size, and thereafter, through a sintering process in a sintering furnace, the molded green body is removed off organic substances from its framework and strength of the metal porous membrane is reinforced, lastly, the metal porous is taken out of the sintering furnace, and then by means of tube-forming and welding, a high-strength and high-toughness metal porous membrane filter medium is obtained, and finally, connection of a whole filter element is accomplished by electric resistance welding.

[0037] Different from a traditional cast molding process, the present disclosure optimizes and improves cast technology by selecting a water-based solvent to substitute an organic solvent used in a traditional process. Generally speaking, organic solvents used in cast technology, such as toluene and xylene, etc., all have certain toxicity, which not only cause pollution to equipment and environment, but also make it difficult to completely remove off a high-content organic substance in a cast slurry, thus affecting performance of a resultant metal membrane and causing quality problems of deformation and cracking during fabrication processing of the metal membrane. Comparatively, the water-based solvent of the present disclosure is an aqueous solution added with a small amount of binder, plasticizer and dispersant, which can be mixed with a metal powder for uniformity in a designed ratio to obtain a stable slurry.

[0038] FIG. 3 is a schematic diagram of a tape casting process equipment used in a preparation method of the present disclosure. As shown in FIG. 3, a metal substrate layer 1′ (such as a metal substrate membrane or a metal wire mesh) in construction of a Fe—Al-based metal porous membrane of the present disclosure is placed on a base plate 3 of a lining belt of a tape casting machine; a prepared cast slurry is put into a slurry tank 4, and then through adjustment of a spacing between a doctor blade 5 and the lining belt as well as a moving speed of a belt pulley 6, a uniform slurry membrane also called a green body is cast onto the metal base substrate layer 1′; after the metal membrane green body is dried and peeled off from the base plate 3, it is transferred to a sintering process for degreasing and sinter-molding.

[0039] Now referring to a sintering and heating process diagram shown in FIG. 4, an organic substance removal and sintering process in the preparation method of the present disclosure will be described below. As seen from the sintering and heating process shown in FIG. 4, a heating procedure in this process is divided into four stages. A first stage (I) is heating up to 280-320° C., in order to remove the organic additive from the prepared slurry. A second stage (II) is heating up to below 450° C. (which is the melting-point temperature of Al element), in order to inhibit self-propagation and induce Kirkendall effect, so as to promote formation of a Fe—Al-based intermetallic porous material. A third stage (III) is slow heating up to 650-730° C., reaching a temperature above the melting point of Al element, in order to consume the Al element in the membrane green body and increase porosity. In this stage, reaction synthesis occurs, releasing a large amount of heat, making the membrane's (i.e., the membrane green body's) temperature rise rapidly; therefore, it is necessary to control a heating-up speed of this stage to reduce reaction intensity, so as to avoid over-intense reaction and uneven heating of the (membrane) green body resulting in cracking and overall deformation of the sintered green body. A fourth stage (IV) is continuing slow heating up, to form sintering necks between powder particles and powder fibers in the membrane, so as to obtain a uniform pore structure.

[0040] According to structural characteristics of the metal membrane, electric resistance welding is selected as a welding method for jointing the metal membrane. The sintered membrane is cut to a suitable size by a shearing machine, and then formed into a cylinder shape by a tube-forming process equipment, with a upper and a lower portions of the membrane being lapped at a joint. The lap-joint is pressed firmly between disc-shaped electrodes and electrically welded, thus a cylinder membrane is obtained.

[0041] To further describe the method for preparing a Fe—Al-based metal porous membrane in accordance with the present disclosure, specific examples of the Fe—Al-based metal powder in the forms of Fe.sub.3Al/FeAl metal powders respectively are given below.

EXAMPLE 1

[0042] 1. Adding a 1000 g-500 mesh atomized Fe3Al powder, a 100 g-500 mesh Al powder, and a 100 g stainless steel fiber powder respectively into a water-based solvent (wherein, a ratio of the three powders is 10:1:1, and a specific range of the ratio may be finely adjusted accordingly), and mixing them with methyl cellulose, polyethylene glycol, etc., and stirring for uniformity, to form a stable slurry.

[0043] 2. Laying a 60 mesh 316L stainless-steel metal substrate membrane on a base plate of a tape casting machine, and then tape casting the slurry on a surface of the metal substrate membrane, by using the tape casting machine, to form a cast green body with a uniform thickness, wherein, according to a desired thickness, a spacing of a doctor blade is controlled in a range between 0.4-0.6 mm, and a moving speed of a lining belt is controlled in a range of 0.5-0.7 mm/s.

[0044] 3. Placing the base plate bearing the cast green body in a room-temperature environment, and drying it for 1-3 h.

[0045] 4. Peeling the dried membrane from the base plate, and transferring it into a vacuum sintering furnace for degreasing and sintering, wherein, a first stage is heating up to 280-320° C. and retaining temperature for 2 h, a second stage is heating up to below 450° C. and retaining temperature for 2 h, a third stage is slow heating up to 650-730° C. and retaining temperature for 1 h, and a fourth stage is continuing slow heating up to about 1300° C. to form firm sintering necks between powder particles and powder fibers in the membrane; after natural cooling, a membrane having a uniform pore structure is obtained.

[0046] 5. The resultant Fe—Al-based metal porous membrane has a smooth and flat surface, with a porosity of 40%-50%.

EXAMPLE 2

[0047] 1. Adding a 750 g-500 mesh atomized Fe3Al powder, a 25 g-500 mesh Al powder, and stainless steel fiber powder respectively into a water-based solvent (wherein, a ratio of the three powders is 30:1:1, and a specific range of the ratio may be finely adjusted accordingly), and mixing them with methyl cellulose, polyethylene glycol, etc., and stirring for uniformity, to form a stable slurry.

[0048] 2. Laying a 60 mesh 316L stainless-steel wire mesh on a base plate of a tape casting machine, and then tape casting the slurry on a surface of the metal wire mesh, by using the tape casting machine, to form a cast green body with a uniform thickness, wherein, according to a desired thickness, a spacing of a doctor blade is controlled in a range between 0.4-0.6 mm, and a moving speed of a lining belt is controlled in a range of 0.5-0.7 mm/s.

[0049] 3. Placing the base plate bearing the cast green body in a room-temperature environment, and drying it for 1-3 h.

[0050] 4. Peeling the dried membrane from the base plate, and transferring it into a vacuum sintering furnace for degreasing and sintering, wherein, a first stage is heating up to 280-320° C. and retaining temperature for 2 h, a second stage is heating up to below 450° C. and retaining temperature for 2 h, a third stage is slow heating up to 650-730° C. and retaining temperature for 1 h, and a fourth stage is continuing slow heating up to about 1300° C. to form firm sintering necks between powder particles and powder fibers in the membrane; after natural cooling, a membrane having a uniform pore structure is obtained.

[0051] 5. The resultant Fe—Al-based metal porous membrane has a smooth and flat surface, with a porosity exceeding 60%.

EXAMPLE 3

[0052] 1. Adding a 750 g-500 mesh atomized FeAl powder, a 25 g-500 mesh Al powder, and a 25 g stainless steel fiber powder respectively into a water-based solvent (wherein, a ratio of the three powders is 30:1:1, and a specific range of the ratio may be finely adjusted accordingly), and mixing them with methyl cellulose, polyethylene glycol, etc., and stirring for uniformity, to form a stable slurry.

[0053] 2. Laying a 60 mesh 316L stainless-steel wire mesh on a base plate of a tape casting machine, and then tape casting the slurry on a surface of the metal wire mesh, by using the tape casting machine, to form a cast green body with a uniform thickness, wherein, according to a desired thickness, a spacing of a doctor blade is controlled in a range between 0.4-0.6 mm, and a moving speed of a lining belt is controlled in a range of 0.5-0.7mm/s.

[0054] 3. Placing the base plate bearing the cast green body in a room-temperature environment, and drying it for 1-3 h.

[0055] 4. Peeling the dried membrane from the base plate, and transferring it into a vacuum sintering furnace for degreasing and sintering, wherein, a first stage is heating up to 280-320° C. and retaining temperature for 2 h, a second stage is heating up to below 450° C. and retaining temperature for 2 h, a third stage is slow heating up to 650-730° C. and retaining temperature for 1 h, and a fourth stage is continuing slow heating up to about 1300° C. to form firm sintering necks between powder particles and powder fibers in the membrane; after natural cooling, a membrane having a uniform pore structure is obtained.

[0056] 5. The resultant Fe—Al-based metal porous membrane has a smooth and flat surface, with a porosity exceeding 60%.

[0057] It should be noted that, based on the above detailed description of the present disclosure, a person of ordinary skill in the art can fully and clearly envisage similar embodiments for Fe—Al-based metal powders other than Fe3Al and FeAl metal powders, therefore, description of them is omitted here.

[0058] Apparently, the aforementioned embodiments are merely examples illustrated for clearly describing the present disclosure, rather than limiting the implementation ways thereof. For those skilled in the art, various changes and modifications in other different forms can be made on the basis of the aforementioned description. It is unnecessary and impossible to exhaustively list all the implementation ways herein. However, any obvious changes or modifications derived from the aforementioned description are intended to be embraced within the protection scope of the present disclosure.