CN110947969A - Preparation method of metallic nickel porous material with controllable main pore diameter value gradient distribution - Google Patents
Preparation method of metallic nickel porous material with controllable main pore diameter value gradient distribution Download PDFInfo
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- CN110947969A CN110947969A CN201911311513.3A CN201911311513A CN110947969A CN 110947969 A CN110947969 A CN 110947969A CN 201911311513 A CN201911311513 A CN 201911311513A CN 110947969 A CN110947969 A CN 110947969A
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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
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
- B22F3/1134—Inorganic fillers
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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
- B22F3/001—Starting from powder comprising reducible metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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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
- B22F3/11—Making porous workpieces or articles
- B22F3/1103—Making porous workpieces or articles with particular physical characteristics
- B22F3/1109—Inhomogenous pore distribution
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention provides a preparation method of a metallic nickel porous material with controllable main pore size value gradient distribution, which comprises the steps of firstly screening pore-forming agents according to different particle sizes, and then fully mixing the pore-forming agents with carbonyl nickel powder to obtain mixed powder; respectively selecting corresponding dies from the inner layer to the outer layer according to the sequence to carry out combined isostatic pressing to obtain a pressed green body; pre-sintering and sintering the pressed green body under the protection of atmosphere to obtain a sintered body; and cleaning the sintered blank, removing the pore-forming agent, and drying to obtain the metallic nickel porous material with controllable gradient distribution of the main pore diameter value. The method of the invention designs the combined pressing with different parameters, and controls the particle size of the pore-forming agent, the weight ratio of the carbonyl nickel powder to the pore-forming agent, the size of the die and the processing size of the pressed green body in a matching way in each pressing procedure, thereby obtaining the metallic nickel porous material with controllable gradient distribution of the main pore size value. The pore diameter of the metal nickel porous material changes along with the thickness or diameter direction of the material, and the pore diameter value of each layer can be reasonably controlled.
Description
Technical Field
The invention belongs to the field of preparing porous metal materials by a powder metallurgy method, and particularly relates to a preparation method of a metal nickel porous material with controllable gradient distribution of main pore diameter values.
Background
The porous metal is composed of a metal skeleton and pores, has the basic characteristics of a metal material, and is remarkably characterized in that the interior of the porous metal has a large number of pores compared with a dense metal material. The porous metal material has a plurality of excellent characteristics due to a large number of internal pores, and has the advantages of small specific gravity, large specific surface area, good energy absorption performance, high heat exchange and heat dissipation capacity, good sound absorption, excellent permeability, good electromagnetic wave absorption and the like.
Due to the excellent permeability of the porous metal, the gas or liquid is filtered and separated by utilizing the blocking and trapping effect of the pore passages of the porous metal on solid particles in the fluid medium, so that the purification or separation effect of the medium is achieved. The porous metal mesoporous structure can be used for an energy absorption device, and can be applied to automobile anti-impact gears, spacecraft landing gears, energy absorption linings of elevators, conveyor safety pads, high-speed grinding machine protective covers and the like. Porous metal materials are also used for battery electrode materials, and porous nickel is used as an electrode in batteries, fuel cells, and air cells, and porosity is required to be as high as possible. Meanwhile, the metal porous material is also widely used as a fluid distribution and control device, a heat exchange device, an electromagnetic shielding device, an electromagnetic compatibility device and the like, and the porous metal material such as titanium and the like is also widely used as a biological material.
Disclosure of Invention
The invention aims to provide a preparation method of a metallic nickel porous material with controllable main pore size value gradient distribution.
In order to realize the purpose, the following technical scheme is adopted:
a preparation method of a metallic nickel porous material with controllable main pore size value gradient distribution comprises the following steps:
crushing 100-500-mesh pore-forming agents, and screening the crushed pore-forming agents according to particle sizes to obtain two or n pore-forming agents with different particle sizes; wherein n is more than or equal to 3;
when two pore-forming agents with different particle sizes are obtained, mixing the pore-forming agent with one particle size with the nickel carbonyl powder to obtain mixed powder a;
mixing the pore-forming agent with the other particle size with the nickel carbonyl powder to obtain mixed powder b;
putting the mixed powder a into a die, and performing isostatic pressing to obtain a green body a;
processing the green body a into a green body a1 with a regular shape;
putting the green body a1 into a mould, then putting the mixed powder b into a gap between the green body a1 and the mould, and carrying out isostatic pressing to obtain a cylindrical green body b 1;
pre-sintering and sintering the green body b1 in a reducing atmosphere to obtain a metallic nickel porous material with controllable gradient distribution of main pore diameter values;
when n kinds of pore-forming agents with different particle sizes are obtained,
mixing the pore-forming agent with the first particle size with the nickel carbonyl powder to obtain mixed powder a;
combining the pore-forming agent with the second particle size with the nickel carbonyl powder to obtain mixed powder b;
by analogy, mixing the pore-forming agent with the nth particle size with the nickel carbonyl powder to obtain mixed powder n;
putting the mixed powder a into a die, and performing isostatic pressing to obtain a green body a;
processing the green body a into a green body a1 with regular external dimensions;
putting the green body a1 into a mould, then placing the mixed powder b into a gap between the green body a1 and the mould, and carrying out isostatic pressing to obtain a green body b;
processing the obtained green body b into a green body b1 with regular external dimensions;
and so on to obtain a green body n,
processing the green body n into a green body n1 with regular external dimensions;
and (3) pre-sintering and sintering the green body n1 in a reducing atmosphere to obtain the metallic nickel porous material with controllable main pore size value gradient distribution.
The invention is further improved in that the pore-forming agent is NaCl.
The further improvement of the invention is that the particle size of the carbonyl nickel powder is less than 500 meshes.
The invention has the further improvement that the moulds are all isostatic pressing rubber moulds, the moulds are hollow cylinders, and rubber seal heads are arranged at two ends of the hollow cylinders; the outer diameter of the rubber seal heads arranged at the two ends of the mold is the same as the inner diameter of the rubber mold.
The further improvement of the invention is that when the pore-forming agent with each particle size is mixed with the nickel carbonyl powder, the mass ratio of the pore-forming agent with each particle size to the nickel carbonyl powder is 1: 1.5 to 1.7.
The further improvement of the invention is that the pressure of isostatic pressing is 80-150 MPa, and the pressure maintaining time is 2-5 min.
A further improvement of the invention is that the reducing atmosphere is a hydrogen atmosphere.
The further improvement of the invention is that the pre-sintering process is as follows: heating to 700-850 ℃ at a heating rate of 3-8 ℃/min for pre-sintering, and keeping the temperature for 4-10 h.
The further improvement of the invention is that the sintering process is as follows: heating to 900-1000 ℃ at a heating rate of 5-15 ℃/min for sintering, and keeping the temperature for 30-90 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention presses the green body by the isostatic pressing combined pressing method, can obtain the pressed green bodies with the same density at each part, obtains the metallic nickel porous material with controllable main pore size value gradient distribution after the presintering and sintering are finished, has the same density at each part of the generated metallic nickel porous material, can control the thickness of each gradient layer by adjusting the combined pressing process parameters, has high feasibility and wide adaptability, and is worthy of popularization and application.
Furthermore, the invention adopts an isostatic pressing combined pressing process route to control the size of an isostatic pressing die and the processing process parameters of a green body, and simultaneously controls the corresponding process parameters of the particle size of a pore-forming agent, the mixing weight ratio of the carbonyl nickel powder and the pore-forming agent, and the like, so as to prepare the metallic nickel porous material with controllable main pore size value gradient distribution.
Drawings
FIG. 1 is a schematic diagram of the preparation and molding of a metallic nickel porous material with controllable gradient distribution of main pore diameter values.
Detailed Description
The present invention will be described in detail below with reference to specific examples.
Referring to fig. 1, a method for preparing a metallic nickel porous material with controllable gradient distribution of main pore diameter values comprises the following steps:
crushing 100-500-mesh pore-forming agents, and screening the crushed pore-forming agents according to particle sizes to obtain two or n pore-forming agents with different particle sizes; wherein n is more than or equal to 3; the maximum n is 8, namely the particle size is 100-150, 150-200, 200-250, 250-300, 300-350, 350-400, 400-450, 450-500, the particle size range of each pore-forming agent is at least 50 meshes, and the screening with the range being too small is difficult to realize.
When two pore-forming agents with different particle sizes are obtained, mixing the pore-forming agent with one particle size with the nickel carbonyl powder to obtain mixed powder a;
mixing the pore-forming agent with the other particle size with the nickel carbonyl powder to obtain mixed powder b;
putting the mixed powder a into a die, and performing isostatic pressing to obtain a green body a;
processing the green body a into a green body a1 with a regular shape;
putting the green body a1 into a mould, then putting the mixed powder b into a gap between the green body a1 and the mould, and carrying out isostatic pressing to obtain a cylindrical green body b 1;
pre-sintering and sintering the green body b1 in a reducing atmosphere to obtain a metallic nickel porous material with controllable gradient distribution of main pore diameter values;
when n kinds of pore-forming agents with different particle sizes are obtained,
mixing the pore-forming agent with the first particle size with the nickel carbonyl powder to obtain mixed powder a;
combining the pore-forming agent with the second particle size with the nickel carbonyl powder to obtain mixed powder b;
by analogy, mixing the pore-forming agent with the nth particle size with the nickel carbonyl powder to obtain mixed powder n;
putting the mixed powder a into a die, and performing isostatic pressing to obtain a green body a;
processing the green body a into a green body a1 with regular external dimensions;
putting the green body a1 into a mould, then placing the mixed powder b into a gap between the green body a1 and the mould, and carrying out isostatic pressing to obtain a green body b;
processing the obtained green body b into a green body b1 with regular external dimensions;
and so on to obtain a green body n,
processing the green body n into a green body n1 with regular external dimensions;
and (3) pre-sintering and sintering the green body n1 in a reducing atmosphere to obtain the metallic nickel porous material with controllable main pore size value gradient distribution.
Specifically, when n is 3, the method comprises the following steps:
step 1: crushing the pore-forming agent, screening the crushed pore-forming agent according to the particle size, and respectively obtaining a pore-forming agent a, a pore-forming agent b and a pore-forming agent c with different particle sizes according to the particle size of the powder;
step 2: fully mixing the pore-forming agent a and the carbonyl nickel powder according to a certain proportion to obtain mixed powder a;
and step 3: fully mixing the pore-forming agent b and the carbonyl nickel powder according to a certain proportion to obtain mixed powder b;
and 4, step 4: fully mixing the pore-forming agent c and the carbonyl nickel powder according to a certain proportion to obtain mixed powder c;
and 5: putting the mixed powder a into a die 1, and performing isostatic pressing to obtain a cylindrical green body a;
step 6: machining the green body a obtained in the step 5 into a green body a1 with a regular external dimension through mechanical machining;
and 7: putting the green body a1 obtained in the step 6 into a mould 2, putting the mixed powder b obtained in the step 3 into a gap between the green body a1 and the mould 2, and performing isostatic pressing to obtain a cylindrical green body b;
and 8: machining the green body b obtained in the step 7 into a green body b1 with a regular external dimension through mechanical machining;
and step 9: putting the green body b1 obtained in the step 8 into a mould 3, putting the mixed powder c obtained in the step 4 into a gap between the green body b1 and the mould 3, and performing isostatic pressing to obtain a cylindrical green body c;
step 10: machining the green body c obtained in step 9 into a green body c1 having a regular outer dimension by machining;
step 11: and (3) pre-sintering and sintering the green compact c1 obtained in the step (10) under the protection of a reducing atmosphere to obtain the metallic nickel porous material with controllable gradient distribution of the main pore size value.
In the preparation method of the metallic nickel porous material with controllable main pore size value gradient distribution, the step 1 meets the following conditions:
① the particle size requirements of the pore-forming agent a, the pore-forming agent b and the pore-forming agent c are all range values, and the particle size range of the same pore-forming agent is not more than 50 meshes;
② the particle size ranges of the pore-forming agent a and the pore-forming agent c are the same, and the particle size ranges of the pore-forming agent b, the pore-forming agent a and the pore-forming agent c are different;
③ the pore-forming agent a, the pore-forming agent b and the pore-forming agent c have different particle size ranges.
In the preparation method of the metallic nickel porous material with controllable main pore size value gradient distribution, in the step 1, the pore-forming agent is NaCl, and the powder is spherical or irregular. The grain size range of the pore-forming agent is 100 meshes-500 meshes.
In the preparation method of the metal nickel porous material with controllable main pore size value gradient distribution, the nickel powder in the steps 1, 2 and 3 is carbonyl nickel powder, the particle size of the carbonyl nickel powder is-500 meshes, and the shape of the carbonyl nickel powder is spherical or irregular.
In the preparation method of the metallic nickel porous material with controllable main pore size value gradient distribution, in the step 2, the mass ratio of the nickel powder to the pore-forming agent a is 1.5-1.7: 1.
in the preparation method of the metallic nickel porous material with controllable main pore size value gradient distribution, in the step 3, the mass ratio of the nickel powder to the pore-forming agent b is 1.5-1.7: 1.
In the preparation method of the metallic nickel porous material with controllable main pore size value gradient distribution, in the step 4, the mass ratio of the nickel powder to the pore-forming agent c is 1.5-1.7: 1.
In the preparation method of the metal nickel porous material with the controllable main pore diameter value gradient distribution, in the step 5, the mold 1 is an isostatic pressing rubber mold, the mold 1 is a hollow cylinder, and rubber end sockets are arranged at two ends of the hollow cylinder; the outer diameter of the rubber seal heads arranged at the two ends of the die 1 is the same as the inner diameter of the rubber die.
In the preparation method of the metallic nickel porous material with controllable main pore size gradient distribution, in step 6, the green compact a1 is a solid cylinder with regular external dimension and flush end face.
In the preparation method of the metal nickel porous material with the controllable main pore diameter value gradient distribution, in step 7, the mold 2 is an isostatic pressing rubber mold, the mold 2 is a hollow cylinder, and rubber end sockets are arranged at two ends of the hollow cylinder; the outer diameter of the rubber seal heads arranged at the two ends of the die 2 is the same as the inner diameter of the rubber die in size; the inner diameter of the die 2 is larger than the diameter of the green body a1 obtained in step 6.
In the preparation method of the metallic nickel porous material with controllable main pore size gradient distribution, in step 8, the green body b1 is a solid cylinder with regular external dimension and flush end face.
In the preparation method of the metal nickel porous material with the controllable main pore diameter value gradient distribution, in step 9, the mold 3 is an isostatic pressing rubber mold, the mold 3 is a hollow cylinder, and rubber end sockets are arranged at two ends of the hollow cylinder; the outer diameter of the rubber seal heads arranged at the two ends of the mold 3 is the same as the inner diameter of the rubber mold in size; the inner diameter of the die 3 is larger than the diameter of the green body b1 obtained in step 8.
In the preparation method of the metallic nickel porous material with controllable main pore size gradient distribution, in step 10, the green compact c1 is a solid cylinder with regular external dimension and flush end face.
In the preparation method of the metal nickel porous material with the controllable main pore size value gradient distribution, isostatic pressing pressure in the steps 5, 7 and 9 is 80-150 MPa, and pressure maintaining time is 2-5 min.
In the preparation method of the metal nickel porous material with the controllable main pore size value gradient distribution, in step 11, the protective atmosphere is hydrogen protection; the pre-sintering process comprises the following steps: raising the temperature from room temperature to 700-850 ℃ at a temperature raising rate of 3-8 ℃/min for pre-sintering, and keeping the temperature for 4-10 h; the sintering process comprises the following steps: heating from room temperature to 900-1000 ℃ at a heating rate of 5-15 ℃/min for sintering, and keeping the temperature for 30-90 min.
In the present invention, the pore-forming agent may be other substances, but the type of the pore-forming agent needs to be determined and selected according to the process temperature, the melting point of the pore-forming agent and the method for cleaning the pore-forming agent, and NaCl is selected because of its high solubility in water and its melting point matched with the process temperature. NaCl was the best and NaF was also used, but the effect was poor.
The following are specific examples.
Example 1
The preparation method of the metallic nickel porous material with controllable gradient distribution of the main pore diameter value comprises the following steps:
step 1: crushing the pore-forming agent, sieving the crushed pore-forming agent according to the particle size, and respectively obtaining a pore-forming agent a, a pore-forming agent b and a pore-forming agent c according to different powder particle sizes, wherein the particle size of the pore-forming agent a is 150-200 meshes, the particle size of the pore-forming agent b is 250-300 meshes, and the particle size of the pore-forming agent c is 300-350 meshes.
Step 2: mixing a pore-forming agent a and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder a;
and step 3: mixing a pore-forming agent b and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder b;
and 4, step 4: mixing a pore-forming agent c and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder c;
and 5: putting the mixed powder a into a die 1, and performing isostatic pressing to obtain a cylindrical green body a;
step 6: machining the green body a obtained in the step 5 into a cylindrical green body a1 with the external dimension of phi 18 x 70mm through mechanical machining;
and 7: putting the green body a1 obtained in the step 6 into a mould 2, putting the mixed powder b obtained in the step 3 into a gap between the green body a1 and the mould 2, and performing isostatic pressing to obtain a cylindrical green body b;
and 8: machining the green body b obtained in the step 7 into a cylindrical green body b1 with the external dimension of phi 25 x 70mm through mechanical machining;
and step 9: putting the green body b1 obtained in the step 8 into a mould 3, putting the mixed powder c obtained in the step 4 into a gap between the green body b1 and the mould 3, and performing isostatic pressing to obtain a cylindrical green body c;
step 10: machining the green compact c obtained in the step 9 into a cylindrical green compact c1 with the external dimension phi of 40X 70mm through mechanical machining;
step 11: and (3) presintering and sintering the green blank c1 obtained in the step (10) under the protection of a reducing atmosphere, wherein the temperature is increased to 750 ℃ at the heating rate of 3 ℃/min for presintering during presintering, the heat is preserved for 6h, the sintering is carried out after the pore-forming agent is completely removed, the temperature is increased to 950 ℃ at the heating rate of 15 ℃/min for sintering during sintering, the heat is preserved for 0.5h, and the width of the inner layer is 9mm, the main pore diameter is 7.5-9 mu m, the width of the middle layer is 3.5mm, the main pore diameter is 3.7-5.0 mu m, the width of the outer layer is 7.5mm, and the main pore diameter is 2.2-4.5 mu m after sintering is completed.
Example 2
The preparation method of the metallic nickel porous material with controllable gradient distribution of the main pore diameter value comprises the following steps:
step 1: crushing the pore-forming agent, sieving the crushed pore-forming agent according to the particle size, and respectively obtaining a pore-forming agent a, a pore-forming agent b and a pore-forming agent c according to different powder particle sizes, wherein the particle size of the pore-forming agent a is 150-200 meshes, the particle size of the pore-forming agent b is 250-300 meshes, and the particle size of the pore-forming agent c is 150-200 meshes.
Step 2: mixing a pore-forming agent a and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder a;
and step 3: mixing a pore-forming agent b and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder b;
and 4, step 4: mixing a pore-forming agent c and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder c;
and 5: putting the mixed powder a into a die 1, and performing isostatic pressing to obtain a cylindrical green body a;
step 6: machining the green body a obtained in the step 5 into a cylindrical green body a1 with the external dimension of phi 12 x 70mm through mechanical machining;
and 7: putting the green body a1 obtained in the step 6 into a mould 2, putting the mixed powder b obtained in the step 3 into a gap between the green body a1 and the mould 2, and performing isostatic pressing to obtain a cylindrical green body b;
and 8: machining the green body b obtained in the step 7 into a cylindrical green body b1 with the external dimension of phi 30 x 70mm through mechanical machining;
and step 9: putting the green body b1 obtained in the step 8 into a mould 3, putting the mixed powder c obtained in the step 4 into a gap between the green body b1 and the mould 3, and performing isostatic pressing to obtain a cylindrical green body c;
step 10: machining the green compact c obtained in the step 9 into a cylindrical green compact c1 with the external dimension phi of 45 x 70mm through mechanical machining;
step 11: and (3) presintering and sintering the green blank c1 obtained in the step (10) under the protection of a reducing atmosphere, wherein the temperature is increased to 750 ℃ at the heating rate of 8 ℃/min for presintering during presintering, the temperature is kept for 6h, the sintering is carried out after the pore-forming agent is completely removed, the temperature is increased to 950 ℃ at the heating rate of 5 ℃/min for sintering during sintering, the temperature is kept for 0.5h, and after the sintering is completed, the inner layer with the width of 6mm, the main pore diameter of 7.5-9 mu m, the middle layer with the width of 9mm, the main pore diameter of 3.7-5.0 mu m, the outer layer with the width of 7.5mm and the main pore diameter of 7.5-.
Example 3
The preparation method of the metallic nickel porous material with controllable gradient distribution of the main pore diameter value comprises the following steps:
step 1: crushing the pore-forming agent, sieving the crushed pore-forming agent according to the particle size, and respectively obtaining a pore-forming agent a, a pore-forming agent b and a pore-forming agent c according to different powder particle sizes, wherein the particle size of the pore-forming agent a is 150-200 meshes, the particle size of the pore-forming agent b is 250-300 meshes, and the particle size of the pore-forming agent c is 150-200 meshes.
Step 2: mixing a pore-forming agent a and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder a;
and step 3: mixing a pore-forming agent b and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder b;
and 4, step 4: mixing a pore-forming agent c and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder c;
and 5: putting the mixed powder a into a die 1, and performing isostatic pressing to obtain a cylindrical green body a;
step 6: machining the green body a obtained in the step 5 into a cylindrical green body a1 with the external dimension of phi 12 x 70mm through mechanical machining;
and 7: putting the green body a1 obtained in the step 6 into a mould 2, putting the mixed powder b obtained in the step 3 into a gap between the green body a1 and the mould 2, and performing isostatic pressing to obtain a cylindrical green body b;
and 8: machining the green body b obtained in the step 7 into a cylindrical green body b1 with the external dimension of phi 30 x 70mm through mechanical machining;
and step 9: putting the green body b1 obtained in the step 8 into a mould 3, putting the mixed powder c obtained in the step 4 into a gap between the green body b1 and the mould 3, and performing isostatic pressing to obtain a cylindrical green body c;
step 10: machining the green compact c obtained in the step 9 into a cylindrical green compact c1 with the external dimension phi of 45 x 70mm through mechanical machining;
step 11: and (3) presintering and sintering the green blank c1 obtained in the step (10) under the protection of reducing atmosphere, wherein the temperature is increased to 750 ℃ at the heating rate of 5 ℃/min for presintering during presintering, the temperature is kept for 6h, the sintering is carried out after the pore-forming agent is completely removed, the temperature is increased to 950 ℃ at the heating rate of 10 ℃/min for sintering during sintering, the temperature is kept for 0.5h, and the width of the inner layer is 6mm, the main aperture is 7.5-9 mu m, the width of the middle layer is 9mm, the main aperture is 3.7-5.0 mu m, the width of the outer layer is 7.5mm, and the main aperture is 7.5-9 mu m after sintering is completed.
Example 4
The preparation method of the metallic nickel porous material with controllable gradient distribution of the main pore diameter value comprises the following steps:
step 1: crushing the pore-forming agent, sieving the crushed pore-forming agent according to the particle size, and respectively obtaining a pore-forming agent a, a pore-forming agent b, a pore-forming agent c and a pore-forming agent d according to different powder particle sizes, wherein the particle size of the pore-forming agent a is 100-150 meshes, the particle size of the pore-forming agent b is 200-250 meshes, the particle size of the pore-forming agent c is 300-350 meshes, and the particle size of the pore-forming agent d is 400-450 meshes.
Step 2: mixing a pore-forming agent a and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder a;
and step 3: mixing a pore-forming agent b and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder b;
and 4, step 4: mixing a pore-forming agent c and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder c;
and 5: mixing a pore-forming agent d and carbonyl nickel powder in a weight ratio of 1: 1.7, fully mixing to obtain mixed powder d;
step 6: putting the mixed powder a into a die 1, and performing isostatic pressing to obtain a cylindrical green body a;
and 7: machining the green body a obtained in the step 6 into a cylindrical green body a1 with the external dimension of phi 15 multiplied by 95mm through mechanical machining;
and 8: putting the green body a1 obtained in the step 7 into a mould 2, putting the mixed powder b obtained in the step 3 into a gap between the green body a1 and the mould 2, and performing isostatic pressing to obtain a cylindrical green body b;
and step 9: machining the green body b obtained in the step 8 into a cylindrical green body b1 with the external dimension of phi 40 multiplied by 95mm through mechanical machining;
step 10: putting the green body b1 obtained in the step 9 into a mould 3, putting the mixed powder c obtained in the step 4 into a gap between the green body b1 and the mould 3, and performing isostatic pressing to obtain a cylindrical green body c;
step 11: machining the green compact c obtained in the step 10 into a cylindrical green compact c1 with the external dimension phi of 55X 95mm by mechanical machining;
step 12: putting the green compact c1 obtained in the step 11 into a mold 4, putting the mixed powder d obtained in the step 5 into a gap between the green compact c1 and the mold 4, and performing isostatic pressing to obtain a cylindrical green compact d;
step 13: machining the green body d obtained in the step 12 into a cylindrical green body d1 with the external dimension phi of 70 x 95mm by mechanical machining;
step 14: and (3) presintering and sintering the green body c1 obtained in the step (10) under the protection of a reducing atmosphere, wherein the temperature is increased to 750 ℃ at the heating rate of 7 ℃/min for presintering during presintering, the heat is preserved for 6h, the sintering is carried out after the pore-forming agent is completely removed, the temperature is increased to 950 ℃ at the heating rate of 8 ℃/min for sintering during sintering, the heat is preserved for 0.5h, and the width of an inner layer is 7.5mm, the main pore diameter is 9-11.5 mu m, the widths of two middle layers are 12.5mm and 7.5mm respectively, the main pore diameters are 4.2-6.3 mu m and 2.2-4.5 mu m respectively, the width of an outer layer is 7.5mm, and the main pore diameter is 0.8-2.0 mu m respectively after the sintering is.
Example 5
Crushing a pore-forming agent of 100-500 meshes, and screening the crushed pore-forming agent according to particle size to obtain two pore-forming agents with different particle sizes; one is 100 to 150 meshes, and the other is 200 to 250 meshes;
mixing a pore-forming agent with a particle size and carbonyl nickel powder according to a mass ratio of 1: 1.5, mixing to obtain mixed powder a;
and (2) mixing another pore-forming agent with the particle size and the nickel carbonyl powder according to the mass ratio of 1: 1.5, mixing to obtain mixed powder b;
putting the mixed powder a into a die, and performing isostatic pressing to obtain a green body a;
processing the green body a into a green body a1 with a regular shape;
putting the green body a1 into a mould, then putting the mixed powder b into a gap between the green body a1 and the mould, and carrying out isostatic pressing to obtain a cylindrical green body b 1;
pre-sintering and sintering the green body b1 in a reducing atmosphere, wherein the temperature is increased to 750 ℃ at the heating rate of 6 ℃/min for pre-sintering, the temperature is kept for 6h, the pore-forming agent is completely removed and then sintering is carried out, the temperature is increased to 950 ℃ at the heating rate of 12 ℃/min for sintering, the temperature is kept for 0.5h, and the metallic nickel porous material with controllable main pore size value gradient distribution can be obtained after sintering is finished;
the aperture of the metallic nickel porous material changes along with the thickness or diameter direction of the material, and the aperture value of each layer can be reasonably controlled. The metal nickel porous material is prepared by mixing, combining, pressing, sintering and cleaning metal carbonyl nickel powder with certain granularity and pore-forming agent powder with certain granularity. The preparation method mainly comprises the following steps: screening the pore-forming agent according to different particle sizes, and then fully mixing the pore-forming agent with the nickel carbonyl powder to obtain mixed powder; respectively selecting corresponding dies from the inner layer to the outer layer according to the sequence to carry out combined isostatic pressing to obtain a pressed green body; pre-sintering and sintering the pressed green body under the protection of atmosphere to obtain a sintered body; and cleaning the sintered blank, removing the pore-forming agent, and drying to obtain the metallic nickel porous material with controllable gradient distribution of the main pore diameter value. The method of the invention designs the combined pressing with different parameters, and controls the particle size of the pore-forming agent, the weight ratio of the carbonyl nickel powder to the pore-forming agent, the size of the die and the processing size of the pressed green body in a matching way in each pressing procedure, thereby obtaining the metallic nickel porous material with controllable gradient distribution of the main pore size value.
Claims (9)
1. A preparation method of a metallic nickel porous material with controllable main pore size value gradient distribution is characterized by comprising the following steps:
crushing 100-500-mesh pore-forming agents, and screening the crushed pore-forming agents according to particle sizes to obtain two or n pore-forming agents with different particle sizes; wherein n is more than or equal to 3;
when two pore-forming agents with different particle sizes are obtained, mixing the pore-forming agent with one particle size with the nickel carbonyl powder to obtain mixed powder a;
mixing the pore-forming agent with the other particle size with the nickel carbonyl powder to obtain mixed powder b;
putting the mixed powder a into a die, and performing isostatic pressing to obtain a green body a;
processing the green body a into a green body a1 with a regular shape;
putting the green body a1 into a mould, then putting the mixed powder b into a gap between the green body a1 and the mould, and carrying out isostatic pressing to obtain a cylindrical green body b 1;
pre-sintering and sintering the green body b1 in a reducing atmosphere to obtain a metallic nickel porous material with controllable gradient distribution of main pore diameter values;
when n kinds of pore-forming agents with different particle sizes are obtained,
mixing the pore-forming agent with the first particle size with the nickel carbonyl powder to obtain mixed powder a;
combining the pore-forming agent with the second particle size with the nickel carbonyl powder to obtain mixed powder b;
by analogy, mixing the pore-forming agent with the nth particle size with the nickel carbonyl powder to obtain mixed powder n;
putting the mixed powder a into a die, and performing isostatic pressing to obtain a green body a;
processing the green body a into a green body a1 with regular external dimensions;
putting the green body a1 into a mould, then placing the mixed powder b into a gap between the green body a1 and the mould, and carrying out isostatic pressing to obtain a green body b;
processing the obtained green body b into a green body b1 with regular external dimensions;
and so on to obtain a green body n,
processing the green body n into a green body n1 with regular external dimensions;
and (3) pre-sintering and sintering the green body n1 in a reducing atmosphere to obtain the metallic nickel porous material with controllable main pore size value gradient distribution.
2. The method for preparing the metallic nickel porous material with the controllable main pore size gradient distribution as claimed in claim 1, wherein the pore-forming agent is NaCl.
3. The method according to claim 1, wherein the particle size of the nickel carbonyl powder is less than 500 mesh.
4. The method for preparing the metallic nickel porous material with the controllable main pore diameter value gradient distribution according to claim 1, wherein the dies are isostatic pressing rubber dies, the dies are hollow cylinders, and rubber end sockets are arranged at two ends of each die; the outer diameter of the rubber seal heads arranged at the two ends of the mold is the same as the inner diameter of the rubber mold.
5. The method according to claim 1, wherein when the pore-forming agent with each particle size is mixed with the nickel carbonyl powder, the mass ratio of the pore-forming agent with each particle size to the nickel carbonyl powder is 1: 1.5 to 1.7.
6. The method for preparing the metallic nickel porous material with the controllable main pore diameter value gradient distribution according to claim 1, wherein the isostatic pressing pressure is 80-150 MPa, and the pressure maintaining time is 2-5 min.
7. The method for preparing the metallic nickel porous material with the controllable main pore size gradient distribution as claimed in claim 1, wherein the reducing atmosphere is a hydrogen atmosphere.
8. The method for preparing the metallic nickel porous material with the controllable main pore size gradient distribution according to claim 1, wherein the pre-sintering process comprises the following steps: heating to 700-850 ℃ at a heating rate of 3-8 ℃/min for pre-sintering, and keeping the temperature for 4-10 h.
9. The method for preparing the metallic nickel porous material with the controllable main pore size gradient distribution according to claim 1, wherein the sintering processes are as follows: heating to 900-1000 ℃ at a heating rate of 5-15 ℃/min for sintering, and keeping the temperature for 30-90 min.
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