CN114559041A - Preparation method of three-dimensional bicontinuous block porous copper - Google Patents
Preparation method of three-dimensional bicontinuous block porous copper Download PDFInfo
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- CN114559041A CN114559041A CN202210045073.7A CN202210045073A CN114559041A CN 114559041 A CN114559041 A CN 114559041A CN 202210045073 A CN202210045073 A CN 202210045073A CN 114559041 A CN114559041 A CN 114559041A
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- Prior art keywords
- porous copper
- block
- copper
- dimensional bicontinuous
- powder
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 45
- 239000010949 copper Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 20
- HPDFFVBPXCTEDN-UHFFFAOYSA-N copper manganese Chemical compound [Mn].[Cu] HPDFFVBPXCTEDN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000914 Mn alloy Inorganic materials 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 10
- 239000010959 steel Substances 0.000 claims abstract description 10
- 238000005260 corrosion Methods 0.000 claims abstract description 5
- 230000007797 corrosion Effects 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000011148 porous material Substances 0.000 abstract description 19
- 239000007783 nanoporous material Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 210000003041 ligament Anatomy 0.000 description 7
- 239000000463 material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005289 physical deposition Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of three-dimensional bicontinuous block porous copper, which is implemented according to the following steps: step 1, heating copper-manganese alloy powder in a corrosion solution in a water bath for dealloying to obtain porous copper powder; step 2, placing the porous copper powder obtained in the step 1 in a steel die sleeve for pressure maintaining, and pressing into blocks; and 3, placing the block-shaped body pressed in the step 2 into an atmosphere furnace, sintering, and cooling to room temperature along with the furnace to obtain the three-dimensional bicontinuous porous copper block body. The porous copper block prepared by the invention can inherit the three-dimensional bicontinuous structure of the nano porous material, and has the characteristics of uniform pore size distribution, no sintering necking, adjustable sintering pore size, higher mechanical property, capability of obtaining a large block and the like. The preparation method has the advantages of short process flow, simple preparation method, controllable structure and engineering application value.
Description
Technical Field
The invention belongs to the field of porous metal preparation, and particularly relates to a preparation method of three-dimensional bicontinuous block porous copper.
Background
The porous metal has the characteristics of low relative density, high specific strength, large specific surface area, strong permeability, good energy absorption and the like, and is a multifunctional material integrating mechanical properties, thermal properties, acoustic properties and electrical properties. Porous metals therefore have a wide range of applications, such as impact buffers, filters, heat-dissipating media, catalyst supports, sensors, steam generators, etc.
The porous copper material is prepared by various methods, such as a melt metal foaming method, a chemical and physical deposition method, a directional solidification method and a metal powder sintering method. The porous copper prepared by various process methods has different structure and performance characteristics, so that the porous copper can be used in different fields. Compared with the traditional sintered metal powder porous material, the porous metal prepared by sintering the metal powder with wider application is easy to have closed pores in the material, and the closed pores are locally generated due to mutual diffusion and aggregation recrystallization among the powder during sintering. Secondly, the pores have large fluctuation of pore necking due to the influence of powder particles, the inner walls of the pores are not smooth, the sizes of pore diameter ligaments are difficult to regulate, and a large-size porous metal material with high mechanical property is difficult to obtain by a chemical dealloying method.
Disclosure of Invention
The invention aims to provide a preparation method of three-dimensional bicontinuous block porous copper, which solves the problems that in the process of preparing a sintered porous material by the conventional method, the sizes of closed pores and pore channels and ligaments are not uniformly distributed, the size of pore diameter ligaments is difficult to regulate and control, and large blocks and high-strength porous metal materials are difficult to obtain.
The technical scheme adopted by the invention is that the preparation method of the three-dimensional bicontinuous block porous copper is implemented according to the following steps:
step 1, heating copper-manganese alloy powder in a corrosion solution in a water bath for dealloying to obtain porous copper powder;
step 2, placing the porous copper powder obtained in the step 1 in a steel die sleeve for pressure maintaining, and pressing into blocks;
and 3, placing the block-shaped body pressed in the step 2 into an atmosphere furnace, and cooling to room temperature after sintering to obtain the three-dimensional bicontinuous porous copper block body.
The present invention is also characterized in that,
the specific process of the step 1 is as follows: and (3) putting the copper-manganese alloy powder with the molar ratio of 3:7-5:5 into corrosive liquid, heating in a water bath to remove the alloy until no bubbles emerge, and obtaining the porous copper powder.
In the step 1, the concentration of the corrosive liquid is 0.1-1 mol/L.
In the step 1, HCl and H are adopted as corrosive liquid2SO4And one of HF.
The heating temperature of the water bath in the step 1 is RT-90 ℃.
In the step 2, the pressing pressure is 2MPa-10 MPa.
The sintering temperature in the step 3 is 700-1000 ℃.
The sintering time in the step 3 is 10min-240 min.
And argon is used as the atmosphere protection in the step 3.
And cooling in the step 3 adopts a furnace cooling mode.
The method has the beneficial effects that the obtained block porous copper can inherit the three-dimensional bicontinuous structure of the nano porous copper, so that the metal block porous copper with uniform distribution of pore ligaments, no closed pores, adjustable pore diameter ligament size and higher mechanical property is obtained. The preparation method has the advantages of short process flow, simple preparation method, controllable structure and engineering application value.
Drawings
FIG. 1 is a microscopic topography of porous copper obtained in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of three-dimensional bicontinuous block porous copper, which comprises the steps of heating copper-manganese alloy powder in a corrosion solution in a water bath for dealloying to obtain porous copper powder; then pressing the porous copper powder into blocks after keeping the pressure in a steel die sleeve; sintering in an atmosphere furnace, and cooling to room temperature to obtain the three-dimensional bicontinuous porous copper block.
The method is implemented according to the following steps:
step 1, heating copper-manganese alloy powder in a corrosion solution in a water bath for dealloying to obtain porous copper powder;
the specific process of the step 1 is as follows: uniformly mixing copper powder and manganese powder according to a molar ratio of 3:7-5:5, putting the copper-manganese alloy powder into corrosive liquid, heating in a water bath to remove alloy until no bubbles emerge, and obtaining porous copper powder; the concentration of the corrosive liquid is 0.1-1 mol/L; the corrosive liquid adopts HCl and H2SO4And HF, the corrosive liquid can remove the manganese by dealloying. The water bath heating temperature is RT-90 ℃.
Step 2, placing the porous copper powder obtained in the step 1 in a steel die sleeve for pressure maintaining, and pressing into blocks; the pressing pressure is 2MPa-10 MPa.
Step 3, placing the block-shaped body pressed in the step 2 into an atmosphere furnace, and cooling the sintered block-shaped body to room temperature along with the furnace to obtain a three-dimensional bicontinuous porous copper block body; the sintering temperature is 700-1000 ℃, the sintering time is 10-240 min, and the atmosphere protection is argon.
Example 1
The copper-manganese alloy powder with the copper-manganese molar ratio of 3:7 is added at 1mol/L H2SO4Heating in water bath under middle RT for dealloying until no bubbles emerge, and preparing porous copper powder; pressing the obtained porous copper powder into blocks in a steel die sleeve under the pressure of 2 MPa; sintering the copper block in an atmosphere furnace at 800 ℃ for 90min, and then cooling the copper block to room temperature along with the furnace to obtain the three-dimensional bicontinuous porous copper block.
Example 2
And heating the copper-manganese alloy powder with the copper-manganese molar ratio of 4:6 in 0.1mol/L HF at 90 ℃ in a water bath for dealloying until no bubbles emerge, thereby preparing the porous copper powder. Pressing the obtained porous copper powder into blocks in a steel die sleeve under the pressure of 8 MPa; sintering the copper block in an atmosphere furnace at 900 ℃ for 180min, and then cooling the copper block to room temperature along with the furnace to obtain the three-dimensional bicontinuous porous copper block.
Example 3
Heating copper-manganese alloy powder with a copper-manganese molar ratio of 4:6 in 0.8mol/L HCl at 70 ℃ in a water bath for dealloying until no bubbles emerge to prepare porous copper powder; pressing the obtained porous copper powder into blocks in a steel die sleeve under the pressure of 6 MPa; sintering the copper block in an atmosphere furnace at 1000 ℃ for 120min, and then cooling the copper block to room temperature along with the furnace to obtain the three-dimensional bicontinuous porous copper block.
Example 4
The copper-manganese alloy powder with the copper-manganese molar ratio of 5:5 is added at 0.5mol/L H2SO4Heating the copper powder in water bath at the temperature of 50 ℃ to remove the alloy until no bubbles emerge, and preparing porous copper powder; pressing the obtained porous copper powder in a steel die sleeve under the pressure of 10MPa to form a block; sintering the copper block in an atmosphere furnace at 1000 ℃ for 240min, and then cooling the copper block to room temperature along with the furnace to obtain the three-dimensional bicontinuous porous copper block.
Example 5
Heating copper-manganese alloy powder with a copper-manganese molar ratio of 5:5 in 0.3mol/L HCL at 40 ℃ in water bath for dealloying until no bubbles emerge to prepare porous copper powder; pressing the obtained porous copper powder into blocks in a steel die sleeve under the pressure of 5 MPa; sintering the copper block in an atmosphere furnace at 700 ℃ for 10min, and then cooling the copper block to room temperature along with the furnace to obtain the three-dimensional bicontinuous porous copper block.
The block porous copper obtained by the invention can inherit the three-dimensional bicontinuous structure of nano porous copper, so that the metal porous copper block with uniform distribution of pore ligaments, no closed pores, controllable pore diameter ligament size and higher mechanical property is obtained. The preparation method has the advantages of short process flow, simple preparation method, controllable structure and engineering application value.
Claims (8)
1. The preparation method of the three-dimensional bicontinuous block porous copper is characterized by comprising the following steps:
step 1, heating copper-manganese alloy powder in a corrosion solution in a water bath for dealloying to obtain porous copper powder;
step 2, placing the porous copper powder obtained in the step 1 in a steel die sleeve for pressure maintaining, and pressing into blocks;
and 3, placing the block pressed in the step 2 into an atmosphere furnace, sintering, and cooling to room temperature along with the furnace to obtain the three-dimensional bicontinuous block porous copper.
2. The method for preparing the three-dimensional bicontinuous block porous copper according to claim 1, wherein the specific process in the step 1 is as follows: and (3) putting the copper-manganese alloy powder into the corrosive liquid, wherein the molar ratio of the copper powder to the manganese powder is 3:7-5:5, heating in a water bath to remove the alloy until no bubbles emerge, and obtaining the porous copper powder.
3. The method for preparing the three-dimensional bicontinuous block porous copper according to claim 1, characterized in that the concentration of the corrosive liquid in the step 1 is 0.1-1 mol/L.
4. The method for preparing three-dimensional bicontinuous block porous copper according to claim 1, wherein HCl and H are adopted as corrosive liquid in the step 12SO4And HF.
5. The method for preparing the three-dimensional bicontinuous block porous copper according to claim 1, characterized in that the water bath heating temperature in step 1 is RT-90 ℃.
6. The method for preparing the three-dimensional bicontinuous bulk porous copper according to claim 1, characterized in that the pressing pressure in step 2 is 2MPa to 10 MPa.
7. The method for preparing the three-dimensional bicontinuous block porous copper according to claim 1, characterized in that the sintering temperature in step 3 is 700-1000 ℃ and the sintering time is 10-240 min.
8. The method according to claim 1, wherein the atmosphere is argon.
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2022
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