CN111687424B - Preparation method and application of copper-iron alloy powder - Google Patents
Preparation method and application of copper-iron alloy powder Download PDFInfo
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- CN111687424B CN111687424B CN202010425932.6A CN202010425932A CN111687424B CN 111687424 B CN111687424 B CN 111687424B CN 202010425932 A CN202010425932 A CN 202010425932A CN 111687424 B CN111687424 B CN 111687424B
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- 239000000843 powder Substances 0.000 title claims abstract description 40
- 229910000640 Fe alloy Inorganic materials 0.000 title claims abstract description 29
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 49
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 239000010949 copper Substances 0.000 claims abstract description 17
- 206010012601 diabetes mellitus Diseases 0.000 claims abstract description 9
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 8
- 238000003723 Smelting Methods 0.000 claims abstract description 6
- 241000700605 Viruses Species 0.000 claims abstract description 6
- 230000012010 growth Effects 0.000 claims abstract description 6
- 238000000889 atomisation Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000000956 alloy Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 16
- 238000009692 water atomization Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000011068 loading method Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 238000007639 printing Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 230000003064 anti-oxidating effect Effects 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 230000002401 inhibitory effect Effects 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 5
- 230000007797 corrosion Effects 0.000 claims description 5
- 238000005260 corrosion Methods 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000010146 3D printing Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 3
- 238000007885 magnetic separation Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000006722 reduction reaction Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims 1
- 238000003825 pressing Methods 0.000 abstract description 9
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 241000894006 Bacteria Species 0.000 abstract description 3
- 229910000881 Cu alloy Inorganic materials 0.000 abstract description 3
- 239000011812 mixed powder Substances 0.000 description 8
- 208000008960 Diabetic foot Diseases 0.000 description 6
- 206010052428 Wound Diseases 0.000 description 6
- 208000027418 Wounds and injury Diseases 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000009694 cold isostatic pressing Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 208000024891 symptom Diseases 0.000 description 4
- 201000001421 hyperglycemia Diseases 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- -1 Silver ions Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000029663 wound healing Effects 0.000 description 2
- 206010011409 Cross infection Diseases 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000002266 amputation Methods 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000031018 biological processes and functions Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000009693 chronic damage Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000034994 death Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000004064 dysfunction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000001508 eye Anatomy 0.000 description 1
- 230000002641 glycemic effect Effects 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 210000002216 heart Anatomy 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003914 insulin secretion Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 230000005541 medical transmission Effects 0.000 description 1
- 208000030159 metabolic disease Diseases 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
Classifications
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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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/26—Iron; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/34—Copper; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/02—Drugs for dermatological disorders for treating wounds, ulcers, burns, scars, keloids, or the like
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- A—HUMAN NECESSITIES
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P3/00—Drugs for disorders of the metabolism
- A61P3/08—Drugs for disorders of the metabolism for glucose homeostasis
- A61P3/10—Drugs for disorders of the metabolism for glucose homeostasis for hyperglycaemia, e.g. antidiabetics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
-
- B22F1/0003—
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0425—Copper-based alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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- A—HUMAN NECESSITIES
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- 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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
- B22F2009/0828—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid with water
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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Abstract
The invention provides a preparation method and application of copper-iron alloy powder, wherein the method comprises the following steps: mixing raw copper powder and raw iron powder, preparing a mixed base block by pressing, performing spark plasma sintering, smelting, and performing ingot atomization powder preparation to obtain copper-iron alloy powder; the prepared copper-iron alloy powder is applied to the germ covering layer of diabetes mellitus to inhibit the growth of viruses; the manufacturing method provided by the invention has the characteristics of low energy consumption and stronger environment protection; the whole quality of the preparation method provided by the invention is easy to control, and the whole working procedure is more suitable for mass production; the invention utilizes the characteristic that copper and copper alloy can effectively inhibit the growth of viruses and bacteria, and the prepared copper-iron alloy powder has the characteristic of low cost, can effectively replace silver ion antibacterial materials with relatively high cost, and is more suitable for mass popularization.
Description
Technical Field
The invention relates to the technical field of preparation processes of CuW90 materials, in particular to a preparation method and application of copper-iron alloy powder.
Background
Diabetes is a group of metabolic diseases characterized by hyperglycemia, as documented. Hyperglycemia is caused by defective insulin secretion or impaired biological action, or both. The prolonged presence of hyperglycemia in diabetes leads to chronic damage, dysfunction of various tissues, especially the eyes, kidneys, heart, blood vessels, nerves. In clinic, diabetic foot is a serious complication of diabetes, often the main cause of disability and death for patients. In recent years, with increasing emphasis on glycemic control and hospital infection control, the probability of amputation has been significantly reduced. Although silver-containing dressing has gained wide acceptance in diabetic foot clinical applications, its effectiveness in promoting wound healing has not been fully investigated.
The method is also very critical in treating the wound and intervening the medicine in time, and can effectively accelerate the wound healing by selecting proper dressing and medicine, regulating the microcirculation of patients, properly controlling the blood sugar and the like. Silver ions are used as an antibacterial material dressing for bacteriostasis of diabetic foot wounds in the prior art.
However, due to the high cost of silver, it is difficult to use it in large amounts in diabetic foot patients. And the study proves that: copper and copper alloy can effectively inhibit disease transmission caused by bacteria; therefore, there is a need for a low cost antimicrobial material that can be applied to diabetic foot wounds in place of silver ions.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method and application of copper-iron alloy powder; the method has the characteristics of low raw material cost and mass production.
The technical scheme of the invention is as follows: the preparation method of the copper-iron alloy powder specifically comprises the following steps:
step one: mixing of raw materials
Mixing 50-10% of raw copper powder and 50-90% of raw iron powder according to mass percentage, and then feeding the mixture into a mixer for 3-5 hours for standby;
step two: preparation of a mixing base block
The mixing base block is prepared by pressing and specifically comprises the following steps: filling the mixed powder into a rubber sleeve, mechanically vibrating, shaking up and upsetting; pressing the treated mixed powder by adopting a cold isostatic pressing method under the pressure of 100-300 MPa to prepare a mixed material base block with the density of more than 75%;
step three: sintering
Loading the pressed material mixing base blocks into a discharge plasma sintering machine for discharge plasma sintering; wherein, the spark plasma sintering specifically comprises the following steps: the initial pressure is 200-300 MPa, and the temperature is raised to 600 ℃ at the heating rate of 10-20 ℃/s; then reducing the pressure to 90-110 MPa at a reducing speed of 10MPa/s, and preserving heat and pressure for 10-30 s; heating to 1020-1200 ℃ at a heating rate of 30 ℃/s, preserving heat and pressure for 240-270 s, and cooling to room temperature to obtain sintered agglomerates;
step four: smelting
Then loading the sintered agglomerate into a vacuum consumable arc melting furnace for melting under the condition that the current is 500-5000A to obtain a primary alloy material;
step five: atomized powder process for ingot casting
And then placing the primary alloy material into a vacuum induction furnace, completely melting the primary alloy material into a liquid state at 1500-1800 ℃, atomizing the liquid state into a water atomized alloy material through a water atomizing nozzle under the conditions of nitrogen serving as an air atomizing medium and water pressure of 130-150 MPa, and dehydrating and drying to obtain copper-iron alloy powder.
Further, the copper powder is prepared by adopting an electrolytic copper plate and atomizing the electrolytic copper plate with high-pressure water to prepare powder; the method comprises the following steps: the electrolytic copper plate is placed in an intermediate frequency furnace, after the electrolytic copper plate is completely melted into a liquid state under the condition of 1150-1200 ℃, the electrolytic copper plate is atomized into atomized copper powder through a water atomization nozzle under the condition that argon is used as an air atomization medium and the water pressure is 110-135 MPa, and then the atomized copper powder is subjected to post-treatment to obtain the raw copper powder. The copper powder prepared by water atomization has the characteristic of low energy consumption, and the process pollution is small, thereby meeting the environmental protection requirement.
Further, the post-treatment of the water atomized copper powder is sequentially oxidation, reduction, crushing and antioxidation treatment; the method comprises the following steps: oxidizing in a dynamic oxidation mode at 2000C/h, reducing for 30-45 min at 650 ℃, crushing for 45-60 min by using ball milling crushing equipment, and performing antioxidation treatment by using a corrosion inhibitor to obtain raw copper powder; the purity of the prepared raw copper powder can reach 99.8%, and the product is stable and has low oxygen content, thereby being more beneficial to the preparation of copper-iron alloy in the later period.
Further, the iron powder is prepared by adopting high-purity iron and atomizing the high-pressure water to prepare powder; the method comprises the following steps: placing high-purity iron in an intermediate frequency furnace, completely melting the high-purity iron into a liquid state at 1600-1650 ℃, atomizing the liquid state into atomized iron powder through a water atomizing nozzle under the conditions that argon is used as an air atomizing medium and the water pressure is 85-95 MPa, and then performing post-treatment on the atomized iron powder to obtain raw material iron powder; the preparation of the iron powder by water atomization has the characteristic of low energy consumption, and the process pollution is small, thereby meeting the environmental protection requirement.
Further, the water atomized iron powder is subjected to post-treatment, namely, dehydration, drying, magnetic separation, reduction annealing, screening and homogenization treatment in sequence to obtain raw material iron powder; the method has low energy consumption, and the purity of the prepared raw material iron powder can reach 99.6 percent.
Alternatively, the step two is performed by 3D printing, specifically: loading the mixed raw materials in the step one into a 3D printer, setting printing parameters, and printing in a vacuum environment to obtain a mixed material base block; the printing parameters are specifically as follows: the laser power is 800-1200W, and the scanning speed is 0.3-0.5 m/min; the manufacturing of the embryo blocks is carried out by utilizing the 3D printing technology, so that the manufacturing efficiency can be effectively increased, and the cost is indirectly reduced.
Further, the spark plasma sintering in the second step specifically comprises the following steps: the initial pressure is 200-300 MPa, and the temperature is raised to 960 ℃ at the heating rate of 10-20 ℃/s; then reducing the pressure to 80-120 MPa at a reducing speed of 20MPa/s, and preserving heat and pressure for 5-10 s; heating to 1020-1200 ℃ at a heating rate of 30 ℃/s, preserving heat and pressure for 210-240 s, and cooling to room temperature to obtain sintered agglomerates;
further, the copper-iron alloy powder prepared by the method is applied to the preparation of a germ coating for inhibiting diabetes.
Further, the copper-iron alloy powder prepared by the method is applied to the preparation of a germ covering layer for inhibiting diabetes; the copper-iron alloy powder material prepared by the invention has a good antibacterial function, and can effectively replace silver ion antibacterial materials with high cost to be widely used.
Compared with the prior art, the invention has the beneficial effects that: the manufacturing method provided by the invention has the characteristics of low energy consumption and stronger environment protection; the whole quality of the preparation method provided by the invention is easy to control, and the whole working procedure is more suitable for mass production; the invention utilizes the characteristic that copper and copper alloy can effectively inhibit the growth of viruses and bacteria, and the prepared copper-iron alloy powder has the characteristic of low cost, can effectively replace silver ion antibacterial materials with relatively high cost, and is more suitable for mass popularization.
Detailed Description
Example 1: the preparation method of the copper-iron alloy powder specifically comprises the following steps:
step one: mixing of raw materials
Raw copper powder with the purity of 99% and raw iron powder with the purity of 99% are adopted, and 10% of raw copper powder and 90% of raw iron powder are mixed according to the mass percentage and then sent into a mixer for mixing for 3 hours for standby;
step two: preparation of a mixing base block
The mixing base block is prepared by pressing and specifically comprises the following steps: filling the mixed powder into a rubber sleeve, mechanically vibrating, shaking up and upsetting; pressing the treated mixed powder by adopting a cold isostatic pressing method under the condition of the pressure of 1000MPa to prepare a mixed material base block with the density of 78%;
step three: sintering
Loading the pressed material mixing base blocks into a discharge plasma sintering machine for discharge plasma sintering; wherein, the spark plasma sintering specifically comprises the following steps: the initial pressure is 200MPa, and the temperature is raised to 600 ℃ at the heating rate of 10 ℃/s; then reducing the pressure to 90MPa at a reducing speed of 10MPa/s, and preserving heat and pressure for 10 s; heating to 1020 ℃ at a heating rate of 30 ℃/s, preserving heat and pressure for 240s, and cooling to room temperature to obtain sintered agglomerates;
step four: smelting
Then, the sintered agglomerate is put into a vacuum consumable arc melting furnace to be melted under the condition that the current is 500A, so as to obtain a primary alloy material;
step five: atomized powder process for ingot casting
And then placing the primary alloy material into a vacuum induction furnace, completely melting the primary alloy material into a liquid state at 1500 ℃, atomizing the liquid state into an atomized alloy material through a water atomizing nozzle under the conditions that nitrogen is used as an air atomizing medium and the water pressure is 130MPa, and dehydrating and drying to obtain copper-iron alloy powder.
The copper-iron alloy powder prepared by the method is applied to the germ coating layer of diabetes mellitus to inhibit the growth of viruses.
Example 2: the preparation method of the copper-iron alloy powder specifically comprises the following steps:
step one: mixing of raw materials
Raw copper powder with the purity of 99% and raw iron powder with the purity of 99% are adopted, and 30% of raw copper powder and 70% of raw iron powder are mixed according to the mass percentage and then are sent into a mixer for mixing for 4 hours for standby;
step two: preparation of a mixing base block
The mixing base block is prepared by pressing and specifically comprises the following steps: filling the mixed powder into a rubber sleeve, mechanically vibrating, shaking up and upsetting; pressing the treated mixed powder by adopting a cold isostatic pressing method under the condition of the pressure of 200MPa to prepare a mixed material base block with the density of 81 percent;
step three: sintering
Loading the pressed material mixing base blocks into a discharge plasma sintering machine for discharge plasma sintering; wherein, the spark plasma sintering specifically comprises the following steps: the initial pressure is 250MPa, and the temperature is raised to 600 ℃ at the heating rate of 15 ℃/s; then reducing the pressure to 100MPa at a reducing speed of 10MPa/s, and preserving heat and pressure for 20 s; then heating to 1100 ℃ at a heating rate of 30 ℃/s, preserving heat and pressure for 260s, and cooling to room temperature to obtain sintered agglomerates;
step four: smelting
Then loading the sintered agglomerate into a vacuum consumable arc melting furnace for melting under the condition that the current is 2000A to obtain a primary alloy material;
step five: atomized powder process for ingot casting
And then placing the primary alloy material into a vacuum induction furnace, completely melting the primary alloy material into a liquid state at 1600 ℃, atomizing the liquid state into an atomized alloy material through a water atomizing nozzle under the conditions that nitrogen is used as an air atomizing medium and the water pressure is 140MPa, and dehydrating and drying to obtain copper-iron alloy powder.
Example 3: the preparation method of the copper-iron alloy powder specifically comprises the following steps:
step one: mixing of raw materials
Raw copper powder with the purity of 99% and raw iron powder with the purity of 99% are adopted, and 50% of raw copper powder and 50% of raw iron powder are mixed according to the mass percentage and then are sent into a mixer for 5 hours for standby;
step two: preparation of a mixing base block
The mixing base block is prepared by pressing and specifically comprises the following steps: filling the mixed powder into a rubber sleeve, mechanically vibrating, shaking up and upsetting; pressing the treated mixed powder by adopting a cold isostatic pressing method under the condition of 300MPa, and preparing a mixed material base block with the density of 80%;
step three: sintering
Loading the pressed material mixing base blocks into a discharge plasma sintering machine for discharge plasma sintering; wherein, the spark plasma sintering specifically comprises the following steps: the initial pressure is 300MPa, and the temperature is raised to 600 ℃ at the heating rate of 20 ℃/s; then reducing the pressure to 110MPa at a reducing speed of 10MPa/s, and preserving heat and pressure for 30 s; then heating to 1200 ℃ at a heating rate of 30 ℃/s, preserving heat and pressure for 270s, and cooling to room temperature to obtain sintered agglomerates;
step four: smelting
Then loading the sintered agglomerates into a vacuum consumable arc melting furnace to be melted under the condition that the current is 5000A, so as to obtain a primary alloy material;
step five: atomized powder process for ingot casting
And then placing the primary alloy material into a vacuum induction furnace, completely melting the primary alloy material into a liquid state at 1800 ℃, atomizing the liquid state into a water atomized alloy material through a water atomizing nozzle under the conditions that nitrogen is used as an air atomizing medium and the water pressure is 150MPa, and dehydrating and drying to obtain copper-iron alloy powder.
Example 4: unlike example 1, the following is: step one, preparing copper powder by adopting an electrolytic copper plate through high-pressure water atomization powder preparation; the method comprises the following steps: placing an electrolytic copper plate in an intermediate frequency furnace, completely melting the electrolytic copper plate to be liquid under the condition of 1200 ℃, atomizing the electrolytic copper plate into atomized copper powder through a water atomization nozzle under the condition that argon is used as an air atomization medium and the water pressure is 125MPa, and then post-treating the atomized copper powder to obtain raw copper powder; wherein, the post-treatment of the water atomized copper powder is oxidation, reduction, crushing and antioxidation treatment in sequence; the method comprises the following steps: oxidizing in a dynamic oxidation mode at 2000C/h, reducing for 40min at 650 ℃, crushing for 50min by using ball milling crushing equipment, and performing antioxidation treatment by using a corrosion inhibitor to obtain raw copper powder. Wherein, the corrosion inhibitor is specifically DH968E, and the corrosion inhibitor with the concentration of 100%Vol is used for 20s.
Example 5: unlike example 1, the following is: the first step, preparing the iron powder by adopting high-purity iron through high-pressure water atomization powder preparation; the method comprises the following steps: placing high-purity iron in an intermediate frequency furnace, completely melting the high-purity iron into a liquid state at 1600 ℃, atomizing the liquid state into water atomized iron powder through a water atomization nozzle under the conditions that argon is used as an air atomization medium and the water pressure is 90MPa, and then performing post-treatment on the water atomized iron powder to obtain raw material iron powder; the water atomized iron powder is subjected to post-treatment, namely, dehydration, drying, magnetic separation, reduction annealing, screening and homogenization treatment in sequence to obtain raw material iron powder.
Example 6: unlike example 1, the following is: step two, preparing the mixing base block through 3D printing, wherein the mixing base block comprises the following concrete steps: loading the mixed raw materials in the step one into a 3D printer, setting printing parameters, and printing in a vacuum environment to obtain a mixed material base block; the printing parameters are specifically as follows: the laser power was 1000W and the scanning speed was 0.5m/min.
Example 7: unlike example 1, the following is: the spark plasma sintering specifically comprises the following steps: the initial pressure is 300MPa, and the temperature is raised to 960 ℃ at a heating rate of 20 ℃/s; then reducing the pressure to 80MPa at a reducing speed of 20MPa/s, and preserving heat and pressure for 10 s; and then heating to 1200 ℃ at a heating rate of 30 ℃/s, preserving heat and pressure for 210s, and cooling to room temperature to obtain the sintering agglomeration.
Experimental example: 90 diabetic foot patients who were at a hospital visit during 1 month of 2019 to 2 months of 2020 were randomly extracted and classified into 9 groups of conventional dressing, silver ion antibacterial material and copper-iron alloy powder material prepared in examples 1 to 7 of the present invention according to treatment methods, each group containing 10 patients. Wherein, traditional dressing adopts hydrogen peroxide solution and normal saline to lap and clear up the wound.
The wound recovery effect of each group of patients was observed (the effects were divided into 1, basic recovery: recovery of skin color of patient and almost no clinical symptoms, 2, remarkable effect: significant change of skin color of patient and significant decrease of clinical symptoms, 3, remission of effect: slight improvement of skin color of patient and healing signs of wound, 4, controlled effect: failure of the above criteria and no worsening signs of clinical symptoms, 5, no worsening signs of clinical symptoms) as follows:
in conclusion, the copper-iron alloy powder material prepared by the invention can play a positive influence on diabetics in clinic, and can be used as a silver ion antibacterial material with higher cost.
Claims (1)
1. The application of copper-iron alloy powder in preparing germ coating for inhibiting diabetes and coating for inhibiting virus growth is characterized by comprising the following steps:
the preparation method of the copper-iron alloy powder comprises the following steps:
step one: mixing of raw materials
Mixing 10% of raw copper powder and 90% of raw iron powder according to mass percentage, and then feeding the mixture into a mixer for 3-5 hours for standby;
the copper powder is prepared by adopting an electrolytic copper plate and atomizing the electrolytic copper plate by high-pressure water to prepare powder; the method comprises the following steps: placing the electrolytic copper plate in an intermediate frequency furnace, completely melting the electrolytic copper plate into a liquid state at 1150-1200 ℃, atomizing the electrolytic copper plate into water atomized copper powder through a water atomization nozzle under the conditions that argon is used as an air atomization medium and the water pressure is 110-135 MPa, and then post-treating the water atomized copper powder to obtain raw material copper powder; the post-treatment of the water atomized copper powder is sequentially oxidation, reduction, crushing and antioxidation treatment; the method comprises the following steps: oxidizing in a dynamic oxidation mode at 2000C/h, reducing for 30-45 min at 650 ℃, crushing for 45-60 min by using ball milling crushing equipment, and performing antioxidation treatment by using a corrosion inhibitor to obtain raw copper powder;
the iron powder is prepared by adopting high-purity iron and atomizing the high-pressure water to prepare powder; the method comprises the following steps: placing high-purity iron in an intermediate frequency furnace, completely melting the high-purity iron into a liquid state at 1600-1650 ℃, atomizing the high-purity iron into atomized iron powder through a water atomizing nozzle under the conditions that argon is used as an air atomizing medium and the water pressure is 85-95 MPa, and then performing post-treatment on the atomized iron powder to obtain raw material iron powder; the water atomized iron powder is subjected to post-treatment, namely, dehydration, drying, magnetic separation, reduction annealing, screening and homogenization treatment in sequence to obtain raw material iron powder;
step two: preparation of a mixing base block
The compounding basic block is prepared through 3D printing, specifically: loading the mixed raw materials in the step one into a 3D printer, setting printing parameters, and printing in a vacuum environment to obtain a mixed material base block; the printing parameters are specifically as follows: the laser power is 800-1200W, and the scanning speed is 0.3-0.5 m/min;
step three: sintering
Loading the pressed material mixing base blocks into a discharge plasma sintering machine for discharge plasma sintering; wherein, the spark plasma sintering specifically comprises the following steps: the initial pressure is 200-300 MPa, and the temperature is raised to 600 ℃ at a heating rate of 10-20 ℃/s; then reducing the pressure to 90-110 MPa at a reducing speed of 10MPa/s, and preserving heat and pressure for 10-30 s; heating to 1020-1200 ℃ at a heating rate of 30 ℃/s, preserving heat and pressure for 240-270 seconds, and cooling to room temperature to obtain sintered agglomerates;
step four: smelting
Then, loading the sintered agglomerates into a vacuum consumable arc melting furnace, and melting under the condition that the current is 500-5000A to obtain a primary alloy material;
step five: atomized powder process for ingot casting
Then placing the primary alloy material into a vacuum induction furnace, completely melting the primary alloy material into a liquid state at 1500-1800 ℃, atomizing the liquid state into a water atomized alloy material through a water atomizing nozzle under the conditions that nitrogen is used as an air atomizing medium and the water pressure is 130-150 MPa, and dehydrating and drying to obtain copper-iron alloy powder;
the copper-iron alloy powder prepared by the method is applied to the preparation of a germ covering layer for inhibiting diabetes;
the copper-iron alloy powder prepared by the method is applied to the preparation of a coating for inhibiting virus growth.
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