CN111719087B - Preparation method of medical CuFe alloy powder - Google Patents
Preparation method of medical CuFe alloy powder Download PDFInfo
- Publication number
- CN111719087B CN111719087B CN202010427015.1A CN202010427015A CN111719087B CN 111719087 B CN111719087 B CN 111719087B CN 202010427015 A CN202010427015 A CN 202010427015A CN 111719087 B CN111719087 B CN 111719087B
- Authority
- CN
- China
- Prior art keywords
- alloy powder
- powder
- cooling
- cufe
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
-
- 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
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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
-
- 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
-
- 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
- A61P31/10—Antimycotics
-
- 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]
-
- 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
-
- 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
-
- 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
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- 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%
-
- 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
- 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
-
- 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
- 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
-
- 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
- B22F2009/0832—Handling of atomising fluid, e.g. heating, cooling, cleaning, recirculating
-
- 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
- B22F2009/0848—Melting process before atomisation
-
- 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
- B22F2009/086—Cooling after atomisation
- B22F2009/0876—Cooling after atomisation by gas
Abstract
The invention discloses a preparation method of medical CuFe alloy powder, which comprises the following steps: mixing S1 materials: selecting Cu 10-50% and the balance of Fe, and then mixing to obtain mixed powder; s2 pressing: loading the mixed powder into a rubber sleeve, mechanically vibrating, shaking evenly, upsetting materials, and pressing the processed mixed powder by a cold isostatic pressing method to obtain a consumable electrode; s3 sintering: loading the consumable electrode into a vacuum sintering furnace for sintering; s4 smelting: putting the sintered consumable electrode into a vacuum consumable arc melting furnace for melting; s5 atomizing to prepare powder: and smelting the CuFe alloy material in a vacuum induction furnace again to obtain alloy liquid, injecting the alloy liquid into a tundish for atomization treatment, and then carrying out combined cooling to obtain CuFe alloy powder. The CuFe alloy powder prepared by the invention has uniform tissue components, does not have macroscopic and microscopic defects such as Cu and Fe enrichment and the like, and can be used for a germ covering layer of diabetes and the like.
Description
Technical Field
The invention relates to the technical field of alloy materials, in particular to a preparation method of medical CuFe alloy powder.
Background
The copper-iron alloy has excellent heat conductivity and bending resistance, and has very excellent magnetism and electromagnetic shielding performance when the iron content is more than 30%, and also has excellent characteristics of low thermal expansion coefficient, wear resistance, sterilization performance and the like.
According to analysis, the CuFe alloy product has huge application background, such as CuFe alloy rods, bars, wires and wires which can be used for electromagnetic shielding wires, high-fidelity audio wires, electromagnetic shielding wires for high-speed motors of unmanned aerial vehicles, high-voltage cables, robot communication control wires, radio frequency wires and the like; the CuFe alloy powder can be used for brake pads, wave-absorbing shielding coatings, 3D printing, medical antibacterial aspects and the like.
Through production practice and summary, the non-vacuum melting process can be adopted for 5-10% of the iron content, and the vacuum melting process is adopted for more than 10% of the iron content; the key process of preparing the CuFe alloy powder is the smelting and powder-making process, and the purposes of preparing the CuFe alloy powder and ensuring the processing and performance of the material are to maintain high purity, high uniformity, high consistency and low cost.
Therefore, a method for preparing the CuFe alloy powder is needed to meet the above-mentioned objectives, so as to promote the application and development of the CuFe alloy powder.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of medical CuFe alloy powder.
The technical scheme of the invention is as follows: a preparation method of medical CuFe alloy powder comprises the following steps:
mixing S1 materials: selecting Cu 10-50% and the balance of Fe, and then mixing to obtain mixed powder;
s2 pressing: loading the mixed powder into a rubber sleeve, mechanically vibrating, shaking evenly, upsetting materials, and pressing the processed mixed powder by a cold isostatic pressing method to obtain a consumable electrode;
s3 sintering: loading the consumable electrode into a vacuum sintering furnace for sintering;
s4 smelting: putting the sintered consumable electrode into a vacuum consumable arc melting furnace for melting;
s5 atomizing to prepare powder: and smelting the CuFe alloy material in a vacuum induction furnace again to obtain alloy liquid, injecting the alloy liquid into a tundish for atomization treatment, and then carrying out combined cooling to obtain CuFe alloy powder.
The preparation method adopts mixed powder pressing and sintering to prepare the CuFe alloy and adopts atomization powder preparation to prepare the CuFe alloy powder, the prepared alloy powder has low gas content, less inclusions, uniform tissue components and no macroscopic and microscopic defects such as Cu and Fe enrichment and the like, can be well applied to a germ covering layer of diabetes to inhibit virus growth, and has good application prospect.
Further, the mixing time in the step S1 is 3-5 h. Under this time quantum can make Cu, Fe powder reach the misce bene effect in the blendor, avoid the mixing time to cause the compounding inequality short, the time overlength causes the equipment power consumption.
Further, the pressure of the cold isostatic pressing method in the step S2 is 100-300 MPa, so that the compactness of the consumable electrode pressed is more than 75%. The mixed powder can be effectively pressed and formed by carrying out cold isostatic pressing on the mixed powder within the pressure range, the density of the mixed powder is controlled to reach more than 75%, contact stress can be rapidly eliminated between Cu and Fe powder particles, the bonded metal powder begins to recover and recrystallize, the subsequent sintering and smelting effect can be enhanced, the use performance of the CuFe alloy is improved, if the density does not reach 75%, the subsequent sintering is insufficient, the composition is not uniform, and the like, so that the use effect of the subsequently prepared CuFe alloy powder is poor or fails.
Further, in the step S3, the maximum sintering temperature is controlled to be 900-1050 ℃, the heat preservation time is 50-200 min, and the vacuum degree is less than 10-2pa. The sintering temperature is controlled within the range, so that the CuFe alloy can be fully sintered to form the basic structure and structure of the alloy so as to obtain the CuFe alloy with high performance, and the heat preservation time is controlled within the range so as to improve the mechanical property of the alloy.
Further, the melting current of the vacuum consumable electrode arc melting furnace in the step S4 is 500-5000A, and the melting temperature of the vacuum induction furnace in the step S5 is 1500-1800 ℃. The alloy is smelted by the smelting current and the temperature of the vacuum induction furnace, the smelting current and the smelting temperature meet the smelting requirement of the CuFe alloy, the requirement on smelting equipment is low, and the applicability of the equipment used by the alloy is high.
As an embodiment of the present invention, the atomization process in step S5 is specifically a water atomization process. The water atomization treatment is specifically carried out on alloy liquid through high-speed water flow formed by composite aqueous solution, wherein the composite aqueous solution is distilled water containing 3.5-5.8% of strengthening liquid by mass concentration, the water atomization water pressure is 7.5-8.5 MPa, and the water atomization water temperature is 68-75 ℃;
the combined cooling is to cool the temperature to 350-450 ℃ by air cooling and then cool the temperature to room temperature by fog cooling, wherein the air cooling speed is 5-7 m/s, the fog cooling spraying pressure is 4-7 MPa, and the fog cooling agent is distilled water.
The water atomization treatment is adopted, the heat capacity is large, the chilling degree of the CuFe alloy powder is high, the solidification time of the alloy liquid is short under the chilling action of atomized fine alloy liquid drops, and compared with the gas atomization treatment, the atomization treatment of the alloy liquid is carried out under the water atomization treatment parameters, the prepared CuFe alloy powder is mostly approximate to spherical alloy powder, but the use influence is small, and the operation cost of the operation is low compared with the operation cost of the gas atomization treatment; and the formed alloy powder is subjected to combined cooling of air cooling and mist cooling in a combined cooling mode, and the physical properties of the formed alloy powder are improved in different cooling treatment processes, so that the CuFe alloy powder with better properties is obtained.
As another technical solution of the present invention, the atomization process in step S5 is specifically an air atomization process. The gas atomization treatment is specifically carried out on the alloy liquid by adopting high-speed airflow formed by inert gas, wherein the gas atomization pressure is 1.5-2.5 MPa, and the inert gas is one of helium and argon, but not limited to the two;
the combined cooling is to cool the temperature to 280-370 ℃ by mist cooling and then cool the temperature to room temperature by air cooling, wherein the air cooling wind speed is 3-5 m/s, the mist cooling spraying pressure is reduced from 6-9 MPa to 1100-1300 ℃, then the spraying pressure is adjusted to 1.5-2 MPa at the speed of 0.1MPa/min, the mist cooling agent is a composite water solution, the using temperature is 23-35 ℃, and the composite water solution is distilled water containing 1.5-2.5% of strengthening liquid by mass concentration.
The gas atomization treatment is adopted, the chilling degree of the CuFe alloy powder is low due to the small heat capacity of the alloy powder, the alloy liquid atomized into fine liquid drops cannot be solidified immediately, the atomization treatment of the alloy liquid is carried out under the water atomization treatment parameters relative to the gas atomization treatment, the prepared CuFe alloy powder is mostly spherical alloy powder, the CuFe alloy powder has relatively better service performance and the like when being applied to a germ covering layer of diabetes, but the operation cost of the CuFe alloy powder is higher relative to the operation cost of the water atomization treatment; the formed alloy powder is subjected to mist cooling and air cooling combined cooling in a combined cooling mode, the characteristic of small heat capacity of gas atomization treatment is utilized to assist the composite aqueous solution in mist cooling treatment, so that the treatment and function effects similar to those of the composite aqueous solution used in water atomization are achieved, and the physical properties are improved through different cooling treatment processes, so that the CuFe alloy powder with better performance is obtained.
Further, the strengthening liquid in the composite aqueous solution comprises the following components in parts by mass: 20-35 parts of sodium polyacrylate, 5-9 parts of sodium chloride, 0.5-1 part of phenoxyethanol, 2-3 parts of maleic acid and 120-150 parts of water. By using the composite aqueous solution in the water atomization treatment and the gas atomization treatment, the prepared CuFe alloy powder can be reinforced by the reinforcing solution prepared according to the proportion, so that macroscopic and microscopic defects of the CuFe alloy powder are further optimized, the performance of the CuFe alloy powder is improved, the application effect of the CuFe alloy powder on pathogenic bacteria covering layers of diabetes and the like is enhanced, and the use effect of the CuFe alloy powder is optimized.
Furthermore, the preparation method of the strengthening liquid in the composite aqueous solution comprises the following steps: selecting sodium polyacrylate, sodium chloride, phenoxyethanol, maleic acid and water according to a proportion for later use, mixing the sodium polyacrylate, the sodium chloride and the water, heating to 37 +/-5 ℃, then dropwise adding the maleic acid, ultrasonically mixing, then cooling at a speed of 3 ℃/min, dropwise adding phenoxyethanol during temperature-controlled cooling, and continuously stirring until the temperature of the strengthening solution is reduced to room temperature to obtain the strengthening solution.
The invention has the beneficial effects that:
(1) the CuFe alloy powder prepared by the preparation method has the advantages of low gas content, less inclusions, uniform tissue components, no macroscopic and microscopic defects such as Cu and Fe enrichment and the like, and good mechanical properties.
(2) The CuFe alloy powder prepared by the preparation method has huge application background, can be used for the germ covering layer of diabetes and the like, is about to inhibit virus growth, and has wide application prospect.
Drawings
FIG. 1 is the antibacterial curve of CuFe alloy powder of the present invention in example 2 and the control group.
Detailed Description
Example 1
A preparation method of medical CuFe alloy powder comprises the following steps:
mixing S1 materials: selecting 35% of Cu and the balance of Fe, and then mixing in a mixer for 4 hours to obtain mixed powder;
s2 pressing: loading the mixed powder into a rubber sleeve, mechanically vibrating, shaking evenly, upsetting materials, pressing the processed mixed powder by a cold isostatic pressing method, wherein the pressure is 230MPa, and the density reaches 80%, so as to obtain a consumable electrode;
s3 sintering: charging consumable electrode into a vacuum sintering furnaceSintering at 900-1050 deg.C for 175min, and vacuum degree less than 10-2pa；
S4 smelting: putting the sintered consumable electrode into a vacuum consumable arc melting furnace for melting, wherein the melting current is 3500A;
s5 atomizing to prepare powder: smelting the CuFe alloy material again in a vacuum induction furnace at the smelting temperature of 1700 ℃ to obtain alloy liquid with qualified components, then injecting the alloy liquid into a tundish above an atomizing nozzle, wherein the alloy liquid flows out from a hole at the bottom of the tundish, meets high-speed water flow formed by a composite aqueous solution when passing through the nozzle and is atomized into fine droplets, and then cooling the atomized droplets in an atomizing cylinder by air cooling to 390 ℃ and then cooling to room temperature by fog cooling to obtain CuFe alloy powder, wherein Fe phase particles reach the nanoscale; wherein the air cooling wind speed is 6m/s, the fog cooling spraying pressure is 5MPa, and the fog cooling agent adopts distilled water;
wherein the composite aqueous solution is distilled water containing 3.5-5.8% of strengthening liquid by mass concentration, the water atomization water pressure is 7.5-8.5 MPa, the water atomization water temperature is 68-75 ℃, and the strengthening liquid in the composite aqueous solution comprises the following components in parts by mass: 31 parts of sodium polyacrylate, 7 parts of sodium chloride, 0.7 part of phenoxyethanol, 2.6 parts of maleic acid and 135 parts of water.
The preparation method of the strengthening solution in the composite aqueous solution comprises the following steps: selecting sodium polyacrylate, sodium chloride, phenoxyethanol, maleic acid and water according to a proportion for later use, mixing the sodium polyacrylate, the sodium chloride and the water, heating to 37 +/-5 ℃, then dropwise adding the maleic acid, ultrasonically mixing, cooling at a speed of 3 ℃/min, dropwise adding phenoxyethanol during temperature-controlled cooling, continuously stirring until the temperature of the strengthening solution is reduced to room temperature to obtain a strengthening solution, heating distilled water to the use temperature, slowly adding the strengthening solution, and continuously stirring to obtain a composite aqueous solution.
The preparation method adopts mixed powder pressing and sintering to prepare the CuFe alloy and adopts atomization powder preparation to prepare the CuFe alloy powder, the prepared alloy powder has low gas content, less inclusions, uniform tissue components and no macroscopic and microscopic defects such as Cu and Fe enrichment, can be well applied to the germ covering layer of diabetes to inhibit the growth of viruses, and has good application prospect. The water atomization treatment is adopted, the heat capacity is large, the chilling degree of the CuFe alloy powder is high, the solidification time of the alloy liquid is short under the chilling action of atomized fine alloy liquid drops, and compared with the gas atomization treatment, the atomization treatment of the alloy liquid is carried out under the water atomization treatment parameters, the prepared CuFe alloy powder is mostly approximate to spherical alloy powder, but the use influence is small, and the operation cost of the operation is low compared with the operation cost of the gas atomization treatment; and the formed alloy powder is subjected to combined cooling of air cooling and mist cooling in a combined cooling mode, and the physical properties of the formed alloy powder are improved in different cooling treatment processes, so that the CuFe alloy powder with better properties is obtained.
Example 2
A preparation method of medical CuFe alloy powder comprises the following steps:
mixing S1 materials: selecting 35% of Cu and the balance of Fe, and then mixing in a mixer for 4 hours to obtain mixed powder;
s2 pressing: loading the mixed powder into a rubber sleeve, mechanically vibrating, shaking evenly, upsetting materials, pressing the processed mixed powder by a cold isostatic pressing method, wherein the pressure is 230MPa, and the density reaches 80%, so as to obtain a consumable electrode;
s3 sintering: loading the consumable electrode into a vacuum sintering furnace for sintering, controlling the sintering maximum temperature to be 900-1050 ℃, keeping the temperature for 175min, and controlling the vacuum degree to be less than 10-2pa；
S4 smelting: putting the sintered consumable electrode into a vacuum consumable arc melting furnace for melting, wherein the melting current is 3500A;
s5 atomizing to prepare powder: smelting the CuFe alloy material in a vacuum induction furnace again at the smelting temperature of 1700 ℃ to obtain alloy liquid with qualified components, injecting the alloy liquid into a tundish above an atomizing nozzle, enabling the alloy liquid to flow out of a hole at the bottom of the tundish, meeting high-speed airflow formed by the alloy liquid and argon when passing through the nozzle, atomizing the alloy liquid into fine droplets, cooling the atomized droplets in an atomizing cylinder to 280-370 ℃ by mist cooling, and cooling the atomized droplets to room temperature by air cooling to obtain CuFe alloy powder, wherein Fe phase particles reach the nanoscale; wherein the air cooling wind speed is 4m/s, the spray pressure of fog cooling is reduced from initial 8MPa to 1200 ℃, then the spray pressure is adjusted to 1.8MPa at the speed of 0.1MPa/min, the fog cooling agent adopts a composite aqueous solution, the using temperature is 32 ℃, and the composite aqueous solution is distilled water containing strengthening liquid with the mass concentration of 2.3%;
wherein the gas atomization air pressure is 2.2MPa, and the strengthening liquid in the composite aqueous solution comprises the following components in parts by mass: 31 parts of sodium polyacrylate, 7 parts of sodium chloride, 0.7 part of phenoxyethanol, 2.6 parts of maleic acid and 135 parts of water.
The preparation method of the strengthening solution in the composite aqueous solution comprises the following steps: selecting sodium polyacrylate, sodium chloride, phenoxyethanol, maleic acid and water according to a proportion for later use, mixing the sodium polyacrylate, the sodium chloride and the water, heating to 39 ℃, then dropwise adding the maleic acid, ultrasonically mixing, cooling at a speed of 3 ℃/min, dropwise adding phenoxyethanol during the temperature-controlled cooling period, continuously stirring until the strengthening solution is cooled to room temperature to obtain strengthening solution, heating distilled water to the use temperature, slowly adding the strengthening solution, and continuously stirring to obtain the composite aqueous solution.
The preparation method adopts mixed powder pressing and sintering to prepare the CuFe alloy and adopts atomization powder preparation to prepare the CuFe alloy powder, the prepared alloy powder has low gas content, less inclusions, uniform tissue components and no macroscopic and microscopic defects such as Cu and Fe enrichment, can be well applied to the germ covering layer of diabetes to inhibit the growth of viruses, and has good application prospect. The gas atomization treatment is adopted, the chilling degree of the CuFe alloy powder is low due to the small heat capacity of the alloy powder, the alloy liquid atomized into fine liquid drops cannot be solidified immediately, the atomization treatment of the alloy liquid is carried out under the water atomization treatment parameters relative to the gas atomization treatment, the prepared CuFe alloy powder is mostly spherical alloy powder, the CuFe alloy powder has relatively better service performance and the like when being applied to a germ covering layer of diabetes, but the operation cost of the CuFe alloy powder is higher relative to the operation cost of the water atomization treatment; the formed alloy powder is subjected to mist cooling and air cooling combined cooling in a combined cooling mode, the characteristic of small heat capacity of gas atomization treatment is utilized to assist the composite aqueous solution in mist cooling treatment, so that the treatment and function effects similar to those of the composite aqueous solution used in water atomization are achieved, and the physical properties are improved through different cooling treatment processes, so that the CuFe alloy powder with better performance is obtained.
Since the preparation cost of example 2 is higher than that of example 1, but the overall performance is relatively better than the performance of the water atomization treatment of example 1, the difference of the manufacturing cost is not studied at all, and the subsequent detailed description studies the influence of different parameters and proportions on the performance of the CuFe alloy powder based on example 2.
Example 3
The present embodiment is substantially the same as embodiment 2, except that in step S1, the material mixture ratio is 10% Cu, and the balance is Fe.
Example 4
The present embodiment is substantially the same as embodiment 2, except that the material mixing ratio in step S1 is different, Cu 50% is selected, and the balance is Fe.
Example 5
This example is substantially the same as example 2, except that the cooling parameters in step S5 are different, the air cooling speed is 3m/S, the spray pressure of the mist cooling is reduced from the initial 6MPa to 1100 ℃, and then the spray pressure is adjusted to 1.5MPa at a rate of 0.1MPa/min, the mist cooling agent is a composite aqueous solution, the use temperature is 32 ℃, and the composite aqueous solution is distilled water containing 2.3% by mass of the strengthening solution.
Example 6
This example is substantially the same as example 2, except that the cooling parameters in step S5 are different, the air cooling speed is 5m/S, the spray pressure of the mist cooling is reduced from 9MPa to 1300 ℃, the spray pressure is adjusted to 2MPa at a rate of 0.1MPa/min, the mist cooling agent is a composite aqueous solution, the use temperature is 32 ℃, and the composite aqueous solution is distilled water containing 2.3% by mass of the strengthening solution.
Example 7
This example is substantially the same as example 2, except that the cooling parameters in step S5 are different, the air cooling speed is 4m/S, the spray pressure of the mist cooling is reduced from the initial 8MPa to 1200 ℃, the spray pressure is adjusted to 1.8MPa at the rate of 0.1MPa/min, the mist cooling agent is a composite aqueous solution, the use temperature is 23 ℃, and the composite aqueous solution is distilled water containing 1.5% by mass of the strengthening solution.
Example 8
This example is substantially the same as example 2, except that the cooling parameters in step S5 are different, the air cooling speed is 4m/S, the spray pressure of the mist cooling is reduced from the initial 8MPa to 1200 ℃, the spray pressure is adjusted to 1.8MPa at the rate of 0.1MPa/min, the mist cooling agent is a composite aqueous solution, the use temperature is 35 ℃, and the composite aqueous solution is distilled water containing 2.5% by mass of the strengthening solution.
Example 9
This example is substantially the same as example 2, except that the compounding ratio of the components of the reinforcing liquid in the aqueous composite solution in step S5 is different, and the reinforcing liquid in the aqueous composite solution is: 20 parts of sodium polyacrylate, 5 parts of sodium chloride, 0.5 part of phenoxyethanol, 2 parts of maleic acid and 120 parts of water.
Example 10
This example is substantially the same as example 2, except that the compounding ratio of the components of the reinforcing liquid in the aqueous composite solution in step S5 is different, and the reinforcing liquid in the aqueous composite solution is: 35 parts of sodium polyacrylate, 9 parts of sodium chloride, 1 part of phenoxyethanol, 3 parts of maleic acid and 150 parts of water.
Comparative experiment of performance of CuFe alloy powder in each embodiment
CuFe alloy powders were prepared according to the above examples 1-10, and the parameters were measured, specifically as follows:
spherical ratio of CuFe alloy powder
Scanning electron microscope magnifying imaging and displaying on a computer, directly observing the particle morphology, measuring the size of the powder particles by using a scanning imaging method, respectively measuring the long axis and the short axis of the particles, wherein the particles with the ratio of the long axis to the short axis being less than or equal to 1.2 can be regarded as spherical, and obtaining the sphericity ratio of the powder through statistics and calculation, wherein the specific table is shown in the following table 1;
TABLE 1 sphericity fraction of CuFe alloy powder prepared in each example
And (4) experimental conclusion:
1) in comparative example 2, examples 3 to 4 and examples 7 to 10, the deviation of the sphericity ratio was within ± 0.3%, that is, the sphericity ratios were substantially the same, and it was found that the ratio of the Cu and Fe components, the mass concentration of the strengthening liquid in the composite aqueous solution, and the component ratio of the strengthening liquid had no effect on the sphericity ratio of the CuFe alloy powder prepared;
2) compared with the embodiment 1, the sphericity ratio of the CuFe alloy powder in the embodiment 2 is greatly different, mainly because the water atomization treatment is adopted, the heat capacity is large, the chilling degree of the CuFe alloy powder is high, the solidification time of the alloy liquid is short under the chilling action of atomized fine alloy liquid drops, compared with the gas atomization treatment, the prepared CuFe alloy powder is mostly approximate to spherical alloy powder, and the deviation between the sphericity ratio and the gas atomization is large;
3) in comparison with examples 5-6, the sphericity ratio of example 2 differs somewhat, and it can be seen that the sphericity ratio of the CuFe alloy powder is affected somewhat under different combined cooling parameters, wherein the sphericity ratio of the alloy powder prepared with the cooling parameters in example 2 is optimal.
Antibacterial property of CuFe alloy powder
The diabetes germ covering layers of all the embodiments are prepared by the same amount of alloy powder, antibacterial performance of each alloy powder is measured and evaluated according to QB/T2591-2003 antibacterial plastic-antibacterial performance test method and antibacterial effect, and the alloy powder is divided into 4 stages (the first stage is less than or equal to 1 day, the second stage is 1-3 days, the third stage is 4-6 days, the fourth stage is more than or equal to 7 days), and the antibacterial performance of each stage is measured and evaluated;
TABLE 2 antibacterial ratio of CuFe alloy powder prepared in each example
And (4) experimental conclusion:
1) compared with the examples 5-6, the antibacterial rate of each stage of the method has no obvious difference, and the combined cooling parameter (namely the spherical rate of the CuFe alloy powder) has no influence on the antibacterial rate in view of certain contingency and errors of measurement, namely the antibacterial rate is basically the same;
2) compared with the example 1, the antibacterial rates of the comparative example 2 and the example 1 in all stages have no obvious difference, and in view of certain contingencies and errors in measurement, namely the antibacterial rates are basically the same, but the antibacterial rates of the examples 5 to 6 with smaller spherical differences are 99% in the first stage, while the antibacterial rate of the example 1 with larger spherical differences is 98%, so that the antibacterial rates of the examples 1 and 2 with larger spherical differences have slight influence but smaller influence, and the preparation method of the examples 1 and 2 can be preferably used according to the requirements of specific production cost;
3) compared with the examples 3-4 and 7-10, the antibacterial rate of the CuFe alloy powder prepared in each stage is obviously different, the antibacterial rate of the CuFe alloy powder prepared in each stage is influenced by different Cu and Fe component proportions, different mass concentrations of the strengthening liquid and the component proportion ratio of the strengthening liquid, wherein the antibacterial rate of the CuFe alloy powder is influenced most by the component proportion of the strengthening liquid, the antibacterial rate of the CuFe alloy powder prepared by the component proportion of the strengthening liquid is influenced less by the different mass concentrations of the strengthening liquid, and the antibacterial rate of the CuFe alloy powder prepared by the component proportion of the Cu and Fe, the mass concentration of the strengthening liquid and the component proportion of the strengthening liquid in the example 2 is optimized;
in order to further study the effect of the CuFe alloy powder prepared by the preparation method of the invention applied to the diabetes germ covering layer, the same mixing, pressing, sintering and smelting parameters are adopted, the combined cooling process is removed, atomization powder preparation is carried out under the same gas atomization air pressure and argon gas, the obtained product is taken as a comparison group, the antibacterial rate of each stage is obtained according to the method, the antibacterial curve is drawn by selecting the data of the embodiment 2 and the comparison group, as shown in figure 1,
as can be seen from the figure, the antibacterial rate of the alloy powder of the embodiment 2 is obviously superior to that of the CuFe alloy powder in the conventional preparation process at each stage, and the antibacterial rate of the alloy powder of the embodiment 2 decreases slowly with the passage of time, while the antibacterial rate of the comparative example starts to decrease more rapidly after about 4 days, so that the antibacterial performance and stability of the CuFe alloy powder are obviously enhanced and improved by applying the composite aqueous solution containing the strengthening solution with a certain mass concentration by using the combined cooling process.
Claims (5)
1. A preparation method of medical CuFe alloy powder is characterized by comprising the following steps:
mixing S1 materials: selecting Cu 10-50% and the balance of Fe, and then mixing to obtain mixed powder;
s2 pressing: loading the mixed powder into a rubber sleeve, mechanically vibrating, shaking evenly, upsetting materials, and pressing the processed mixed powder by a cold isostatic pressing method to obtain a consumable electrode;
s3 sintering: loading the consumable electrode into a vacuum sintering furnace for sintering;
s4 smelting: putting the sintered consumable electrode into a vacuum consumable arc melting furnace for melting;
s5 atomizing to prepare powder: smelting the CuFe alloy material again in a vacuum induction furnace to obtain alloy liquid, injecting the alloy liquid into a tundish for atomization treatment, and then carrying out combined cooling to obtain CuFe alloy powder, wherein the atomization treatment is water atomization treatment or gas atomization treatment;
the water atomization treatment is specifically carried out on alloy liquid through high-speed water flow formed by composite aqueous solution, wherein the composite aqueous solution is distilled water containing 3.5-5.8% of strengthening liquid by mass concentration, the water atomization water pressure is 7.5-8.5 MPa, and the water atomization water temperature is 68-75 ℃; the combined cooling is to cool the temperature to 350-450 ℃ by air cooling and then cool the temperature to room temperature by fog cooling, wherein the air cooling speed is 5-7 m/s, the fog cooling spraying pressure is 4-7 MPa, and the fog cooling agent is distilled water;
the gas atomization treatment is specifically carried out on the alloy liquid by adopting high-speed gas flow formed by inert gas, wherein the gas atomization pressure is 1.5-2.5 MPa; the combined cooling is to cool the temperature to 280-370 ℃ by fog cooling and cool the temperature to room temperature by air cooling, wherein the air cooling wind speed is 3-5 m/s, the spraying pressure of the fog cooling is reduced from the initial 6-9 MPa to 1100-1300 ℃, then the spraying pressure is adjusted to 1.5-2 MPa at the speed of 0.1MPa/min, the fog cooling agent is a composite aqueous solution, and the use temperature is 23-35 ℃;
the composite water solution is distilled water containing 1.5-2.5% of reinforcing liquid by mass concentration, and the reinforcing liquid in the composite water solution comprises the following components in parts by mass: 20-35 parts of sodium polyacrylate, 5-9 parts of sodium chloride, 0.5-1 part of phenoxyethanol, 2-3 parts of maleic acid and 120-150 parts of water.
2. The method for preparing CuFe alloy powder for medical use according to claim 1, wherein the mixing time in step S1 is 3-5 h.
3. The method for preparing CuFe alloy powder for medical use according to claim 1, wherein the pressure of cold isostatic pressing in step S2 is 100-300 MPa, so that the compaction of the consumable electrode is more than 75%.
4. The method for preparing CuFe alloy powder for medical use according to claim 1, wherein in step S3, the maximum sintering temperature is controlled to 900-1050 ℃, the heat preservation time is 50-200 min, and the vacuum degree is less than 10-2pa。
5. The method for preparing CuFe alloy powder for medical use according to claim 1, wherein a melting current of the consumable vacuum arc melting furnace in step S4 is 500-5000A, and a melting temperature of the induction vacuum furnace in step S5 is 1500-1800 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010427015.1A CN111719087B (en) | 2020-05-19 | 2020-05-19 | Preparation method of medical CuFe alloy powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010427015.1A CN111719087B (en) | 2020-05-19 | 2020-05-19 | Preparation method of medical CuFe alloy powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111719087A CN111719087A (en) | 2020-09-29 |
| CN111719087B true CN111719087B (en) | 2021-06-01 |
Family
ID=72564724
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010427015.1A Active CN111719087B (en) | 2020-05-19 | 2020-05-19 | Preparation method of medical CuFe alloy powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111719087B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112387978B (en) * | 2020-10-21 | 2023-03-14 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of CuFe alloy powder for brake pad |
| CN113278830A (en) * | 2021-04-28 | 2021-08-20 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of high-uniformity copper-iron alloy |
| CN113414398A (en) * | 2021-06-21 | 2021-09-21 | 江苏天楹等离子体科技有限公司 | Equipment and method for preparing metal powder by using plasma |
| CN113510245B (en) * | 2021-09-14 | 2021-12-07 | 陕西斯瑞新材料股份有限公司 | Method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization |
| CN114686747B (en) * | 2022-02-15 | 2022-11-25 | 陕西斯瑞新材料股份有限公司 | Method for preparing copper stainless steel in-situ composite material by adopting vacuum consumable arc melting |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103658668A (en) * | 2013-12-06 | 2014-03-26 | 湖北鄂信钻石材料有限责任公司 | Method for preparing iron-based prealloy powder |
| CN103862190A (en) * | 2012-12-17 | 2014-06-18 | 北京有色金属研究总院 | Novel cathode high-temperature brazing material and preparation method thereof |
| CN108796304A (en) * | 2018-06-22 | 2018-11-13 | 江苏钛坦新材料有限公司 | A kind of γ-TiAl prealloys gas-atomized powder electrode bar and preparation method thereof |
| CN109055801A (en) * | 2018-07-31 | 2018-12-21 | 陕西斯瑞新材料股份有限公司 | A kind of preparation method using vacuum consumable arc-melting CuFe alloy material |
| CN109351982A (en) * | 2018-11-21 | 2019-02-19 | 陕西斯瑞新材料股份有限公司 | A kind of continuous production chromiumcopper milling method |
| CN109943746A (en) * | 2019-04-20 | 2019-06-28 | 陕西斯瑞新材料股份有限公司 | A kind of preparation method of Ultra-fine Grained copper chromium contact |
-
2020
- 2020-05-19 CN CN202010427015.1A patent/CN111719087B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103862190A (en) * | 2012-12-17 | 2014-06-18 | 北京有色金属研究总院 | Novel cathode high-temperature brazing material and preparation method thereof |
| CN103658668A (en) * | 2013-12-06 | 2014-03-26 | 湖北鄂信钻石材料有限责任公司 | Method for preparing iron-based prealloy powder |
| CN108796304A (en) * | 2018-06-22 | 2018-11-13 | 江苏钛坦新材料有限公司 | A kind of γ-TiAl prealloys gas-atomized powder electrode bar and preparation method thereof |
| CN109055801A (en) * | 2018-07-31 | 2018-12-21 | 陕西斯瑞新材料股份有限公司 | A kind of preparation method using vacuum consumable arc-melting CuFe alloy material |
| CN109351982A (en) * | 2018-11-21 | 2019-02-19 | 陕西斯瑞新材料股份有限公司 | A kind of continuous production chromiumcopper milling method |
| CN109943746A (en) * | 2019-04-20 | 2019-06-28 | 陕西斯瑞新材料股份有限公司 | A kind of preparation method of Ultra-fine Grained copper chromium contact |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111719087A (en) | 2020-09-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111719087B (en) | Preparation method of medical CuFe alloy powder | |
| CN112222419B (en) | Method for preparing nano molybdenum powder by regulating nucleation and growth processes and application | |
| CN105063403A (en) | Preparation method of copper matrix graphene alloy | |
| Lee et al. | Synthesis of Mn–Al alloy nanoparticles by plasma arc discharge | |
| CN110229971B (en) | Preparation method of novel Cu-nano WC composite material | |
| CN106205935B (en) | A kind of amorphous state soft magnetism composite magnetic powder core and preparation method thereof | |
| CN113278842B (en) | Preparation method of titanium diboride copper-based spherical composite material powder | |
| CN105112694A (en) | Preparation method of magnesium base graphene alloy | |
| CN106756376A (en) | tungsten-copper alloy and its processing method and application | |
| CN111957971A (en) | Sintering preparation method of pure copper, copper alloy and copper-based composite material | |
| CN115044794B (en) | Cu- (Y) with excellent performance 2 O 3 -HfO 2 ) Alloy and preparation method thereof | |
| CN110976889A (en) | Preparation method of high-W-content W-Cu composite material | |
| CN111004959A (en) | FeNiCrCuCoBxNano high-entropy alloy and preparation method thereof | |
| CN113337747B (en) | Preparation method of high-strength and high-conductivity copper alloy | |
| CN107841669B (en) | High-thermal-conductivity active composite packaging material and preparation method thereof | |
| CN109317689A (en) | A kind of permalloy magnetic Nano absorbing material of core-shell structure and preparation method thereof | |
| Ding et al. | Microstructure and properties of WCu composites with low copper content at different sintering temperatures | |
| CN107414070A (en) | A kind of uniform-spherical graphene/monocrystalline copper composite powder and preparation method thereof | |
| CN114990383B (en) | Titanium alloy for improving yield ratio of electrode induction smelting inert gas atomized powder fine powder and preparation method of atomized powder | |
| CN114433859B (en) | High-quality electrode for titanium alloy powder, and preparation and application thereof | |
| CN109722561A (en) | High-performance Cu-Cr alloy and preparation method | |
| CN110453123A (en) | The method for preparing aluminium lithium alloy | |
| CN113755739B (en) | Method for improving mechanical property of additive manufactured austenitic steel | |
| CN109128143A (en) | A kind of fine/nano tungsten-copper raw powder's production technology with core-shell structure | |
| CN109545494A (en) | A kind of iron silica magnetic particle core material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |