CN108465806B - Method for preparing high-performance powder metallurgy product by coating alloy powder with organic matter - Google Patents
Method for preparing high-performance powder metallurgy product by coating alloy powder with organic matter Download PDFInfo
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- CN108465806B CN108465806B CN201810200270.5A CN201810200270A CN108465806B CN 108465806 B CN108465806 B CN 108465806B CN 201810200270 A CN201810200270 A CN 201810200270A CN 108465806 B CN108465806 B CN 108465806B
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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Abstract
The invention provides a method for preparing a high-performance powder metallurgy product by coating alloy powder with organic matters, belonging to the field of powder metallurgy. The method is characterized in that a solution film covering method is adopted to coat a layer of organic film on the surface of the alloy powder, the organic is dissolved in a solvent to form a layer of liquid film on the surface of the alloy powder, after the solvent is removed, the organic can be uniformly coated on the alloy powder, and the organic film is coated on the surface of the alloy powder without any chemical reaction, so that the aim of isolating the easily oxidized alloy powder from oxygen is fulfilled. The surface of the easily oxidized alloy powder can react with oxygen easily, the formed alloy part has poor mechanical property due to the increase of the oxygen content in the forming process, the organic matter is used for coating, the effect of controlling oxygen in the forming process can be effectively achieved, the oxidation resistance of the alloy powder can be improved through coating treatment in the forming process, and the low oxygen content and the excellent mechanical property can be kept after forming.
Description
Technical Field
the invention belongs to the field of powder metallurgy, and provides a method for preparing a high-performance powder metallurgy product by coating alloy powder with organic matters.
background
powder materials in powder metallurgy, particularly particles having smaller particle diameters, are susceptible to oxidation due to their increased surface active sites, large specific surface area, large specific surface energy, and the like, caused by their small size effect. In the case of oxygen-sensitive metal materials, oxidation of the metal powder results in an increase in the oxygen content of the raw material, which not only affects the press-formability of the powder, but also ultimately severely affects various properties of the final product. In the case of titanium alloy, the plasticity of titanium alloy decreases sharply with the increase of oxygen content, and when the oxygen content increases from 0.3% to 0.4%, the elongation decreases from 10% or more to about 3%. Controlling the oxygen content of the powder is of great significance for forming high performance metal materials. At present, the preparation process of the titanium alloy mainly comprises casting and powder metallurgy, the casting process has higher cost due to active chemical property of the titanium alloy at high temperature, difficult smelting and long processing route, and is difficult to meet the requirement of large-scale application in the civil market, and the powder metallurgy product greatly promotes the application of the titanium alloy in the civil market, so that the significance of developing high-performance powder metallurgy products and advanced preparation technology is great.
The common preparation processes for powder metallurgy products include hot isostatic pressing, cold isostatic pressing, injection molding, gel casting, 3D printing and the like. When the processes are applied, easily oxidized alloy powder, such as titanium, magnesium, copper, neodymium iron boron and the like, is easy to react with oxygen due to large surface energy, and the formed alloy part has poor mechanical properties due to the increase of oxygen content in the forming process, particularly, the thinner the titanium alloy powder, the larger the specific surface area is, the more serious the oxygen increasing condition is, and the oxidation can be caused when the titanium alloy powder is exposed and placed at room temperature. Generally, injection molding and 3D printing have requirements for low oxygen content of the raw material of the easily-oxidizable alloy powder, which leads to increased cost, and measures such as controlling the molding atmosphere, temperature, sintering environment and other production conditions are generally adopted for controlling oxygen of the alloy powder in the molding process.
the existing oxygen control method for easily oxidized alloy powder mainly focuses on the oxygen increasing and carbon increasing conditions of the process in the processing process, and the surface modification is rarely carried out on the alloy powder. The invention adopts the organic matter to coat the alloy powder, and uses the organic matter to coat, which not only can increase the compatibility of the forming agent, the binder and the titanium powder in some processes, but also can be easily removed, the metal powder which is easily oxidized at normal temperature does not react with the organic matter and is very stable, and the effect of controlling oxygen in the forming process can be effectively achieved by the pretreatment before the alloy powder is formed. And the oxidation resistance of the alloy powder can be improved by coating treatment in the forming process, so that the low oxygen content and excellent mechanical property can be kept after forming.
Disclosure of Invention
The invention aims to provide a method for preparing a high-performance powder metallurgy product by using organic matter coated alloy powder, which achieves a satisfactory result in controlling the oxygen increasing condition of easily-oxidized alloy powder in the forming process, can improve the oxidation resistance of the powder, reduces the forming cost and obtains more excellent mechanical properties.
In order to obtain the method for preparing the high-performance powder metallurgy product by using the organic matter coated alloy powder, the invention adopts the following technical scheme, and the method comprises the following specific steps:
(1) preparing a coating solution: dissolving the organic matter coating body in an organic solvent, and uniformly stirring to prepare an organic matter coating solution, wherein the concentration of the solution is 0.01g/ml-1.5 g/ml;
(2) powder coating: according to the mass percentage, the mass of the organic matter coating body is 0.05-0.5 wt% of the mass of the alloy powder, the organic matter coating solution in the step (1) with the corresponding volume is measured, the organic matter coating solution and the alloy powder are uniformly mixed, so that the solution soaks all the powder, and the whole process is carried out in an argon atmosphere in a glove box;
(3) Powder treatment: putting the coated powder into a vacuum drying oven, drying for 30-120min at 25-40 ℃, taking out, putting the dried coated powder into a ball milling tank, introducing argon gas for atmosphere protection, putting the ball milling tank on a ball mill for ball milling and crushing, wherein the ball milling speed is 100r/min-250r/min, the ball-to-material ratio is 4:1-7:1, and the ball milling time is 15-60min to obtain alloy powder coated with organic matters;
(4) forming: and (4) forming the alloy powder coated in the step (3) by using a powder metallurgy technology to obtain a blank.
(5) And (3) sintering: and (4) sintering the green body obtained in the step (4) in the atmosphere of hydrogen, argon or vacuum at the sintering temperature of 500-1400 ℃, and preserving heat for 30-300min to prepare the metal structural member in the required shape.
Further, the organic coating in the step (1) is one or more of stearic acid, polymethyl methacrylate, polyvinyl alcohol, polyethylene glycol, paraffin, beeswax, rosin, polyethylene and the like.
Further, the solvent in the step (1) is toluene, xylene, acetone, ethanol, dichloromethane, gasoline, kerosene and water.
further, the alloy powder in the step (2) may be titanium and titanium alloy powder, magnesium and magnesium alloy powder, copper and copper alloy powder or neodymium iron boron powder, etc., and the particle size of the powder is 10-100 μm.
Further, the powder metallurgy technology in the step (4) is compression molding, injection molding, 3D printing, 3D cold printing or gel injection molding technology.
The invention has the advantages that:
1. The increase of the oxygen content of the alloy powder in the forming process is well controlled, and the mechanical property is improved.
2. The organic matter is burnt at high temperature to generate protective atmosphere, and the oxygen increasing condition of the alloy powder in the forming process is further controlled.
3. Under the action of thermal convection of thermal processing such as sintering and the like, the organic matter coating layer can further isolate air, thereby effectively inhibiting the generation of defects and reducing the defects such as air holes and the like.
Detailed Description
Example 1:
Stearic acid-coated TC4 titanium alloy powder for gel casting.
(1) preparing a coating solution: dissolving 25g of stearic acid in 500ml of dichloromethane, and uniformly stirring to prepare an organic matter coating solution, wherein the concentration of the solution is 0.05 g/ml;
(2) powder coating: according to the mass percentage, the mass of the organic coating is 0.1 percent of the mass of TC4 titanium alloy powder, 100g of 45-micron hydrogenated and dehydrogenated TC4 titanium alloy powder is weighed, 200ml of the organic coating solution in the step (1) is weighed, the solution and the titanium alloy powder are uniformly mixed, the solution is made to soak all the powder, and the whole process is carried out in a glove box under the argon atmosphere;
(3) powder treatment: putting the coated powder into a vacuum drying oven, drying for 90min at 30 ℃, taking out, putting the dried coated powder into a ball milling tank, introducing argon for atmosphere protection, putting the ball milling tank on a ball mill for ball milling and crushing at the ball milling speed of 100r/min and the ball-to-material ratio of 5:1, and carrying out ball milling for 20min to obtain TC4 titanium alloy powder coated with stearic acid;
(4) forming: preparing a premixed solution from an organic monomer methacrylamide and a solvent toluene, mixing the premixed solution with the coated metal powder to prepare slurry with the solid content of 50%, then adding a cross-linking agent, uniformly stirring in a ball mill, and pouring into a mold for carrying out gel reaction.
(5) And (3) sintering: and (4) sintering the gel-casting green body obtained in the step (4) in argon at 1300 ℃ for 90min, and preparing the metal structural member with the required shape.
Example 2:
A polyethylene glycol coated pure copper powder for press forming.
(1) Preparing a coating solution: dissolving 10g of polyethylene glycol in 1000ml of water, and uniformly stirring to prepare an organic matter coating solution, wherein the concentration of the solution is 0.01 g/ml;
(2) Powder coating: weighing 50g of water atomized pure copper powder with the particle size of 25 microns, wherein the mass of the organic coating is 0.5 percent of the mass of the pure copper powder, weighing 25ml of the organic coating solution in the step (1), adding 100ml of deionized water into the weighed organic solution, uniformly mixing the solution and the titanium alloy powder to enable the solution to infiltrate the whole powder, and carrying out the whole process in a glove box under the argon atmosphere;
(3) Powder treatment: putting the coated powder into a vacuum drying oven, drying for 90min at 40 ℃, taking out, putting the dried coated powder into a ball milling tank, introducing argon for atmosphere protection, putting the ball milling tank on a ball mill for ball milling and crushing at the ball milling speed of 150r/min and the ball-to-material ratio of 6:1, and carrying out ball milling for 30min to obtain pure copper powder coated with polyethylene glycol;
(4) Forming: putting the pure copper powder coated with the polyethylene glycol into a standard cylindrical die with the diameter of 10mm and the height of 15mm for pressing, wherein the pressing pressure is 240MPa, and the pressure maintaining time is 10 s.
(5) and (3) sintering: and (4) sintering the pressed compact obtained in the step (4) in hydrogen at 950 ℃ for 45min to prepare the metal product with the required shape.
Claims (3)
1. A method for preparing a powder metallurgy product by using organic matter coated alloy powder is characterized by comprising the following steps:
(1) preparing a coating solution: dissolving the organic matter coating body in an organic solvent or water, and uniformly stirring to prepare an organic matter coating solution, wherein the concentration of the solution is 0.01g/ml-1.5 g/ml;
(2) Powder coating: according to the mass percentage, the mass of the organic matter coating body is 0.05-0.5 wt% of the mass of the alloy powder, the organic matter coating solution in the step (1) with the corresponding volume is measured, the organic matter coating solution and the alloy powder are uniformly mixed, so that the solution soaks all the powder, and the whole process is carried out in an argon atmosphere in a glove box;
(3) powder treatment: putting the coated powder into a vacuum drying oven, drying for 30-120min at 25-40 ℃, taking out, putting the dried coated powder into a ball milling tank, introducing argon gas for atmosphere protection, putting the ball milling tank on a ball mill for ball milling and crushing, wherein the ball milling speed is 100r/min-250r/min, the ball-to-material ratio is 4:1-7:1, and the ball milling time is 15-60min to obtain alloy powder coated with organic matters;
(4) forming: forming the alloy powder coated in the step (3) by a powder metallurgy technology to prepare a green body;
(5) And (3) sintering: sintering the green body obtained in the step (4) in hydrogen, argon or vacuum at the sintering temperature of 500-1400 ℃, and keeping the temperature for 30-300min to prepare a powder metallurgy product with a required shape;
The organic matter coating body in the step (1) is one or more of stearic acid, polymethyl methacrylate, polyvinyl alcohol, polyethylene glycol, paraffin, beeswax, rosin and polyethylene;
In the step (2), the alloy powder is easily oxidized powder and comprises titanium powder, titanium alloy powder, magnesium alloy powder, copper alloy powder or neodymium iron boron powder, and the particle size of the powder is 10-100 μm.
2. The method for preparing a powder metallurgy product from the organic matter coated alloy powder according to claim 1, wherein the method comprises the following steps: the organic solvent in the step (1) is toluene, xylene, acetone, ethanol, dichloromethane, gasoline or kerosene.
3. the method for preparing a powder metallurgy product from the organic matter coated alloy powder according to claim 1, wherein the method comprises the following steps: the powder metallurgy technology in the step (4) is compression molding, injection molding, 3D printing or gel casting molding technology.
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