CN113333752A - Titanium and titanium alloy injection molding feed product and preparation method thereof - Google Patents
Titanium and titanium alloy injection molding feed product and preparation method thereof Download PDFInfo
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- CN113333752A CN113333752A CN202010140760.8A CN202010140760A CN113333752A CN 113333752 A CN113333752 A CN 113333752A CN 202010140760 A CN202010140760 A CN 202010140760A CN 113333752 A CN113333752 A CN 113333752A
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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
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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Abstract
The invention relates to a feeding product for titanium and titanium alloy injection molding. The raw material of the product consists of titanium-containing powder and a binder, wherein the titanium-containing powder accounts for 55-60% of the total volume of the feed product; the binder accounts for 40-45% of the total volume of the feed product; the binder consists of PEG, PMMA, PVB, EVA, PW and SA; the mass percentage of each component of the adhesive is 50-70% of PEG, 5-10% of PMMA, 15-25% of PVB, 1-5% of EVA, 1-5% of PW and 1-5% of SA respectively. The feeding product has good fluidity, high strength and high solvent degreasing rate in the injection molding process, the obtained sintered blank has few defects, good shape retention, low porosity and high strength, and the final product has excellent texture and mechanical properties.
Description
Technical Field
The invention relates to the technical field of titanium alloy injection molding, in particular to a feeding product for titanium hydride powder injection molding and a preparation method thereof.
Background
Titanium and titanium alloy have a series of advantages of low density, high specific strength, corrosion resistance, good biocompatibility, no magnetism and the like, have wide application in the fields of aerospace, nuclear energy chemical industry and the like, and are important metal materials with wide application.
Titanium and titanium alloy have high processing difficulty and high processing cost, so that the application of the final product is limited. The titanium and titanium alloy injection molding technology has the characteristic of near-net-shape molding, and can be used for large-scale industrial production of small-size and precise parts. The injection molding products of titanium and titanium alloy can obtain structural substitute products with excellent performance, can be applied to aerospace and biomedical, and can meet the requirements of light weight and size. However, injection molding of titanium and titanium alloys places high demands on the powder, and requires a finer prealloyed powder with a low oxygen content, which is therefore a strict demand for powder and is costly. Compared with other metal injection molding technologies, the formula of the binder for titanium and titanium alloy injection molding has the advantages of large shrinkage ratio of the finished product after sintering and large control difficulty. The selection of the binder requires good conglobation, convenient degreasing, high powder ratio, shrinkage ratio control, powder cost reduction and performance improvement. The binder selected in the prior stage is prepared by proportioning main components of Paraffin Wax (PW) and backbone components of polymethyl methacrylate (PMMA) or polyvinyl butyral (PVB) and the like to obtain the wax-based binder, and the binder has good conglobation property and high viscosity, but has complex degreasing, needs solvent degreasing and has certain pollution to the environment.
The invention utilizes the TiH with low cost and simple preparation2Compared with the prior prealloying powder titanium alloy injection molding technology, the powder has the advantages of reduced cost, simple raw material acquisition and laying a foundation for the further development of titanium alloy injection molding. In addition, the product performance of injection molding is improved through the use and formula development of the water-soluble adhesive.
Disclosure of Invention
The invention provides a feeding formula for titanium and titanium alloy injection molding, aiming at the defects of the prior art.
The invention relates to a feeding formula for titanium and titanium alloy injection molding. The raw material of the feed comprises titanium-containing powder and a binder, wherein the titanium-containing powder accounts for 55-60% of the total volume of the feed product; the binder accounts for 40-45% of the total volume of the feed product; the binder consists of polyethylene glycol (PEG), polymethyl methacrylate (PMMA), polyvinyl butyral (PVB), ethylene-vinyl acetate copolymer (EVA), Paraffin (PW) and Stearic Acid (SA); the adhesive comprises 50-70% of polyethylene glycol, 5-10% of polymethyl methacrylate, 15-25% of polyvinyl butyral, 1-5% of ethylene-vinyl acetate copolymer, 1-5% of paraffin and 1-5% of stearic acid by mass percent.
The invention relates to a feeding formula for titanium and titanium alloy injection molding; the chemical components of the titanium-containing powder can be titanium hydride powder, hydrogenated titanium hydride powder, titanium-containing alloy powder and titanium sponge powder.
The invention relates to a feeding formula for titanium and titanium alloy injection molding; the chemical composition of the titanium hydride powder is that the hydrogen content is more than 3 percent; the titanium-containing powder is hydrogen-containing titanium powder with the total content of oxygen, nitrogen and carbon being less than 0.1%, and the particle size range D50 is 30-35 mu m.
The invention relates to a feeding formula for titanium and titanium alloy injection molding; the polyethylene glycol (PEG) in the adhesive is prepared by matching 10000 and 4000 of molecular weight according to a ratio of 5:2, and the total amount accounts for 60-70% of the total mass of the adhesive.
The invention relates to a feeding formula for titanium and titanium alloy injection molding; the injection product may be titanium alloy such as pure titanium, Ti6Al4V, Ti6Al7Nb, and the like.
The invention relates to a feeding formula for titanium and titanium alloy injection molding; the adhesive is divided into a high-melting point part and a low-melting point part, wherein the high-melting point part comprises polymethyl methacrylate (PMMA), polyvinyl butyral (PVB) and ethylene-vinyl acetate copolymer (EVA); the low-melting-point part comprises polyethylene glycol (PEG), Paraffin (PW) and Stearic Acid (SA), and the ratio of the high melting point to the low melting point is 2.5: 7.5-3: 7.
As a preferred embodiment; the invention relates to a feeding product formed by injection molding of titanium and titanium alloy; when the raw material is titanium hydride powder with the granularity range of 500-800 mm, controlling the titanium hydride powder to account for 60% of the total volume of the feeding product and controlling the binder to account for 40% of the total volume of the feeding product; when the mass percentage of each component of the binder is controlled to be 65 percent of polyethylene glycol, 6.7 percent of polymethyl methacrylate, 20 percent of polyvinyl butyral, 3.3 percent of ethylene-vinyl acetate copolymer, 3 percent of paraffin and 2 percent of stearic acid, the tensile strength of the obtained product is 676MPa, the elongation is 19 percent and the Vickers hardness is HV200 after injection molding and vacuum sintering.
As a preferred embodiment; the invention relates to a feeding product formed by injection molding of titanium and titanium alloy; when the raw material is titanium hydride powder with the granularity range of 500-800 mm, controlling the titanium hydride powder to account for 55% of the total volume of the feeding product and controlling the binder to account for 45% of the total volume of the feeding product; when the mass percentage of each component of the binder is controlled to be 65 percent of polyethylene glycol, 6.7 percent of polymethyl methacrylate, 20 percent of polyvinyl butyral, 3.3 percent of ethylene-vinyl acetate copolymer, 3 percent of paraffin and 2 percent of stearic acid, the tensile strength of the obtained product is 680MPa, the elongation is 17 percent and the Vickers hardness is HV 194 after injection molding and vacuum sintering. The single or combined performance of the two groups of optimized schemes is far beyond the corresponding indexes in the prior art.
The invention relates to a preparation method of a feeding formula for titanium and titanium alloy injection molding; the method comprises the following steps: respectively taking the components of the titanium hydride powder and the binder which are subjected to ball milling and sieving under the protection of argon, putting the components into an internal mixer for uniformly mixing, stirring at 180-200 ℃, mixing for 4-5 h, taking out the mixed feed, cooling, crushing in a crusher, and finally putting into a vacuum drying oven for storage or vacuumizing for packaging and storage.
Compared with other titanium alloy powder injection molding technologies, the titanium alloy powder injection molding technology has the following advantages:
(1) the water-soluble binder and the binder are easy and convenient to remove, can be directly dissolved in water, are easy to degrease and environment-friendly, have the degreasing rate of 99 percent, have few defects of degreased embryos, are good in shape retention, and have high strength and hardness.
(2) The components of the adhesive have good compatibility, the obtained feed product has good rheological property, and the defects of bubbles, flash and the like are avoided in the injection process.
(3) The sintered blank has small pores, the porosity is only about 1%, the final density of the product is about 99%, and the production requirement of a fully-compact and composite injection product is easily met.
(4) The product performance meets the requirement, and the tensile property basically reaches the average level of the fusion casting titanium alloy.
Drawings
FIG. 1 is an SEM image of a raw titanium hydride powder used in the embodiment.
FIG. 2 is an SEM image of a titanium metal product as an end product made from the feed product designed in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples.
The first embodiment is as follows:
1. putting titanium hydride raw material powder (the particle size range is 500-800 mm) into a roller ball mill, wherein the mass of the powder is 6.5kg, the mass of a stainless steel ball is 15kg, pumping argon for three times for atmosphere protection, the ball milling time is 2h, and the powder after ball milling is sieved by a 325-mesh screen to obtain hydrogen-containing powder with the particle size range D50: 20-25 mu m.
2. Mixing the sieved powder with a binder, wherein the powder accounts for 60%, the binder accounts for 40%, the binder comprises 65% of polyethylene glycol (PEG), 6.7% of polymethyl methacrylate (PMMA), 20% of polyvinyl butyral (PVB), 3.3% of ethylene-vinyl acetate copolymer (EVA), 2% of Stearic Acid (SA) and 3% of paraffin.
3. And banburying the mixed powder at 200 ℃ for 3h, repeatedly hammering for three times to stir, and finally cooling to obtain the feed.
4. Feeding the material into an injection machine for injection molding, wherein the injection temperature is 90 ℃, obtaining an injection product, degreasing the injection product in water at normal temperature for 15 hours, drying the injection product in the air, and thermally degreasing the injection product in an argon atmosphere, wherein the degreasing temperature is 800 ℃.
5. Putting the injection product into a vacuum sintering furnace, and vacuumizing (the vacuum degree is less than 10)-3Pa), raising the temperature to 1200 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
6. Opening the vacuum sintering furnace, taking out to obtain a molded injection product, wherein the density reaches over 99 percent, the tensile strength reaches 676MPa, the elongation is 19 percent, and the Vickers hardness is HV 200.
Example two:
1. putting titanium hydride raw material powder (the particle size range is 500-800 mm) into a roller ball mill, wherein the mass of the powder is 6.5kg, the mass of a stainless steel ball is 15kg, pumping argon for three times for atmosphere protection, the ball milling time is 1.5h, and the powder after ball milling is sieved by a 325-mesh screen to obtain hydrogen-containing powder with the particle size range D50: 20-25 mu m.
2. And mixing the sieved powder with a binder, wherein the powder accounts for 55% and the binder accounts for 45%. The binder comprises 65% of polyethylene glycol (PEG), 6, 7% of polymethyl methacrylate (PMMA), 20% of polyvinyl butyral (PVB), 3.3% of ethylene-vinyl acetate copolymer (EVA), 2% of Stearic Acid (SA) and 3% of paraffin.
3. And banburying the mixed powder at 200 ℃ for 3h, repeatedly hammering for three times to stir, and finally cooling to obtain the feed.
4. Feeding the material into an injection machine for injection molding, wherein the injection temperature is 90 ℃, obtaining an injection product, degreasing the injection product in water at normal temperature for 15 hours, drying the injection product in the air, and thermally degreasing the injection product in an argon atmosphere, wherein the degreasing temperature is 800 ℃.
5. Putting the degreased product into a vacuum sintering furnace, and vacuumizing (the vacuum degree is less than 10)-3Pa), raising the temperature to 1200 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
6. And opening the vacuum sintering furnace, taking out to obtain a molded injection product, wherein the density reaches over 99 percent, the tensile strength reaches 680MPa, the elongation is 17 percent, and the Vickers hardness HV reaches 194.
Example three:
1. putting titanium hydride raw material powder (the particle size range is 500-800 mm) into a roller ball mill, wherein the mass of the powder is 6.5kg, the mass of a stainless steel ball is 15kg, pumping argon for three times for atmosphere protection, the ball milling time is 1.5h, and the powder after ball milling is sieved by a 325-mesh screen to obtain hydrogen-containing powder with the particle size range D50: 20-25 mu m.
2. And mixing the sieved powder with a binder, wherein the powder accounts for 55% and the binder accounts for 45%. The binder comprises 65% of polyethylene glycol (PEG), 10% of polymethyl methacrylate (PMMA), 15% of polyvinyl butyral (PVB), 5% of ethylene-vinyl acetate copolymer (EVA), 2% of Stearic Acid (SA) and 3% of paraffin.
3. And banburying the mixed powder at 200 ℃ for 3h, repeatedly hammering for three times to stir, and finally cooling to obtain the feed.
4. Feeding the material into an injection machine for injection molding, wherein the injection temperature is 90 ℃, obtaining an injection product, degreasing the injection product in water at normal temperature for 15 hours, drying the injection product in the air, and thermally degreasing the injection product in an argon atmosphere, wherein the degreasing temperature is 800 ℃.
5. Putting the degreased product into a vacuum sintering furnace, and vacuumizing (the vacuum degree is less than 10)-3Pa), raising the temperature to 1200 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
6. And opening the vacuum sintering furnace, taking out to obtain a molded injection product, wherein the density reaches over 99 percent, a plurality of bubbles are generated and accompanied with partial defects, the shape is poor to maintain, and the tensile strength reaches 550 MPa.
Comparative example 1:
1. putting titanium hydride raw material powder (the particle size range is 500-800 mm) into a roller ball mill, wherein the mass of the powder is 6.5kg, the mass of a stainless steel ball is 15kg, pumping argon for three times for atmosphere protection, the ball milling time is 1.5h, and the powder after ball milling is sieved by a 325-mesh screen to obtain hydrogen-containing powder with the particle size range D50: 20-25 mu m.
2. And mixing the sieved powder with a binder, wherein the powder accounts for 55% and the binder accounts for 45%. The binder comprises 65% of polyethylene glycol (PEG), 4% of polymethyl methacrylate (PMMA), 25% of polyvinyl butyral (PVB), 1% of ethylene-vinyl acetate copolymer (EVA), 2% of Stearic Acid (SA) and 3% of paraffin.
3. And (3) banburying the mixed powder at 200 ℃ for 3h, repeatedly hammering for three times to stir, and finally cooling to obtain a feed with high feed viscosity.
4. Feeding the material into an injection machine for injection molding, wherein the injection temperature is 90 ℃, an injection product is obtained, the viscosity of an injection blank is high, the injection blank is easy to adhere to a mold and cannot fall off normally, and the product is softened to a certain extent.
5. Putting the degreased product into a vacuum sintering furnace, and vacuumizing (the vacuum degree is less than 10)-3Pa), raising the temperature to 1200 ℃, keeping for 2 hours and stoppingAnd (6) cooling the furnace.
6. Opening the vacuum sintering furnace, taking out to obtain a molded injection product, wherein the density is over 99 percent, the shape retention is poor, the molded injection product has certain deformation, and the tensile strength reaches 535 MPa.
Comparative example 2:
1. putting titanium hydride raw material powder (the particle size range is 500-800 mm) into a roller ball mill, wherein the mass of the powder is 6.5kg, the mass of a stainless steel ball is 15kg, pumping argon for three times for atmosphere protection, the ball milling time is 1.5h, and the powder after ball milling is sieved by a 325-mesh screen to obtain hydrogen-containing powder with the particle size range D50: 20-25 mu m.
2. And mixing the sieved powder with a binder, wherein the powder accounts for 60 percent, and the binder accounts for 40 percent. The binder comprises 65% of polyethylene glycol (PEG), 30% of polymethyl methacrylate (PMMA), 2% of Stearic Acid (SA) and 3% of paraffin.
3. Banburying the mixed powder at 200 ℃ for 3h, repeatedly hammering for three times to stir for better fluidity, and finally cooling to obtain the feed.
4. Feeding the material into an injection machine for injection molding, wherein the injection temperature is 90 ℃, obtaining an injection product, then carrying out water degreasing in normal temperature water for 15 hours, and airing, wherein the obtained degreased blank is bent, the shape of the degreased blank has defects, the product is softened, the shape of the degreased blank cannot be kept, and the experiment fails.
Comparative example 3:
1. putting titanium hydride raw material powder (the particle size range is 500-800 mm) into a roller ball mill, wherein the mass of the powder is 6.5kg, the mass of a stainless steel ball is 15kg, pumping argon for three times for atmosphere protection, the ball milling time is 1.5h, and the powder after ball milling is sieved by a 325-mesh screen to obtain hydrogen-containing powder with the particle size range D50: 20-25 mu m.
2. And mixing the sieved powder with a binder, wherein the powder accounts for 60 percent, and the binder accounts for 40 percent. The binder comprises 65% of polyethylene glycol (PEG), 30% of polyvinyl butyral (PVB) and 2% of Stearic Acid (SA).
3. Banburying the mixed powder at 200 ℃ for 3h, repeatedly hammering for three times to stir, wherein the viscosity is high, and finally cooling to obtain the feed.
4. Feeding the material into an injection machine for injection molding, wherein the injection temperature is 90 ℃, obtaining an injection product, then carrying out water degreasing in normal temperature water for 15 hours, airing, obtaining a degreased blank which is scattered, and the clear water turns black in color and has powder precipitates, so that the shape cannot be kept, and the experiment fails.
Claims (9)
1. A titanium and titanium alloy injection molded feed product; the raw material of the product consists of titanium-containing powder and a binder, and is characterized in that: the titanium-containing powder accounts for 55 to 60 percent of the total volume of the feed product; the binder accounts for 40-45% of the total volume of the feed product; the binder consists of polyethylene glycol, polymethyl methacrylate, polyvinyl butyral, ethylene-vinyl acetate copolymer, paraffin and stearic acid; the adhesive comprises 50-70% of polyethylene glycol, 5-10% of polymethyl methacrylate, 15-25% of polyvinyl butyral, 1-5% of ethylene-vinyl acetate copolymer, 1-5% of paraffin and 1-5% of stearic acid by mass percent.
2. A titanium and titanium alloy injection molded feedstock product according to claim 1; the method is characterized in that: the adhesive comprises 65 mass percent of polyethylene glycol, 6.7 mass percent of polymethyl methacrylate, 20-25 mass percent of polyvinyl butyral, 3.3 mass percent of ethylene-vinyl acetate copolymer, 3 mass percent of paraffin and 2 mass percent of stearic acid.
3. A titanium and titanium alloy injection molded feedstock product according to claim 1; the method is characterized in that: the chemical components of the titanium-containing powder are at least one of titanium hydride powder, hydrogenated titanium hydride powder, titanium alloy-containing powder and titanium sponge powder.
4. A titanium and titanium alloy injection molded feedstock product according to claim 2; the method is characterized in that: the chemical composition of the titanium hydride powder is that the hydrogen content is more than 3 wt%; the titanium-containing powder is hydrogen-containing titanium powder with the total content of oxygen, nitrogen and carbon less than 0.1 wt%, and the particle size range D50 is 30-35 mu m.
5. A titanium and titanium alloy injection molded feedstock product according to claim 1; the method is characterized in that: the polyethylene glycol in the binder is prepared by mixing two components with the molecular weight of 10000 and the molecular weight of 4000 according to the proportion of 8: 3-5: 2, and the total amount accounts for 60-70% of the total mass of the binder.
6. A titanium and titanium alloy injection molded feedstock product according to claim 1; the method is characterized in that: the binder is divided into a high melting point part and a low melting point part, and the high melting point part is polymethyl methacrylate, polyvinyl butyral and ethylene-vinyl acetate copolymer; the low-melting-point part is polyethylene glycol, paraffin and stearic acid, and the mass ratio of the high-melting-point part to the low-melting-point part is 2.5: 7.5-3: 7.
7. A titanium and titanium alloy injection molded feedstock product according to claim 1; the method is characterized in that: when the raw material is titanium hydride powder with the granularity range of 500-800 mm, controlling the titanium hydride powder to account for 60% of the total volume of the feeding product and controlling the binder to account for 40% of the total volume of the feeding product; when the mass percentage of each component of the binder is controlled to be 65 percent of polyethylene glycol, 6.7 percent of polymethyl methacrylate, 20 percent of polyvinyl butyral, 3.3 percent of ethylene-vinyl acetate copolymer, 3 percent of paraffin and 2 percent of stearic acid, the tensile strength of the obtained product is 676MPa, the elongation is 19 percent and the Vickers hardness is HV200 after injection molding and vacuum sintering.
8. A titanium and titanium alloy injection molded feedstock product according to claim 1; the method is characterized in that: when the raw material is titanium hydride powder with the granularity range of 500-800 mm, controlling the titanium hydride powder to account for 55% of the total volume of the feeding product and controlling the binder to account for 45% of the total volume of the feeding product; when the mass percentage of each component of the binder is controlled to be 65 percent of polyethylene glycol, 6.7 percent of polymethyl methacrylate, 20 percent of polyvinyl butyral, 3.3 percent of ethylene-vinyl acetate copolymer, 3 percent of paraffin and 2 percent of stearic acid, the tensile strength of the obtained product is 680MPa, the elongation is 17 percent and the Vickers hardness is HV 194 after injection molding and vacuum sintering.
9. A method of preparing a feed formulation for injection molding of titanium and titanium alloys as defined in claim 1; the method is characterized by comprising the following steps: respectively taking the components of the titanium hydride powder and the binder which are subjected to ball milling and sieving under the protection of argon, putting the components into an internal mixer for uniformly mixing, stirring at 180-200 ℃, mixing for 4-5 h, taking out the mixed feed, cooling, crushing in a crusher, and finally putting into a vacuum drying oven for storage or vacuumizing for packaging and storage.
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| CN114160795A (en) * | 2021-10-29 | 2022-03-11 | 深圳艾利佳材料科技有限公司 | Low-cost porous titanium alloy injection molding method |
| CN115055674A (en) * | 2022-06-29 | 2022-09-16 | 中南大学 | Feed suitable for additive manufacturing of tungsten-cobalt hard alloy parts and preparation method and application thereof |
| CN117340252A (en) * | 2023-10-09 | 2024-01-05 | 广东潮艺金属实业有限公司 | High-heat-conductivity injection molding feed containing titanium-stainless steel composite powder and preparation method and application thereof |
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| CN117340252B (en) * | 2023-10-09 | 2024-03-29 | 广东潮艺金属实业有限公司 | High-heat-conductivity injection molding feed containing titanium-stainless steel composite powder and preparation method and application thereof |
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