CN113500192A - High-fluidity high-strength metal powder injection molding feed and application method thereof - Google Patents

High-fluidity high-strength metal powder injection molding feed and application method thereof Download PDF

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CN113500192A
CN113500192A CN202110573393.5A CN202110573393A CN113500192A CN 113500192 A CN113500192 A CN 113500192A CN 202110573393 A CN202110573393 A CN 202110573393A CN 113500192 A CN113500192 A CN 113500192A
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percent
temperature
feed
injection molding
injection
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CN113500192B (en
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姜洪亮
苏来军
王茂堂
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Dongguan Huayingxin Technology Co.,Ltd.
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Ningbo Xinruihong New Material Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture 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
    • B22F3/225Manufacture 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • B22F3/1021Removal of binder or filler
    • B22F3/1025Removal of binder or filler not by heating only
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a high-fluidity high-strength metal powder injection molding feed and an application method thereof, wherein the feed comprises alloy powder and a binder combination; according to the mass percentage, the alloy powder accounts for 90% of the feeding mass, and the binder combination accounts for 10% of the feeding mass; the binder combination comprises the following components in percentage by mass: 82 to 84 percent of polyformaldehyde, 3 to 6.5 percent of low-density polyethylene, 3.5 to 4.5 percent of rubber elastomer, 1 to 3.5 percent of paraffin, 1.5 to 2 percent of silicone oil, 0.5 to 1.5 percent of zinc stearate, 0.5 to 1 percent of antioxidant, 0.5 to 1 percent of formaldehyde curing agent and 0.5 to 2.5 percent of oleic acid, wherein the total amount of all the components is 100 percent. The feeding material has the comprehensive advantages of ultrahigh flow rate, excellent physical properties of materials, good dimensional stability and the like, greatly reduces the production cost and improves the production efficiency.

Description

High-fluidity high-strength metal powder injection molding feed and application method thereof
Technical Field
The invention relates to the technical field of metal powder injection molding, in particular to a high-fluidity high-strength metal powder injection molding feed and an application method thereof.
Background
The current technology of manufacturing is rapidly developed, and the parts manufactured in various fields are developed towards the light weight, miniaturization and structure complication of products. The miniature precision part has the structural characteristics that: miniature, accurate, material high performance etc. because the structure is too little and accurate, traditional technology is not especially ideal in production efficiency, cost, precision aspect.
Metal powder Injection Molding (MIM) is a new technology emerging in recent years, and has the characteristics of high efficiency, high precision and low cost, and the minimally invasive clamp taking characteristic is very suitable for batch production by using the MIM powder Injection Molding process. The key control point of the sampling clamp for producing tiny, high-precision and high-performance materials by powder injection molding is the preparation of binder feed for powder injection molding.
Because the structure of the miniature precision part is too micro, small and thin, the miniature precision part has very high requirements on the flowability of powder injection molding feed, the shape retention property and the dimensional stability of post sintering treatment and the high performance of materials.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the technical defects of the background technology and provides a high-fluidity high-strength metal powder injection molding feed and an application method thereof. The invention redesigns the particle size of the powder material, the content of metal elements and the like to ensure the high performance of the material, and performs targeted design on the melting speed and the product structure shape-keeping property in feeding aiming at the characteristics of a product with a tiny and single structure; the feeding material has the comprehensive advantages of ultrahigh flow rate, excellent physical properties of materials, good dimensional stability and the like, greatly reduces the production cost and improves the production efficiency.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a high flow high strength metal powder injection molding feed comprising an alloy powder and binder combination; according to the mass percentage, the alloy powder accounts for 90% of the feeding mass, and the binder combination accounts for 10% of the feeding mass; the binder combination comprises the following components in percentage by mass: 82 to 84 percent of polyformaldehyde, 3 to 6.5 percent of low-density polyethylene, 3.5 to 4.5 percent of rubber elastomer, 1 to 3.5 percent of paraffin, 1.5 to 2 percent of silicone oil, 0.5 to 1.5 percent of zinc stearate, 0.5 to 1 percent of antioxidant, 0.5 to 1 percent of formaldehyde curing agent and 0.5 to 2.5 percent of oleic acid, wherein the total amount of all the components is 100 percent.
Preferably, the alloy powder is 17-4PH material powder atomized by water and gas of-800 meshes, the D50 particle size is about 7 microns, and the tap density of the powder is 4.7g/cm3
More preferably, the alloy powder has elemental contents of: 0.04% of carbon, 18% of chromium, 6% of nickel, 4% of copper, 0.5% of niobium, 0.5% of manganese and the balance of iron.
The application method of the high-fluidity high-strength metal powder injection molding feed comprises the following steps:
(1) mixing:
preparing a feed in an internal mixer-granulator integrated machine, setting a temperature value of an internal mixing cavity to be 185-190 ℃, firstly adding polyformaldehyde, low-density polyethylene and a rubber elastomer into the cavity of the internal mixer, and stirring and melting; then adding alloy powder, stirring for about 5-8 minutes, adding paraffin, silicone oil, zinc stearate, an antioxidant and a formaldehyde curing agent, stirring at the rotating speed of 39-65 revolutions per minute, stirring and melting to form mud, adding oleic acid, and finally uniformly stirring for 16-25 minutes; after banburying is finished, cooling the banburying cavity to 163-171 ℃, starting extrusion granulation, wherein the rotation speed of a granulation screw is 120-133 revolutions per minute, the extrusion granulation temperature is 162-168 ℃, and an extruder head cools granulation by using air to obtain a feed;
(2) injection molding:
the obtained feed is used for injection molding of a mold on a high-speed injection machine of a specially-made high-wear-resistant alloy screw barrel assembly, the set temperature of the mold is 93-102 ℃, the set temperature of injection is 185-190 ℃, the injection speed is 95-110%, and the injection pressure is 100-110 MPa, so that a complete injection blank is finally obtained;
(3) catalytic degreasing:
putting the product into a catalytic degreasing furnace, introducing air to remove the POM binder carrier, and introducing N2Atmosphere protection is carried out on the gas, the heating temperature of a hearth is set to be 120 ℃, the acid flow is 3.3-3.6 g per minute, the degreasing time is set to be 400-420 min, and the degreasing rate is controlled to be more than 7.1%;
(4) and (3) sintering:
putting the obtained injection blank into a degreasing and sintering integrated furnace for sintering treatment, raising the temperature of room temperature to 600 ℃ at the rate of 2 ℃ per minute at the temperature of between 600 and 600 ℃, and carrying out N2The flow rate is 40-44L/min per minute, then the temperature is kept for 180min, and the inert gas is N2And the gas flow is 41-47L/min, after the 600 ℃ temperature is held, the temperature is raised to 1060-1100 ℃ at the rate of 3 ℃ per minute and held for 60min in vacuum sintering, after the 1060-1100 ℃ temperature is held, AR gas is introduced at the rate of 3 ℃ per minute to maintain the pressure in the furnace from 15KPa to 1353-1360 ℃ for 180min, after the 1353-1360 ℃ temperature is held, the furnace is cooled to the room temperature, and the whole sintering process is finished.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention uses the combination of metal nano alloy powder and a special binder formula to prepare a feed for alloy injection in a metal banburying and granulating integrated machine, and the prepared alloy feed has the characteristic of ultrahigh fluidity and has a high-strength binder framework to ensure that the subsequent molding sintering has excellent performance by adopting the special binder formula, so that the alloy feed has obvious molding advantages on the molding of products with special structures and ultrathin structures and surpasses the conventional process in the mechanical property and surface property of the products;
(2) the feed has ultrahigh flow rate, the melt index can reach 1800-2200 g/10min, the feed has the obvious advantage of rapid injection filling for products with ultrathin structures and tiny complex structures, the special binder proportion ensures the stability of repeated cyclic utilization of the recycled nozzle material, the number of times of cyclic utilization of the nozzle material can reach 40 times of high-proportion cycle, the feed has great improvement on the dimensional stability of subsequent sintering, the precision of a final product can be controlled within the range of 0.2-0.3%, and the production cost is greatly reduced.
Detailed Description
For a better understanding of the present invention, reference is made to the following examples. It is to be understood that these examples are for further illustration of the invention and are not intended to limit the scope of the invention. In addition, it should be understood that the invention is not limited to the above-described embodiments, but is capable of various modifications and changes within the scope of the invention.
The integrated banburying and granulating machine of embodiments 1 to 4 is a bridge Yilong composite banburying and granulating machine, model M-H-10L-DCSS-H.
The high speed injection machine described in examples 1-4 was a Cantonese Norhn MIM 130.
Example 1
A high flow high strength metal powder injection molding feed comprising an alloy powder and binder combination; the feeding binder system is a catalytic degreasing system, the alloy powder accounts for 90% of the feeding mass, and the binder combination accounts for 10% of the feeding mass; the binder combination comprises the following components in percentage by mass: 82% of polyformaldehyde, 6% of low-density polyethylene, 4% of rubber elastomer, 3% of paraffin, 2% of silicone oil, 0.5% of zinc stearate, 0.5% of antioxidant, 1% of formaldehyde curing agent and 1% of oleic acid.
The alloy powder is 17-4PH material powder atomized by water and gas of-800 meshes, the D50 particle size is about 7 microns, and the tap density of the powder is 4.7g/cm3(ii) a The element structure of the alloy powder is finely adjusted, and the content of nickel element and the content of chromium element are increased slightly on the existing material element system, so as to improve the corrosion resistance and the structural strength of the material; the content of alloy powder elements is as follows: 0.04% of carbon, 18% of chromium, 6% of nickel, 4% of copper, 0.5% of niobium, 0.5% of manganese and the balance of iron.
The proportioning design of the alloy powder elements improves the material performance of the product and obviously improves the corrosion resistance and the mechanical property of the product.
The application method of the high-fluidity high-strength metal powder injection molding feed comprises the following steps:
(1) mixing:
the preparation method comprises the following steps of preparing a feed in an internal mixer-granulator, setting a temperature value of an internal mixing cavity to be 185 ℃, firstly adding polyformaldehyde, low-density polyethylene and a rubber elastomer into the cavity of the internal mixer for stirring and melting, wherein the purpose of the step is to fully fuse molecular chains of high polymer materials with each other and contribute to the uniformity of a binder system; after the high molecular components are stirred and fused, adding metal alloy powder, stirring for about 5 minutes, and then adding paraffin, silicone oil, zinc stearate, an antioxidant and a formaldehyde curing agent, wherein the stirring speed is 45 revolutions per minute, and the step aims to fully wrap the low molecular lubricant on the surface of the powder, ensure that excellent lubrication effect is achieved among powder microparticles and promote the improvement of melt index; the antioxidant is added to improve the heat resistance stability of the high polymer material so as to ensure the stability of subsequent nozzle circulating materials; the formaldehyde curing agent is added to increase the strength of the main body framework adhesive and increase the strength and deformation resistance of the injection blank; and adding oleic acid after stirring and melting into mud, and finally uniformly stirring for 16 minutes, wherein the oleic acid has the functions of reducing the adhesion among the powder, improving the dispersibility of the feed and promoting the uniformity among the components of each binder and the powder. After banburying is finished, cooling the banburying cavity to 168 ℃, starting extrusion granulation, wherein the rotation speed of a granulation screw is 120 revolutions per minute, the extrusion granulation temperature is 166 ℃, an extruder head is used for cooling granulation by wind, the length-width ratio of the prepared finished product feed particles is about 2.0-2.5 mm, and the excellent production stability of the feed with the external shape size can be ensured in the injection process;
(2) injection molding:
the obtained feed is used for injection molding on a die on a high-speed injection machine of a specially-made high-wear-resistant alloy screw barrel component, the set temperature of the die is 100 ℃, the set temperature of the injection is 185 ℃, the injection speed is 95%, the injection pressure is 100MPa, and finally a complete injection blank is obtained;
(3) catalytic degreasing:
product storage devicePutting the mixture into a catalytic degreasing furnace, introducing air to remove the POM binder carrier, and introducing N2Atmosphere protection is carried out on gas, the heating temperature of a hearth is set to be 120 ℃, the acid flow is 3.5 g/min, the degreasing time is set to be 420min, and the degreasing rate is controlled to be more than 7.2%;
(4) and (3) sintering:
putting the obtained injection blank into a degreasing and sintering integrated furnace for sintering treatment, raising the temperature of room temperature to 600 ℃ at the rate of 2 ℃ per minute at the temperature of between 600 and 600 ℃, and carrying out N2The flow rate is 40L/min per minute, and the temperature is maintained for 180min, and the inert gas is N2The gas flow is 45L/min, the temperature is raised to 1100 ℃ at the rate of 3 ℃ per minute after the temperature is maintained at 600 ℃ for 60min, AR gas is introduced at the rate of 3 ℃ per minute after the temperature is maintained at 1100 ℃ to maintain the pressure in the furnace from 15KPa to 1360 ℃ for 180min, the temperature is maintained at 1360 ℃ and then the furnace is cooled to the room temperature, and the whole sintering process is finished.
Example 2
A high flow high strength metal powder injection molding feed comprising an alloy powder and binder combination; the feeding binder system is a catalytic degreasing system, the alloy powder accounts for 90% of the feeding mass, and the binder combination accounts for 10% of the feeding mass; the binder combination comprises the following components in percentage by mass: 83% of polyformaldehyde, 5.5% of low-density polyethylene, 4.5% of rubber elastomer, 2% of paraffin, 1.5% of silicone oil, 1.0% of zinc stearate, 1.0% of antioxidant, 1.0% of formaldehyde curing agent and 0.5% of oleic acid.
The alloy powder is 17-4PH material powder atomized by water and gas of-800 meshes, the D50 particle size is about 7 microns, and the tap density of the powder is 4.7g/cm3(ii) a The element structure of the alloy powder is finely adjusted, and the content of nickel element and the content of chromium element are increased slightly on the existing material element system, so as to improve the corrosion resistance and the structural strength of the material; the content of alloy powder elements is as follows: 0.04% of carbon, 18% of chromium, 6% of nickel, 4% of copper, 0.5% of niobium, 0.5% of manganese and the balance of iron.
The proportioning design of the alloy powder elements improves the material performance of the product and obviously improves the corrosion resistance and the mechanical property of the product.
The application method of the high-fluidity high-strength metal powder injection molding feed comprises the following steps:
(1) mixing:
the preparation method comprises the following steps of preparing a feed in an internal mixer-granulator, setting a temperature value of an internal mixing cavity to be 185 ℃, firstly adding polyformaldehyde, low-density polyethylene and a rubber elastomer into the cavity of the internal mixer for stirring and melting, wherein the purpose of the step is to fully fuse molecular chains of high polymer materials with each other and contribute to the uniformity of a binder system; after the high molecular components are stirred and fused, adding metal alloy powder, stirring for about 6 minutes, and then adding paraffin, silicone oil, zinc stearate, an antioxidant and a formaldehyde curing agent, wherein the stirring speed is 65 revolutions per minute, and the step aims to fully wrap the low molecular lubricant on the surface of the powder, ensure that excellent lubrication effect is achieved among powder microparticles and promote the improvement of melt index; the antioxidant is added to improve the heat resistance stability of the high polymer material so as to ensure the stability of subsequent nozzle circulating materials; the formaldehyde curing agent is added to increase the strength of the main body framework adhesive and increase the strength and deformation resistance of the injection blank; and adding oleic acid after stirring and melting into mud, and finally uniformly stirring for 18 minutes, wherein the oleic acid has the functions of reducing the adhesion among the powder, improving the dispersibility of the feed and promoting the uniformity among the components of each binder and the powder. After banburying is finished, the temperature of a banburying cavity is reduced to 171 ℃, extrusion granulation is started, the rotation speed of a granulation screw is 120 revolutions per minute, the extrusion granulation temperature is 168 ℃, an extruder head is used for cooling granulation by wind, the length-width ratio of the prepared finished product feed particles is about 2.0-2.5 mm, and the excellent production stability of the feed with the external shape size can be ensured in the injection process;
(2) injection molding:
the obtained feed is used for injection molding on a die on a high-speed injection machine of a specially-made high-wear-resistant alloy screw barrel component, the set temperature of the die is 99 ℃, the set temperature of the injection is 186 ℃, the injection speed is 96%, and the injection pressure is 105MPa, so that a complete injection blank is finally obtained;
(3) catalytic degreasing:
putting the product into a catalytic degreasing furnace, introducing air to remove the POM binder carrier, and introducing N2Atmosphere protection is carried out on gas, the heating temperature of a hearth is set to be 120 ℃, the acid flow is 3.6 g per minute, the degreasing time is set to be 400min, and the degreasing rate is controlled to be more than 7.1%;
(4) and (3) sintering:
putting the obtained injection blank into a degreasing and sintering integrated furnace for sintering treatment, raising the temperature of room temperature to 600 ℃ at the rate of 2 ℃ per minute at the temperature of between 600 and 600 ℃, and carrying out N2The flow rate is 42L/min per minute, and the temperature is maintained for 180min, and the inert gas is N2The gas flow is 46L/min, the temperature is raised to 1080 ℃ at the rate of 3 ℃ per minute and is held for 60min after the temperature holding at 600 ℃ is finished, AR gas is introduced at the temperature raising rate of 3 ℃ per minute after the temperature holding at 1080 is finished to maintain the pressure in the furnace from 15KPa to 1358 ℃ and hold the temperature for 180min, the furnace is cooled to the room temperature after the temperature holding at 1358 ℃ is finished, and the whole sintering process is finished.
Example 3
A high flow high strength metal powder injection molding feed comprising an alloy powder and binder combination; the feeding binder system is a catalytic degreasing system, the alloy powder accounts for 90% of the feeding mass, and the binder combination accounts for 10% of the feeding mass; the binder combination comprises the following components in percentage by mass: 84% of polyformaldehyde, 6.5% of low-density polyethylene, 3.5% of rubber elastomer, 1% of paraffin, 1.5% of silicone oil, 1.5% of zinc stearate, 1.0% of antioxidant, 0.5% of formaldehyde curing agent and 0.5% of oleic acid.
The alloy powder is 17-4PH material powder atomized by water and gas of-800 meshes, the D50 particle size is about 7 microns, and the tap density of the powder is 4.7g/cm3(ii) a The element structure of the alloy powder is finely adjusted, and the content of nickel element and the content of chromium element are increased slightly on the existing material element system, so as to improve the corrosion resistance and the structural strength of the material; the content of alloy powder elements is as follows: 0.04% of carbon, 18% of chromium, 6% of nickel, 4% of copper, 0.5% of niobium, 0.5% of manganese and the balance of iron.
The proportioning design of the alloy powder elements improves the material performance of the product and obviously improves the corrosion resistance and the mechanical property of the product.
The application method of the high-fluidity high-strength metal powder injection molding feed comprises the following steps:
(1) mixing:
the preparation of the feed is carried out in an internal mixer-granulator, the temperature value of an internal mixing cavity is set to be 189 ℃, firstly, polyformaldehyde, low-density polyethylene and rubber elastomer are added into the cavity of the internal mixer to be stirred and melted, and the step aims to ensure that molecular chains of high polymer materials are fully fused with each other and contribute to the uniformity of a binder system; after the high molecular components are stirred and fused, adding metal alloy powder, stirring for about 5 minutes, and then adding paraffin, silicone oil, zinc stearate, an antioxidant and a formaldehyde curing agent, wherein the stirring speed is 45 revolutions per minute, and the step aims to fully wrap the low molecular lubricant on the surface of the powder, ensure that excellent lubrication effect is achieved among powder microparticles and promote the improvement of melt index; the antioxidant is added to improve the heat resistance stability of the high polymer material so as to ensure the stability of subsequent nozzle circulating materials; the formaldehyde curing agent is added to increase the strength of the main body framework adhesive and increase the strength and deformation resistance of the injection blank; and adding oleic acid after stirring and melting into mud, and finally uniformly stirring for 19 minutes, wherein the oleic acid has the functions of reducing the adhesion among the powder, improving the dispersibility of the feed and promoting the uniformity among the components of each binder and the powder. After banburying is finished, cooling the banburying cavity to 163 ℃, and starting extrusion granulation, wherein the rotation speed of a granulation screw is 130 revolutions per minute, the extrusion granulation temperature is 162 ℃, an extruder head is used for cooling granulation by air, the length-width ratio of the prepared finished product feed particles is about 2.0-2.5 mm, and the excellent production stability of the feed with the external shape and size can be ensured in the injection process;
(2) injection molding:
the obtained feed is used for injection molding on a die on a high-speed injection machine of a specially-made high-wear-resistant alloy screw barrel component, the set temperature of the die is 93 ℃, the set temperature of the injection is 188 ℃, the injection speed is 98 percent, and the injection pressure is 108MPa, so that a complete injection blank is finally obtained;
(3) catalytic degreasing:
putting the product into a catalytic degreasing furnace, introducing air to remove the POM binder carrier, and introducing N2Atmosphere protection is carried out on gas, the heating temperature of a hearth is set to be 120 ℃, the acid flow is 3.5 g/min, the degreasing time is set to be 420min, and the degreasing rate is controlled to be more than 7.2%;
(4) and (3) sintering:
putting the obtained injection blank into a degreasing and sintering integrated furnace for sintering treatment, raising the temperature of room temperature to 600 ℃ at the rate of 2 ℃ per minute at the temperature of between 600 and 600 ℃, and carrying out N2The flow rate is 43L/min per minute, and the temperature is maintained for 180min, and the inert gas is N2The gas flow is 41L/min, after the temperature holding at 600 ℃ is finished, the temperature is raised to 1090 ℃ at the rate of 3 ℃ per minute and is held for 60min in vacuum sintering, after the temperature holding at 1090 ℃ is finished, AR gas is introduced at the rate of 3 ℃ per minute to maintain the pressure in the furnace from 15KPa to 1355 ℃ for 180min, after the temperature holding at 1355 ℃ is finished, the furnace is cooled to the room temperature, and the whole sintering process is finished.
Example 4
A high flow high strength metal powder injection molding feed comprising an alloy powder and binder combination; the feeding binder system is a catalytic degreasing system, the alloy powder accounts for 90% of the feeding mass, and the binder combination accounts for 10% of the feeding mass; the binder combination comprises the following components in percentage by mass: 83% of polyformaldehyde, 3% of low-density polyethylene, 4% of rubber elastomer, 3.5% of paraffin, 2.0% of silicone oil, 1.0% of zinc stearate, 0.5% of antioxidant, 0.5% of formaldehyde curing agent and 2.5% of oleic acid.
The alloy powder is 17-4PH material powder atomized by water and gas of-800 meshes, the D50 particle size is about 7 microns, and the tap density of the powder is 4.7g/cm3(ii) a The element structure of the alloy powder is finely adjusted, and the content of nickel element and the content of chromium element are increased slightly on the existing material element system, so as to improve the corrosion resistance and the structural strength of the material; the content of alloy powder elements is as follows:0.04% of carbon, 18% of chromium, 6% of nickel, 4% of copper, 0.5% of niobium, 0.5% of manganese and the balance of iron.
The proportioning design of the alloy powder elements improves the material performance of the product and obviously improves the corrosion resistance and the mechanical property of the product.
The application method of the high-fluidity high-strength metal powder injection molding feed comprises the following steps:
(1) mixing:
the preparation method comprises the following steps of preparing a feed in an internal mixer-granulator, setting a temperature value of an internal mixing cavity to be 190 ℃, firstly adding polyformaldehyde, low-density polyethylene and a rubber elastomer into a cavity of the internal mixer for stirring and melting, wherein the purpose of the step is to fully fuse molecular chains of high polymer materials with each other and contribute to the uniformity of a binder system; after the high molecular components are stirred and fused, adding metal alloy powder, stirring for about 8 minutes, and then adding paraffin, silicone oil, zinc stearate, an antioxidant and a formaldehyde curing agent, wherein the stirring speed is 39 revolutions per minute, and the step aims to fully wrap the low molecular lubricant on the surface of the powder, ensure that excellent lubrication effect is achieved among powder microparticles and promote the improvement of melt index; the antioxidant is added to improve the heat resistance stability of the high polymer material so as to ensure the stability of subsequent nozzle circulating materials; the formaldehyde curing agent is added to increase the strength of the main body framework adhesive and increase the strength and deformation resistance of the injection blank; and adding oleic acid after stirring and melting into mud, and finally uniformly stirring for 25 minutes, wherein the oleic acid has the functions of reducing the adhesion among the powder, improving the dispersibility of the feed and promoting the uniformity among the components of each binder and the powder. After banburying is finished, the temperature of a banburying cavity is reduced to 170 ℃, extrusion granulation is started, the rotation speed of a granulation screw is 133 revolutions per minute, the extrusion granulation temperature is 168 ℃, an extruder head is used for cooling granulation by air, the length-width ratio of the prepared finished product feed particles is about 2.0-2.5 mm, and the excellent production stability of the feed with the external shape size can be ensured in the injection process;
(2) injection molding:
the obtained feed is used for injection molding on a die on a high-speed injection machine of a specially-made high-wear-resistant alloy screw barrel component, the set temperature of the die is 102 ℃, the set temperature of the injection is 190 ℃, the injection speed is 110%, and the injection pressure is 110MPa, so that a complete injection blank is finally obtained;
(3) catalytic degreasing:
putting the product into a catalytic degreasing furnace, introducing air to remove the POM binder carrier, and introducing N2Atmosphere protection is carried out on gas, the heating temperature of a hearth is set to be 120 ℃, the acid flow is 3.3 g/min, the degreasing time is set to be 410min, and the degreasing rate is controlled to be more than 7.2%;
(4) and (3) sintering:
putting the obtained injection blank into a degreasing and sintering integrated furnace for sintering treatment, raising the temperature of room temperature to 600 ℃ at the rate of 2 ℃ per minute at the temperature of between 600 and 600 ℃, and carrying out N2The flow rate is 44L/min per minute, and the temperature is maintained for 180min, and the inert gas is N2The gas flow is 47L/min, the temperature is raised to 1060 ℃ at the rate of 3 ℃ per minute after the temperature is held at 600 ℃ for 60min in vacuum sintering, AR gas is introduced at the rate of 3 ℃ per minute after the temperature is held at 1060 ℃ to maintain the pressure in the furnace from 15KPa to 1353 ℃ for 180min, the temperature is cooled to room temperature along with the furnace after the temperature is held at 1353 ℃, and the whole sintering process is finished.
The invention has the beneficial effects that:
(1) the invention selects the feeding powder and the binder system which are in a nearly spherical shape and have oxygen content lower than 500ppm, and through special design, the prepared alloy feeding has the physical property of the melt flow rate of more than or equal to 1800g/10min, and can realize the molding of ultrathin 0.15mm thin wall and 15mm thick structural products, and the content ratio of the special binder skeleton high polymer material is added, so that the feeding can mold the thin wall products with the ultrahigh melt flow rate, and simultaneously, the cycle use frequency of the water gap material generated by injection can reach 40 times of high-proportion cycle, and the material has high-strength structural support in the subsequent sintering process, the deformation difference can be controlled within 0.3 percent, and the product deformation caused by shrinkage in the sintering process is greatly reduced;
(2) the injection blank prepared by the invention has excellent physical properties, the tensile strength of the blank is 50MPa, the elongation at break is 5%, the bending strength is 45MPa, the thermal deformation temperature is 145 ℃, and the final firing is carried outThe sintered product has high-performance mechanical and physical properties, and the sintered density can reach 7.65g/cm3The hardness is higher than HV300, the salt spray test is more than 48 hours, the aging hardness can reach more than HRC38 through subsequent heat treatment, the performance has obvious advantages and competitiveness, and the use of the material in the field of high-requirement performance can be completely met.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the true spirit and scope of the invention.

Claims (4)

1. A high-fluidity high-strength metal powder injection molding feed is characterized by comprising alloy powder and a binder combination; according to the mass percentage, the alloy powder accounts for 90% of the feeding mass, and the binder combination accounts for 10% of the feeding mass; the binder combination comprises the following components in percentage by mass: 82 to 84 percent of polyformaldehyde, 3 to 6.5 percent of low-density polyethylene, 3.5 to 4.5 percent of rubber elastomer, 1 to 3.5 percent of paraffin, 1.5 to 2 percent of silicone oil, 0.5 to 1.5 percent of zinc stearate, 0.5 to 1 percent of antioxidant, 0.5 to 1 percent of formaldehyde curing agent and 0.5 to 2.5 percent of oleic acid, wherein the total amount of all the components is 100 percent.
2. The high-fluidity high-strength metal powder injection molding feed as claimed in claim 1, wherein the alloy powder is 17-4PH material powder atomized by water and gas combined with-800 meshes, the D50 particle size is 7 microns, and the tap density of the powder is 4.7g/cm3
3. A high flow, high strength metal powder injection molding feedstock as claimed in claim 2 wherein said alloy powder has elemental contents of: 0.04% of carbon, 18% of chromium, 6% of nickel, 4% of copper, 0.5% of niobium, 0.5% of manganese and the balance of iron.
4. The method of using a high flow, high strength metal powder injection molding feed as claimed in claim 1, comprising the steps of:
(1) mixing:
preparing a feed in an internal mixer-granulator integrated machine, setting a temperature value of an internal mixing cavity to be 185-190 ℃, firstly adding polyformaldehyde, low-density polyethylene and a rubber elastomer into the cavity of the internal mixer, and stirring and melting; then adding alloy powder, stirring for about 5-8 minutes, adding paraffin, silicone oil, zinc stearate, an antioxidant and a formaldehyde curing agent, stirring at the rotating speed of 39-65 revolutions per minute, stirring and melting to form mud, adding oleic acid, and finally uniformly stirring for 16-25 minutes; after banburying is finished, cooling the banburying cavity to 163-171 ℃, starting extrusion granulation, wherein the rotation speed of a granulation screw is 120-133 revolutions per minute, the extrusion granulation temperature is 162-168 ℃, and an extruder head cools granulation by using air to obtain a feed;
(2) injection molding:
the obtained feed is used for injection molding of a mold on a high-speed injection machine of a specially-made high-wear-resistant alloy screw barrel assembly, the set temperature of the mold is 93-102 ℃, the set temperature of injection is 185-190 ℃, the injection speed is 95-110%, and the injection pressure is 100-110 MPa, so that a complete injection blank is finally obtained;
(3) catalytic degreasing:
putting the product into a catalytic degreasing furnace, introducing air to remove the POM binder carrier, and introducing N2Atmosphere protection is carried out on the gas, the heating temperature of a hearth is set to be 120 ℃, the acid flow is 3.3-3.6 g per minute, the degreasing time is set to be 400-420 min, and the degreasing rate is controlled to be more than 7.1%;
(4) and (3) sintering:
putting the obtained injection blank into a degreasing and sintering integrated furnace for sintering treatment, raising the temperature of room temperature to 600 ℃ at the rate of 2 ℃ per minute at the temperature of between 600 and 600 ℃, and carrying out N2The flow rate is 40-44L/min per minute, then the temperature is kept for 180min, and the inert gas is N2The gas flow is 41-47L/min, after the 600 ℃ temperature is held, the temperature is raised to 1060-1100 ℃ in vacuum sintering at the rate of 3 ℃ per minute and held for 60min, after the 1060-1100 ℃ temperature is held, AR gas is introduced at the rate of 3 ℃ per minute to maintain the pressure in the furnace 1And (3) keeping the temperature for 180min at the temperature of between 5KPa and 1353 and 1360 ℃, cooling the mixture to room temperature along with the furnace after the temperature keeping at the temperature of between 1353 and 1360 ℃, and finishing the whole sintering process.
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