CN113337749A - Alloy porous material and preparation method thereof - Google Patents

Alloy porous material and preparation method thereof Download PDF

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Publication number
CN113337749A
CN113337749A CN202110571685.5A CN202110571685A CN113337749A CN 113337749 A CN113337749 A CN 113337749A CN 202110571685 A CN202110571685 A CN 202110571685A CN 113337749 A CN113337749 A CN 113337749A
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temperature
product
per minute
injection
porous material
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姜洪亮
苏来军
王茂堂
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Ningbo Furuihong Metal Material Co ltd
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Ningbo Furuihong Metal Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores
    • 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
    • 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
    • B22F3/1025—Removal of binder or filler not by heating only
    • 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
    • B22F3/11—Making porous workpieces or articles
    • 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
    • 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
    • B22F3/227—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 organic binder assisted extrusion
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten

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

Abstract

The invention discloses an alloy porous material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) feeding and mixing; (2) performing injection molding on the product; (3) catalytic degreasing; (4) vacuum degreasing and sintering; (5) and (5) surface passivation treatment. The invention can fully exert the advantages of the injection molding process in the aspect of structure molding, particularly can perfectly mold the alloy porous material in the aspect of special-shaped difficult structures such as high complex structures, ultrathin wall structures and the like, and has competitive advantages compared with the manufacturing processes of other industries.

Description

Alloy porous material and preparation method thereof
Technical Field
The invention relates to the technical field of metal powder injection molding, in particular to an alloy porous material and a preparation method thereof.
Background
The porous material product is an alloy material product with porosity, low specific gravity, large specific surface and excellent permeability, is mainly applied to the fields of filtration, energy absorption, noise reduction, conduction and the like, and the current manufacturing process mainly focuses on powder compression molding, casting molding, 3D printing and the like.
The market development trend of the current porous material products is developed towards the directions of high performance, high complex structuring, diversification of alloy materials and the like of materials, the traditional porous material production process can not meet the market demand in the aspect of realizing efficiency and performance requirements in certain novel application fields, and the demand of the porous material market needs to be met by expanding and combining other novel production processes.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the technical defects of the background technology and provides an alloy porous material and a preparation method thereof. The invention can fully exert the advantages of the injection molding process in the aspect of structure molding, particularly can perfectly mold the alloy porous material in the aspect of special-shaped difficult structures such as high complex structures, ultrathin wall structures and the like, and has competitive advantages compared with the manufacturing processes of other industries.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of an alloy porous material comprises the following steps:
(1) feeding and mixing:
the feeding material 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: 86-89% of POM, 4.5-7% of HDPE, 2-3% of EVA, 1.5-2% of microcrystalline wax, 1.5-3% of stearic acid and 0.5-1.0% of antioxidant, wherein the total amount of the components is 100%;
adding POM, HDPE and EVA into an internal mixing and granulating integrated machine, heating to 183-188 ℃, stirring for 13-16 min in a fusion state at a paddle rotating speed of 18-25 revolutions per minute, then adding alloy powder at a rotating speed of 43-46 revolutions per minute, stirring, adding microcrystalline wax, stearic acid and antioxidant, fully stirring for 25-32 min after feeding into mud, and then cooling, extruding and granulating to obtain a finished feed required by injection;
(2) and (3) product injection molding:
the product injection molding is carried out on a high-speed injection machine, and the injection temperature is set as follows: 196-199 ℃ of a nozzle, 193-196 ℃ of a first section, 188-195 ℃ of a second section, 182-185 ℃ of a third section, 178-182 ℃ of a fourth section, 170-176 ℃ of a fifth section, 83-91% of injection speed, 84-86 MPa of injection pressure, 38-41 MPa of pressure maintaining, 95-102 ℃ of set temperature of a mold and 1.0-1.8S of set injection time;
(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) vacuum degreasing and sintering:
the process is fully sintered at 1200 ℃ to complete densification of the material, and the sintering temperature rise curve is as follows: the temperature is raised at the rate of 3 ℃ per minute at the room temperature of 600 ℃ to 110-120 min, and the protective gas is N2The gas flow is 42-45L/min per minute, the temperature is raised to 1050 ℃ at the rate of 5 ℃ per minute after the temperature is maintained at 600 ℃, vacuum sintering is carried out, the temperature is maintained for 60-62 min, the temperature is raised to 1200 ℃ at the rate of 5 ℃ per minute after the temperature is maintained for 160-166 min, the pressure in the furnace is controlled at 15KPa, AR gas protective atmosphere is introduced, the gas flow is 25-26L/min per minute, the furnace is cooled to 80 ℃ after the temperature is maintained, and the whole process is finished;
(5) surface passivation treatment:
and cleaning the sintered product by using ultrasonic waves for 4-6 min, throwing, soaking in an environment-friendly passivation solution for passivation for 85-92 min, taking out the product after passivation, washing the product by using clear water, drying by spin, soaking in a sealing agent for 8-12 min, washing by using clear water after sealing treatment is finished, and drying in an oven at 120 ℃ for 20-22 min to finish the whole process.
Preferably, in the step (1), 316L powder with the powder particle size of 40 micrometers, 14 micrometers and 84.2 micrometers in total content of 1.8 wt% and the tap density of 4.57-4.63 g/cm and with the total content of 100 micrometers and 40-100 micrometers is adopted3Apparent density of4.08g/cm3And the water and gas combined atomized 316L alloy powder with the oxygen content of 520 ppm.
More preferably, the alloy powder has elemental contents of: -0.29% of oxygen, -18% of chromium, -0.79% of manganese, -0.023% of carbon, -0.004% of sulfur, -0.018% of phosphorus, -0.62% of silicon, -11% of nickel, -2.2% of molybdenum and the balance-iron.
Preferably, in the step (1), the antioxidant is an antioxidant 1010.
The alloy porous material is prepared by the preparation method of the alloy porous material.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention has the advantages that the high-efficiency forming can be realized quickly, conveniently and efficiently, compared with the traditional industries such as machining, pressing and the like, a large amount of manpower and material resource investment and cost are saved, and the cost can be reduced by about 30% in the aspect of cost control; in addition, the invention has the technical advantages that the injection feeding can be adjusted by selecting powder with different grain diameters and powder shapes in multiple ranges, so as to manufacture the porosity meeting the requirements of different products;
(2) the invention has flexible and changeable material options, can support the selection of different materials, and particularly can reduce the material and processing cost which can not be replaced by other processes because the process characteristic of the invention is net forming process in the aspect of high-hardness wear-resistant porous material;
(3) the invention can fully exert the advantages of the injection molding process in the aspect of structure molding, can perfectly mold products in the aspect of special-shaped difficult structures such as high complex structures, ultrathin wall structures and the like, and has competitive advantages compared with the manufacturing processes of other industries.
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 preparation method of an alloy porous material comprises the following steps:
(1) feeding and mixing:
the feeding material 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;
adopting 316L powder with the powder particle size of 40 micrometers, 14 weight percent of 100 micrometers and 84.2 weight percent of 40-100 micrometers in the total content of 1.8 weight percent and the tap density of 4.63g/cm3Apparent density of 4.08g/cm3316L alloy powder atomized by water and gas with 520ppm of oxygen content; the alloy powder comprises the following elements: -0.29% oxygen, -18% chromium, -0.79% manganese, -0.023% carbon, -0.004% sulfur, -0.018% phosphorus, -0.62% silicon, -11% nickel, -2.2% molybdenum, and the balance-iron;
the injection feeding binder system adopts a catalytic system, and the binder combination comprises the following components in percentage by mass: 89% of POM (polyoxymethylene), 5% of HDPE (high density polyethylene), 2% of EVA (acrylic resin), 2% of microcrystalline wax, 1.5% of SA (stearic acid) and 0.5% of antioxidant (1010);
firstly adding a binding agent POM, HDPE and EVA3 group item into an internal mixing and granulating integrated machine, heating to 185 ℃, stirring for 15min to obtain a fusion state, wherein the purpose of the step is to ensure that high molecular components are fully compatible and improve the uniformity of the binding agent, then adding 316L alloy powder, stirring for 45 min at a rotating speed, and adding a microcrystalline wax, SA and antioxidant binding agent group item, the purpose of the step is to reduce friction among powder particles of a low molecular lubricant, so as to improve the fluidity of the binding agent, stirring for 30min after feeding into mud, and then cooling, extruding and granulating to obtain a finished feed required by injection;
(2) and (3) product injection molding:
the product injection molding is carried out on a high-speed injection machine, and the injection temperature is set as follows: the injection nozzle is 198 ℃, the first section is 195 ℃, the second section is 190 ℃, the third section is 185 ℃, the fourth section is 180 ℃, the fifth section is 175 ℃, the injection speed is 90%, the injection pressure is 85MPa, the pressure is maintained at 40MPa, the set temperature of the mold is 100 ℃, and the injection time is set to be 1.0S;
(3) catalytic degreasing:
the process aims at removing the POM main body binder in the product, the removal aims at facilitating subsequent sintering, the product is fully shrunk and compact, the product is placed in a special catalytic degreasing furnace, air is fed to remove the POM binder carrier, and N is introduced2Atmosphere 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) vacuum degreasing and sintering:
the process is fully sintered at 1200 ℃ to complete densification of the material, and the sintering temperature rise curve is as follows: the temperature is increased at the rate of 3 ℃ per minute at the room temperature to 600 ℃ and is kept at 600 ℃ for 120min, and the protective gas is N2The gas flow is 45L/min per minute, the temperature is raised to 1050 ℃ at the rate of 5 ℃ per minute after the temperature holding at 600 ℃ is finished, the vacuum sintering is carried out, the temperature is held for 60min, the temperature is raised to 1200 ℃ at the rate of 5 ℃ per minute after the temperature holding is finished, the temperature is held for 160min, the pressure in the furnace is controlled at 15KPa, the AR gas protective atmosphere is introduced, the gas flow is 25L/min per minute, the temperature is cooled to 80 ℃ along with the furnace after the temperature holding is finished, and the whole process is finished. Note: the process is a key step for controlling the porosity and material performance of the porous material, and the set temperature of 1200 ℃ and the temperature of 160min are the optimal temperature points for determining the porosity of the product;
(5) surface passivation treatment:
cleaning the sintered product by ultrasonic waves for 5min, throwing to dry and soaking in an environment-friendly passivation solution for passivation for 90min, taking out the product after passivation, washing the product by clean water and drying the product by spin, soaking the product in a sealing agent for 10min, washing the product by clean water after sealing treatment is finished, and drying the product in an oven at 120 ℃ for 20min to finish the whole process.
Example 2
A preparation method of an alloy porous material comprises the following steps:
(1) feeding and mixing:
the feeding material 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 powder with the particle size of 1.8 wt% of 40 micrometers, 14 wt% of 100 micrometers and 84.2 wt% of 316L powder with the particle size of 40-100 micrometers is adopted, and the tap density is 4.58g/cm3Apparent density of 4.08g/cm3316L alloy powder atomized by water and gas with 520ppm of oxygen content; the alloy powder comprises the following elements: -0.29% oxygen, -18% chromium, -0.79% manganese, -0.023% carbon, -0.004% sulfur, -0.018% phosphorus, -0.62% silicon, -11% nickel, -2.2% molybdenum, and the balance-iron;
the injection feeding binder system adopts a catalytic system, and the binder combination comprises the following components in percentage by mass: 88% of POM (polyoxymethylene), 5.5% of HDPE (high density polyethylene), 3% of EVA (acrylic resin), 1.5% of microcrystalline wax, 1.5% of SA (stearic acid) and 0.5% of antioxidant (1010);
firstly adding a binding agent POM, HDPE and EVA3 group item into an internal mixing and granulating integrated machine, heating to 186 ℃, rotating speed of a paddle is 22 revolutions per minute, stirring for 15min to obtain a fusion state, aiming at fully compatibilizing high molecular components and improving uniformity of the binding agent, then adding 316L alloy powder, rotating speed is 46 revolutions per minute, stirring and adding a microcrystalline wax, SA and antioxidant binding agent group item, aiming at reducing friction of a low molecular lubricant among powder particles so as to improve fluidity of the binding agent, fully stirring for 30min after feeding and forming mud, and then cooling, extruding and granulating to obtain a finished feed required by injection;
(2) and (3) product injection molding:
the product injection molding is carried out on a high-speed injection machine, and the injection temperature is set as follows: 199 ℃ of a nozzle, 194 ℃ of a first section, 195 ℃ of a second section, 183 ℃ of a third section, 182 ℃ of a fourth section, 176 ℃ of a fifth section, 91% of injection speed, 86MPa of injection pressure, 38MPa of pressure maintaining, 98 ℃ of set temperature of a mold and 1.0S of set injection time;
(3) catalytic degreasing:
the process aims at removing the POM main body binder in the product, the removal aims at facilitating subsequent sintering, the knots are fully shrunk and compact, the product is placed into a special catalytic degreasing furnace, air is fed to remove the POM binder carrier, and N is introduced2Atmosphere 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) vacuum degreasing and sintering:
the process is fully sintered at 1200 ℃ to complete densification of the material, and the sintering temperature rise curve is as follows: the temperature is increased at the rate of 3 ℃ per minute at the room temperature to 600 ℃ and is kept at 600 ℃ for 120min, and the protective gas is N2The gas flow is 45L/min per minute, the temperature is raised to 1050 ℃ at the rate of 5 ℃ per minute after the temperature holding at 600 ℃ is finished, the vacuum sintering is carried out, the temperature is held for 60min, the temperature is raised to 1200 ℃ at the rate of 5 ℃ per minute after the temperature holding is finished, the temperature is held for 160min, the pressure in the furnace is controlled at 15KPa, the AR gas protective atmosphere is introduced, the gas flow is 25L/min per minute, the temperature is cooled to 80 ℃ along with the furnace after the temperature holding is finished, and the whole process is finished. Note: the process is a key step for controlling the porosity and material performance of the porous material, and the set temperature of 1200 ℃ and the temperature of 160min are the optimal temperature points for determining the porosity of the product;
(5) surface passivation treatment:
and cleaning the sintered product by ultrasonic waves for 5min, throwing to dry and soaking in an environment-friendly passivation solution for passivation for 90min, taking out the product after passivation, washing the product by clean water, drying the product by spin, soaking the product in a sealing agent for 10min, washing the product by clean water after sealing treatment is finished, and drying the product in an oven at 120 ℃ for 20min to finish the whole process.
Example 3
A preparation method of an alloy porous material comprises the following steps:
(1) feeding and mixing:
the feeding material 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 powder with the particle size of 1.8 wt% of 40 micrometers, 14 wt% of 100 micrometers and 84.2 wt% of 316L powder with the particle size of 40-100 micrometers is adopted, and the tap density is 4.59g/cm3Apparent density of 4.08g/cm3316L alloy powder atomized by water and gas with 520ppm of oxygen content; the alloy powder comprises the following elements: -0.29% oxygen, -18% chromium, -0.79% manganese, -0.023% carbon, -0.004% sulfur, -0.018% phosphorus, -0.62% silicon, -11% nickel, -2.2% molybdenum, and the balance-iron;
the injection feeding binder system adopts a catalytic system, and the binder combination comprises the following components in percentage by mass: 87% of POM (polyoxymethylene), 4.5% of HDPE (high density polyethylene), 2.5% of EVA (acrylic resin), 2% of microcrystalline wax, 3% of SA (stearic acid) and 1.0% of antioxidant (1010);
firstly adding a binding agent POM, HDPE and EVA3 group item into an internal mixing and granulating integrated machine, heating to 188 ℃, rotating speed of a paddle 25 r/min, stirring for 16min to obtain a fusion state, wherein the step aims to ensure that high molecular components are fully compatible to improve the uniformity of the binding agent, then adding 316L powder, rotating speed 46 r/min, stirring and adding a microcrystalline wax, SA and antioxidant binding agent group item, the step aims to reduce friction between powder particles of a low molecular lubricant, so as to improve the fluidity of the binding agent, stirring fully for 32min after feeding and forming mud, and then cooling, extruding and granulating to obtain a finished feed required by injection;
(2) and (3) product injection molding:
the product injection molding is carried out on a high-speed injection machine, and the injection temperature is set as follows: 197 ℃ of a nozzle, 196 ℃ of the first section, 191 ℃ of the second section, 183 ℃ of the third section, 182 ℃ of the fourth section, 172 ℃ of the fifth section, 85 percent of injection speed, 86MPa of injection pressure, 41MPa of pressure maintaining, 95 ℃ of set temperature of a mold and 1.5 seconds of set injection time;
(3) catalytic degreasing:
the process aims at removing the POM main body binder in the product, the removal aims at facilitating subsequent sintering, the product is fully shrunk and compact, the product is placed in a special catalytic degreasing furnace, air is fed to remove the POM binder carrier, and N is introduced2Atmosphere 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) vacuum degreasing and sintering:
the process is fully sintered at 1200 ℃ to complete densification of the material, and the sintering temperature rise curve is as follows: the temperature is increased at the rate of 3 ℃ per minute at the room temperature to 600 ℃ and is kept at 600 ℃ for 120min, and the protective gas is N2The gas flow is 42L/min per minute, the temperature is raised to 1050 ℃ at the rate of 5 ℃ per minute after the temperature holding at 600 ℃ is finished, the vacuum sintering is carried out, the temperature is held for 62min, the temperature is raised to 1200 ℃ at the rate of 5 ℃ per minute and the temperature is held for 165min after the temperature holding is finished, the pressure in the furnace is controlled at 15KPa, the AR gas protective atmosphere is introduced, the gas flow is 25L/min per minute, the temperature is cooled to 80 ℃ along with the furnace after the temperature holding is finished, and the whole process is finished. Note: the process is a key step for controlling the porosity and material performance of the porous material, and the set temperature of 1200 ℃ and the set temperature of 165min are the optimal temperature points for determining the porosity of the product;
(5) surface passivation treatment:
cleaning the sintered product with ultrasonic waves for 4min, throwing to dry and soaking in an environment-friendly passivation solution for passivation for 92min, taking out the product after passivation, washing the product with clear water and drying the product by spin drying, soaking the product in a sealing agent for 12min, washing the product with clear water after sealing treatment is finished, and drying the product in an oven at 120 ℃ for 22min to finish the whole process.
Example 4
A preparation method of an alloy porous material comprises the following steps:
(1) feeding and mixing:
the feeding material 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 powder with the particle size of 1.8 wt% of 40 micrometers, 14 wt% of 100 micrometers and 84.2 wt% of 316L powder with the particle size of 40-100 micrometers is adopted, and the tap density is 4.57g/cm3Apparent density of 4.08g/cm3316L alloy powder atomized by water and gas with 520ppm of oxygen content; the alloy powder comprises the following elements: -0.29% oxygen, -18% chromium, -0.79% manganese, -0.023% carbon, -0.004% sulfur, -0.018% phosphorus, -0.62% silicon, -11% nickel, -2.2% molybdenum, and the balance-iron;
the injection feeding binder system adopts a catalytic system, and the binder combination comprises the following components in percentage by mass: POM (polyoxymethylene) content of 86%, HDPE (high density polyethylene) content of 7%, EVA (acrylic resin) content of 3%, microcrystalline wax content of 2%, SA (stearic acid) content of 1.5%, antioxidant (1010) content of 0.5%;
firstly adding a binding agent POM, HDPE and EVA3 group item into an internal mixing and granulating integrated machine, heating to 183 ℃, stirring for 13min to be in a fusion state, wherein the purpose of the step is to ensure that high molecular components are fully compatible to improve the uniformity of the binding agent, then adding 316L powder, stirring for adding a microcrystalline wax, SA and antioxidant binding agent group item at a rotating speed of 43 rpm, and the purpose of the step is to reduce friction of a low molecular lubricant among powder particles so as to improve the fluidity of the binding agent, fully stirring for 25min after feeding and forming mud, and then cooling, extruding and granulating to obtain a finished product feed required by injection;
(2) and (3) product injection molding:
the product injection molding is carried out on a high-speed injection machine, and the injection temperature is set as follows: a nozzle is 196 ℃, a first section is 193 ℃, a second section is 188 ℃, a third section is 182 ℃, a fourth section is 178 ℃, a fifth section is 170 ℃, the injection speed is 83 percent, the injection pressure is 84MPa, the pressure is maintained at 39MPa, the set temperature of a mold is 102 ℃, and the injection time is set to be 1.8S;
(3) catalytic degreasing:
the process aims at removing the POM main body binder in the product, the removal aims at facilitating subsequent sintering, the product is fully shrunk and compact, the product is placed in a special catalytic degreasing furnace, air is fed to remove the POM binder carrier, and N is introduced2Atmosphere 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) vacuum degreasing and sintering:
the process is fully sintered at 1200 ℃ to complete densification of the material, and the sintering temperature rise curve is as follows: the temperature is increased at the rate of 3 ℃ per minute at the room temperature to 600 ℃, and the temperature is maintained at 600 ℃ for 110min, and the protective gas is N2The gas flow is 43L/min per minute, the temperature is raised to 1050 ℃ at the rate of 5 ℃ per minute after the temperature holding at 600 ℃ is finished, the vacuum sintering is carried out, the temperature is held for 60min, the temperature is raised to 1200 ℃ at the rate of 5 ℃ per minute after the temperature holding is finished, the temperature is held for 166min, the pressure in the furnace is controlled at 15KPa, the AR gas protective atmosphere is introduced, the gas flow is 26L/min per minute, the temperature is cooled to 80 ℃ along with the furnace after the temperature holding is finished, and the whole process is finished. Note: the process is a key step for controlling the porosity and material performance of the porous material, and the set temperature of 1200 ℃ and the set temperature of 166min are the optimal temperature points for determining the porosity of the product;
(5) surface passivation treatment:
and cleaning the sintered product by ultrasonic waves for 6min, soaking the sintered product in an environment-friendly passivation solution for passivation for 85min, taking out the product after passivation, washing the product by clean water, drying the product by spin, soaking the product in a sealing agent for 8min, washing the product by clean water after sealing treatment is finished, and drying the product in an oven for 22min at 120 ℃ to finish the whole process.
The invention has the following technical effects:
(1) the present invention has the advantage of extending from conventional plastic injection moldingThe powder metal injection molding is carried out, plastic serves as a powder carrier to enable the powder to have rheological property, then the molding is carried out quickly through a mold, the molding of an ultrathin-wall structural part with the thickness of 0.18mm can be achieved, the molding of a product with an ultrathin-wall structure with the wall thickness of 60mm can be achieved, the molding of a product with a complex 3D structure can be achieved, then the product with the required pore space of 0.02-0.1 mm can be prepared according to the requirements of different porous material products through the selectable particle size of the powder, and the product can be controlled to be at the lowest density of 5.2g/cm3Maximum density of 7.5g/cm3And has the capability of producing large-batch and high-quality porous material products;
(2) the invention can prepare the circular porous filter nozzle head with the matrix porosity of 0.05mm, the length of 23.4mm, the diameter of 16.6mm and the wall thickness of 1.5 mm.
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 (5)

1. The preparation method of the alloy porous material is characterized by comprising the following steps of:
(1) feeding and mixing:
the feeding material 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: 86-89% of POM, 4.5-7% of HDPE, 2-3% of EVA, 1.5-2% of microcrystalline wax, 1.5-3% of stearic acid and 0.5-1.0% of antioxidant, wherein the total amount of the components is 100%;
adding POM, HDPE and EVA into an internal mixing and granulating integrated machine, heating to 183-188 ℃, stirring for 13-16 min in a fusion state at a paddle rotating speed of 18-25 revolutions per minute, then adding alloy powder at a rotating speed of 43-46 revolutions per minute, stirring, adding microcrystalline wax, stearic acid and antioxidant, fully stirring for 25-32 min after feeding into mud, and then cooling, extruding and granulating to obtain a finished feed required by injection;
(2) and (3) product injection molding:
the product injection molding is carried out on a high-speed injection machine, and the injection temperature is set as follows: 196-199 ℃ of a nozzle, 193-196 ℃ of a first section, 188-195 ℃ of a second section, 182-185 ℃ of a third section, 178-182 ℃ of a fourth section, 170-176 ℃ of a fifth section, 83-91% of injection speed, 84-86 MPa of injection pressure, 38-41 MPa of pressure maintaining, 95-102 ℃ of set temperature of a mold and 1.0-1.8S of set injection time;
(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) vacuum degreasing and sintering:
the process is fully sintered at 1200 ℃ to complete densification of the material, and the sintering temperature rise curve is as follows: the temperature is raised at the rate of 3 ℃ per minute at the room temperature of 600 ℃ to 110-120 min, and the protective gas is N2The gas flow is 42-45L/min per minute, the temperature is raised to 1050 ℃ at the rate of 5 ℃ per minute after the temperature is maintained at 600 ℃, vacuum sintering is carried out, the temperature is maintained for 60-62 min, the temperature is raised to 1200 ℃ at the rate of 5 ℃ per minute after the temperature is maintained for 160-166 min, the pressure in the furnace is controlled at 15KPa, AR gas protective atmosphere is introduced, the gas flow is 25-26L/min per minute, the furnace is cooled to 80 ℃ after the temperature is maintained, and the whole process is finished;
(5) surface passivation treatment:
and cleaning the sintered product by using ultrasonic waves for 4-6 min, throwing, soaking in an environment-friendly passivation solution for passivation for 85-92 min, taking out the product after passivation, washing the product by using clear water, drying by spin, soaking in a sealing agent for 8-12 min, washing by using clear water after sealing treatment is finished, and drying in an oven at 120 ℃ for 20-22 min to finish the whole process.
2. The method for preparing an alloy porous material according to claim 1, wherein the step of(1) In the method, 316L powder with the particle size of 40 micrometers, 14 weight percent of 100 micrometers and 84.2 weight percent of 40-100 micrometers in the total content of 1.8 weight percent and the tap density of 4.57-4.63 g/cm is adopted3Apparent density of 4.08g/cm3And the water and gas combined atomized 316L alloy powder with the oxygen content of 520 ppm.
3. The method for preparing an alloy porous material according to claim 2, wherein the contents of the alloy powder elements are as follows: -0.29% of oxygen, -18% of chromium, -0.79% of manganese, -0.023% of carbon, -0.004% of sulfur, -0.018% of phosphorus, -0.62% of silicon, -11% of nickel, -2.2% of molybdenum and the balance-iron.
4. The method for preparing the porous alloy material according to claim 1, wherein in the step (1), the antioxidant is 1010.
5. An alloy porous material, which is prepared by the preparation method of the alloy porous material as claimed in any one of claims 1 to 4.
CN202110571685.5A 2021-05-25 2021-05-25 Alloy porous material and preparation method thereof Pending CN113337749A (en)

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Application publication date: 20210903