CN109014211B - Low-cost MIM (metal-insulator-metal) manufacturing process for high-nitrogen non-magnetic high-strength stainless steel part - Google Patents
Low-cost MIM (metal-insulator-metal) manufacturing process for high-nitrogen non-magnetic high-strength stainless steel part Download PDFInfo
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- CN109014211B CN109014211B CN201810903147.XA CN201810903147A CN109014211B CN 109014211 B CN109014211 B CN 109014211B CN 201810903147 A CN201810903147 A CN 201810903147A CN 109014211 B CN109014211 B CN 109014211B
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a low-cost MIM (metal-insulator-metal) manufacturing process of a high-nitrogen non-magnetic high-strength stainless steel part, which comprises the following steps: the preparation, forming, degreasing, sintering and solid solution processes of raw materials comprise: in the sintering step, the blank after catalytic degreasing is sintered and compacted by a vacuum batch furnace, the sintering process is sintering in a full-range nitrogen atmosphere, the nitrogen atmosphere sintering is mainly carried out in two steps, low-pressure sintering compaction is carried out firstly, and high-pressure nitriding is carried out later to ensure the performance; the low-pressure sintering nitrogen pressure is 10-30kpa, the inlet gas flow is 20-50L/min, the sintering temperature is 1150-1250 ℃, the heat preservation time is 90-360min, the high-pressure nitriding nitrogen pressure is 60-90kpa, the inlet gas flow is 20-50L/min, the sintering temperature is 1280-1320 ℃, and the heat preservation time is 90-120 min. The technical scheme of the invention realizes the feasibility of mass production of the self-made feed which is cheaper than the Basff feed, and solves the defects of poor dimensional stability and difficult performance guarantee when the self-made feed is produced in a large scale by adopting a conventional sintering process.
Description
Technical Field
The invention relates to a low-cost MIM (metal injection molding) manufacturing process of a high-nitrogen non-magnetic high-strength stainless steel part, in particular to a manufacturing process of a Fe17Cr11Mn3Mo material, belonging to the field of powder metallurgy and metal powder injection molding.
Background
The nickel-free high-nitrogen austenitic stainless steel is a new steel grade developed in the year by replacing nickel with nitrogen to stabilize an austenitic structure, the nitrogen content in the stainless steel is more than 0.4 wt.%, so that the mechanical property and the corrosion resistance of the steel are obviously improved, and the nickel-free component characteristics further solve the problem of nickel anaphylactic reaction of a human body caused when the traditional nickel-containing stainless steel is used as a wearing product or a human body implant, so that the nickel-free high-nitrogen austenitic stainless steel has wide development prospects in the fields of industry, biomedicine and the like.
The preparation method of the high-nitrogen stainless steel mainly comprises a high-pressure smelting method and a powder metallurgy method. Stainless steel prepared by a conventional smelting method has low nitrogen content, and high nitrogen content, high strength and high toughness can be obtained only by high-pressure smelting, but the high-pressure smelting method has complex equipment and large investment, and the development of the stainless steel is limited because the stainless steel passes through a ferrite phase region with the rapidly reduced nitrogen content during cooling according to a phase diagram smelting method. Compared with a smelting method, the powder metallurgy technology for producing the high-nitrogen steel is easier to obtain higher nitrogen content, and in addition, the technology is flexible, and the capital investment is low, so the powder metallurgy high-nitrogen steel becomes one of the most important directions in the current research of the high-nitrogen steel. The injection molding technology is used as a advanced powder metallurgy forming method, and high-performance parts with responsible shapes can be directly prepared.
The MIM-Fe17Cr11Mn3Mo material is the only choice of nonmagnetic (relative magnetic permeability <1.01), nickel-free and high-strength (yield strength >600MPa, microhardness HV >280) stainless steel in the MIM industry at present, and can be used for camera rings, mobile phone middle frames and the like with high strength requirements on double-sided glass mobile phones. The prior MIM manufacturers almost adopt a German Pasv feeding system and a technical scheme, so that the price is high (about 300 yuan/Kg), and the risk of overall poor products caused by raw material problems exists. If the self-made feed is used, the conventional process provided in the literature, particularly the sintering process, is adopted, the dimensional stability is extremely poor, and the level of mass production cannot be achieved.
Disclosure of Invention
The invention aims to provide a low-cost MIM (metal-insulator-metal) manufacturing process of a high-nitrogen non-magnetic high-strength stainless steel part, which aims to solve the problems in the prior art.
The purpose of the invention is realized by the following technical scheme.
A low-cost MIM manufacturing process of a high-nitrogen non-magnetic high-strength stainless steel part comprises the following steps:
s1, preparation of raw materials: adding domestic gas atomized non-magnetic nickel-free stainless steel powder and a binder into a kneader according to a certain ratio, kneading for 50-120min at the temperature of 165-195 ℃, and granulating for later use;
s2, forming: forming qualified injection blanks from the feed prepared in the step 1) on an injection machine according to a proper process, wherein the injection process comprises the following steps: the injection nozzle temperature is 160-210 ℃, the injection pressure is 40-120Mpa, and the mold temperature is 90-130 ℃;
s3, degreasing: nitric acid is needed to carry out catalytic degreasing before sintering the injection blank, and polyformaldehyde which accounts for a large proportion in the blank body is removed, wherein the catalytic degreasing process comprises the following steps: the temperature is 110 ℃ and 140 ℃, and the acid is introduced
3.5-4.8ml/min, and the acid introduction time is 1-4 hours;
s4, sintering: the blank after catalytic degreasing is sintered and compacted by a vacuum batch furnace, the sintering process is sintering in a full-range nitrogen atmosphere, the nitrogen atmosphere sintering is mainly carried out in two steps, low-pressure sintering is firstly carried out for compacting, and then high-pressure nitriding is carried out for ensuring the performance; the low-pressure sintering nitrogen pressure is 10-30kpa, the inlet gas flow is 20-50L/min, the sintering temperature is 1150-1250 ℃, the heat preservation time is 90-360min, the high-pressure nitriding nitrogen pressure is 60-90kpa, the inlet gas flow is 20-50L/min, the sintering temperature is 1280-1320 ℃, and the heat preservation time is 90-120 min. In the sintering process, after the heat preservation is finished, the nitrogen pressure is kept, and forced cooling is carried out when the temperature is cooled to a certain temperature.
S5, solid solution: and (3) carrying out solution treatment on the sintered part in the S4 in a vacuum furnace with a certain partial pressure of nitrogen protection, wherein the solution treatment process has the advantages that the solution temperature is higher than that of the conventional 17-4PH material, and the cooling speed is higher.
In S1, the domestic gas atomized non-magnetic nickel-free stainless steel powder has a granularity of-500 meshes, a D50 [ mu ] m or less than 13 mu ] m and a tap density>4.6g/cm3(ii) a The adhesive is a plastic-based adhesive system taking POM as a main raw material, and the components of the adhesive are 60-80wt.% of Polyformaldehyde (POM), 5-10wt.% of high-density polyethylene (HDPE), 10-20% of polypropylene (PP), a small amount of Stearic Acid (SA) and the like; the mass fraction of the binder in the feed is 5-10%. Preferably, its constituents are 60-80wt.% Polyoxymethylene (POM), 5-10wt.% High Density Polyethylene (HDPE), 10-20% polypropylene (PP), Stearic Acid (SA)2-5 wt.%; 2-5 wt.% of other auxiliaries.
In S4, nitrogen is introduced into the whole process, the temperature is raised from room temperature to 600 ℃ at the speed of 2.5 ℃/min, nitrogen is introduced into the mixture for negative pressure degreasing and presintering; heating to 1250 ℃ at the speed of 3-8 ℃/min at the temperature of 600 ℃, and preserving heat for 180min, wherein the nitrogen pressure in the process is 20 kpa; heating to 1250 ℃ at the speed of 2.5 ℃/min to 1300 ℃, preserving heat for 120min, and keeping the nitrogen pressure of 90kpa in the process; the nitrogen pressure was maintained while cooling.
In S5, in the solid solution process, the partial pressure of nitrogen is 60-90kpa, the solid solution temperature is 1150-1200 ℃, the heat preservation time is 60-120min, the cooling medium is nitrogen, and the cooling speed is more than 150K/min.
The technical scheme of the invention realizes the feasibility of mass production of the self-made feed which is cheaper than the Basff feed (the price of the self-made feed is about half of that of the Basff feed), and solves the defects of poor dimensional stability and difficult performance guarantee when the self-made feed is produced in a large scale by adopting a conventional sintering process. An innovative two-step sintering scheme is adopted, namely low-pressure sintering is firstly carried out to compact, then high-pressure nitriding is carried out to ensure the performance, the standard deviation of the size during full-furnace sintering can reach below 0.04, some can even reach 0.025 stability, and the full-furnace size fluctuation range of a product with the size of 30mm is only 0.15 mm.
Detailed Description
The technical features of the present invention will be further described with reference to the following embodiments.
Example 1:
the mobile phone camera ring produced by the technical scheme has the density of 7.6g/cm3Above, in ten thousand products in a full furnace, the standard deviation of the total length of 34mm is 0.03, the neutral salt spray test at 35 ℃ after solid solution is more than 48H, the relative magnetic conductivity is less than 1.01, the microhardness HV280-320, and the yield strength is 600-630 MPa.
The specific embodiment is as follows:
1) preparing a feed: domestic gas atomized-500-mesh Fe17Cr11Mn3Mo powder and a binder are kneaded and granulated on a kneading and extruding all-in-one machine according to the mass ratio of 92:8, wherein the content of each component in a binder system is as follows: polyoxymethylene (POM): high Density Polyethylene (HDPE): polypropylene (PP): stearic Acid (SA): other auxiliaries 70:5: 20: 2: 3.
2) and forming: forming qualified injection blanks from the feed prepared in the step 1) on an injection machine according to a proper process, wherein the injection process comprises the following steps: the nozzle temperature is 200 ℃, the injection pressure is 100Mpa, and the mold temperature is 120 ℃.
3) Degreasing: nitric acid is needed to carry out catalytic degreasing before sintering the injection blank, and polyformaldehyde which accounts for a large proportion in the blank body is removed, wherein the catalytic degreasing process comprises the following steps: the temperature is 110 ℃, the acid introducing amount is 3.5ml/min, and the acid introducing time is 2 hours.
4) And sintering: introducing nitrogen in the whole process, heating from room temperature to 600 ℃ at the speed of 2.5 ℃/min, degreasing by nitrogen negative pressure, and pre-sintering; heating to 1250 ℃ at the speed of 3-8 ℃/min at the temperature of 600 ℃, and preserving heat for 180min, wherein the nitrogen pressure in the process is 20 kpa; heating to 1250 ℃ at the speed of 2.5 ℃/min to 1300 ℃, preserving heat for 120min, and keeping the nitrogen pressure of 90kpa in the process; the nitrogen pressure was maintained while cooling.
5) Solid solution: and (3) carrying out solid solution treatment on the sintered part in a vacuum furnace under the protection of nitrogen, heating to 1275 ℃ at the speed of 3 ℃/min under the pressure of 70kpa of nitrogen, preserving heat for 2H, and rapidly cooling to room temperature under the pressure of 8bar of nitrogen.
Example 2:
in contrast to example 1, in step 1), the binder system, whose constituents are 60 wt.% Polyoxymethylene (POM), 10wt.% High Density Polyethylene (HDPE), 20% polypropylene (PP), 5% Stearic Acid (SA) and 5% other auxiliaries; the mass fraction of the binder in the feed is 8%.
Example 3:
the difference from example 1 is: in step 1), the binder system comprises 80wt.% of Polyoxymethylene (POM), 5 wt.% of High Density Polyethylene (HDPE), 10% of polypropylene (PP), 2% of Stearic Acid (SA) and 3% of other additives; the mass fraction of the binder in the feed is 8%.
Example 4:
the difference from example 1 is: in the step 4), nitrogen is introduced in the whole process, the temperature is raised from room temperature to 600 ℃ at the speed of 2.5 ℃/min, nitrogen is subjected to negative pressure degreasing and pre-sintering; heating to 1150 ℃ at the speed of 3-8 ℃/min at the temperature of 600 ℃, and keeping the temperature for 180min, wherein the nitrogen pressure in the process is 20 kpa; heating to 1300 deg.C at 1150 deg.C at 2.5 deg.C/min, maintaining the temperature for 120min, and maintaining the nitrogen pressure at 90 kpa; the nitrogen pressure was maintained while cooling.
Embodiments 2-4 the mobile phone camera ring produced by the technical scheme has the density of 7.6g/cm3Above, in ten thousand products in a full furnace, the standard deviation of the total length of 34mm is 0.03, the neutral salt spray test at 35 ℃ after solid solution is more than 48H, the relative magnetic conductivity is less than 1.01, the microhardness HV280-320, and the yield strength is 600-630 MPa.
Claims (5)
1. A low-cost MIM manufacturing process of a high-nitrogen non-magnetic high-strength stainless steel part is characterized in that: the method comprises the following steps:
s1, preparation of raw materials: adding domestic atomized Fe17Cr11Mn3Mo powder and a binder into a kneader according to a certain ratio, kneading for 50-120min at the temperature of 165-195 ℃, and granulating for later use;
s2, forming: forming qualified injection blanks from the feed prepared in the S1 on an injection machine according to a proper process, wherein the injection process comprises the following steps: the injection nozzle temperature is 160-210 ℃, the injection pressure is 40-120Mpa, and the mold temperature is 90-130 ℃;
s3, degreasing: before sintering, the injection blank needs nitric acid catalytic degreasing to remove polyformaldehyde which accounts for a large part in the injection blank, and the catalytic degreasing process comprises the following steps: the temperature is 110-;
s4, sintering: the blank after catalytic degreasing is sintered and compacted by a vacuum batch furnace, the sintering process is sintering in a full-range nitrogen atmosphere, the sintering in the nitrogen atmosphere is mainly carried out in two steps, low-pressure sintering is carried out for compacting, and high-pressure nitriding is carried out for ensuring the performance; the low-pressure sintering nitrogen pressure is 10-30kpa, the inlet gas flow is 20-50L/min, the sintering temperature is 1150-1250 ℃, the heat preservation time is 90-360min, the high-pressure nitriding nitrogen pressure is 60-90kpa, the inlet gas flow is 20-50L/min, the sintering temperature is 1280-1320 ℃, and the heat preservation time is 90-120 min; in the sintering process, after heat preservation is finished, the nitrogen pressure is kept, and forced cooling is carried out when the temperature is cooled to a certain temperature;
s5, solid solution: and (3) carrying out solution treatment on the sintered part in S4 in a vacuum furnace under the protection of nitrogen with a certain partial pressure, wherein the solution treatment comprises the following steps: the nitrogen partial pressure is 60-90kpa, the solid solution temperature is 1150-1200 ℃, the heat preservation time is 60-120min, the cooling medium is nitrogen, and the cooling speed is more than 150K/min.
2. The low-cost MIM manufacturing process of high-nitrogen non-magnetic high-strength stainless steel parts according to claim 1, characterized in that: in S1, the domestic atomized Fe17Cr11Mn3Mo powder has the particle size of-500 meshes, the D50 is less than or equal to 13 mu m, and the tap density is more than 4.6g/cm 3.
3. The low-cost MIM manufacturing process of high-nitrogen non-magnetic high-strength stainless steel parts according to claim 1, characterized in that: the adhesive is a plastic-based adhesive system taking POM as a main raw material, and the components of the adhesive are 60-80wt.% of Polyformaldehyde (POM), 5-10wt.% of high-density polyethylene (HDPE), 10-20% of polypropylene (PP) and a small amount of Stearic Acid (SA); the mass fraction of the binder in the feed is 5-10%.
4. The low-cost MIM manufacturing process of high-nitrogen non-magnetic high-strength stainless steel parts according to claim 3, characterized in that: the adhesive comprises 60-80wt.% of Polyformaldehyde (POM), 5-10wt.% of High Density Polyethylene (HDPE), 10-20 wt.% of polypropylene (PP), 2-5 wt.% of Stearic Acid (SA) and 2-5 wt.% of other additives.
5. The low-cost MIM manufacturing process of high-nitrogen non-magnetic high-strength stainless steel parts according to claim 1, characterized in that: in S4, nitrogen is introduced into the whole process, the temperature is raised from room temperature to 600 ℃ at the speed of 2.5 ℃/min, nitrogen is introduced into the mixture for negative pressure degreasing and presintering; heating to 1250 ℃ at the speed of 3-8 ℃/min at the temperature of 600 ℃, preserving heat for 180min, and keeping the nitrogen pressure of 20kpa in the low-pressure sintering process; heating to 1300 ℃ at 1250 ℃ at a speed of 2.5 ℃/min, preserving heat for 120min, and keeping the nitrogen pressure at 90kpa in the high-pressure nitriding process; the nitrogen pressure was maintained while cooling.
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