CN115740427A - MIM powder of 1800MPa grade ultrahigh-strength high-toughness steel and MIM forming process - Google Patents
MIM powder of 1800MPa grade ultrahigh-strength high-toughness steel and MIM forming process Download PDFInfo
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- CN115740427A CN115740427A CN202211523867.6A CN202211523867A CN115740427A CN 115740427 A CN115740427 A CN 115740427A CN 202211523867 A CN202211523867 A CN 202211523867A CN 115740427 A CN115740427 A CN 115740427A
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 64
- 239000010959 steel Substances 0.000 title claims abstract description 64
- 239000000843 powder Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 39
- 230000008569 process Effects 0.000 title claims abstract description 38
- 238000005245 sintering Methods 0.000 claims abstract description 66
- 238000005238 degreasing Methods 0.000 claims abstract description 57
- 239000002184 metal Substances 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 41
- 238000001816 cooling Methods 0.000 claims description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 230000003197 catalytic effect Effects 0.000 claims description 25
- 238000002347 injection Methods 0.000 claims description 18
- 239000007924 injection Substances 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000006104 solid solution Substances 0.000 claims description 17
- 230000032683 aging Effects 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 238000005261 decarburization Methods 0.000 claims description 13
- 239000011230 binding agent Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
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- 239000002826 coolant Substances 0.000 claims description 9
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- 238000004898 kneading Methods 0.000 claims description 7
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000001746 injection moulding Methods 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 10
- 238000000465 moulding Methods 0.000 abstract description 3
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- 239000000463 material Substances 0.000 description 14
- 229910000734 martensite Inorganic materials 0.000 description 11
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- 238000004519 manufacturing process Methods 0.000 description 9
- -1 polyoxymethylene Polymers 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000004698 Polyethylene Substances 0.000 description 7
- 229920000573 polyethylene Polymers 0.000 description 7
- 229920006324 polyoxymethylene Polymers 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
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- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910001240 Maraging steel Inorganic materials 0.000 description 1
- 229910000797 Ultra-high-strength steel Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
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- 229920003023 plastic Polymers 0.000 description 1
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- 230000002035 prolonged effect Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- 239000013585 weight reducing agent Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention belongs to the technical field of metal powder injection molding, and particularly relates to MIM powder of 1800 MPa-grade ultrahigh-strength high-toughness steel and an MIM molding process. The MIM powder consists of the following metal powders in percentage by weight: 0.0-0.6% of C, 2.0-3.5% of Cr, 11.0-14.0% of Ni, 14.0-17.0% of Co, 1.5-2.5% of Mo and the balance of Fe and impurities, wherein the grain diameter of the MIM powder is less than or equal to 50 mu m. According to the MIM forming process, the raw material components and the thermal degreasing and sintering processes are improved, so that the ultrahigh-strength high-toughness steel part with the yield strength of more than or equal to 1800MPa, the elongation of more than or equal to 5% and the hardness of 52-58 HRC is prepared.
Description
Technical Field
The invention belongs to the technical field of metal powder injection molding, and particularly relates to MIM powder of 1800 MPa-grade ultrahigh-strength high-toughness steel and an MIM molding process.
Background
With the continuous upgrading of the functional requirements of consumers on the mobile intelligent terminal, the folding screen mobile phone becomes a new growth point of the intelligent mobile phone. The folding screen scheme can well give consideration to the contradiction between a large screen and a small body, and endows the smart phone with a trendy appearance and richer use experience. However, the weight of the folding screen mobile phone is heavier than that of the traditional mobile phone, so that the portability of the mobile phone is reduced to a certain extent, and the user experience is influenced. Under the condition of not influencing the functions of the folding screen mobile phone, the adoption of a hinge which is more precise, lighter and thinner and has high strength is one of important ways for realizing the weight reduction of the folding screen mobile phone. At present, the 17-4PH and 420W stainless steels commonly used for the hinge of the folding screen mobile phone are limited by the ultimate strength of the materials, and the requirements of thinning and strengthening the hinge are difficult to meet. Therefore, it is urgently needed to develop an ultra-high strength and high toughness steel with high strength, high toughness and good fatigue resistance, which is used for manufacturing a high-precision hinge and achieves the effect of reducing the weight of a folding screen mobile phone.
The Metal Powder Injection Molding (MIM) technology is a novel Powder metallurgy Molding technology formed by introducing the modern plastic Injection technology into the Powder metallurgy field. The MIM technology utilizes a mold to injection mold a blank and rapidly manufacture parts with high precision and complex three-dimensional shapes through sintering, is particularly suitable for mass production and can be widely applied to the production of folding screen mobile phone hinge parts.
At present, the metal parts formed by the MIM technology are difficult to meet the requirements of ultrahigh strength and high toughness at the same time. The Chinese patent with application number of 202010154524.1 discloses an injection molding method of high-strength and high-toughness metal parts, which comprises the following components of 17.0-18.0% of Ni, 8.5-9.5% of Co, 4.5-5% of Mo and the balance of Fe, wherein the yield strength is only 1350MPa and the elongation is 6% after sintering and heat treatment; the Chinese invention patent with application number of 202010852638.3 discloses an injection molding ultrahigh strength steel, which comprises the following material components of less than 0.1% of C, 15.5-19.5% of Ni, 7.0-10.0% of Co, 4.0-6.0% of Mo, less than 1.5% of Ti and the balance of Fe, wherein although the yield strength can reach 1500MPa, the elongation rate is only 6% at most, and the elongation rate is reduced along with the improvement of the yield strength; the Chinese invention patent with application number 202010200648.9 discloses an MIM process for corrosion-resistant steel complex parts, the material components are C less than 0.1%, cr 11.0-15.0%, ni10.0-14.0%, mo 0.5-2.0%, si less than 0.5%, mn less than 0.5%, ti 1.0-4.0%, and the balance Fe, the elongation of the heat-treated material is 12-13%, but the yield strength only reaches 1500MPa; the Chinese patent application No. 201410248360.3 discloses a method for injection molding of high-strength maraging steel by metal powder, which comprises the following components of less than or equal to 0.08% of C, 17.0-19.0% of Ni, 8.0-10.0% of Co, 4.5-6.5% of Mo and the balance of Fe and inevitable impurities, wherein although the elongation is more than or equal to 10%, the strength is still low, and only the tensile strength can reach 1500MPa.
Therefore, the MIM forming process of the ultrahigh-strength high-toughness steel part with the yield strength of more than or equal to 1800MPa and the elongation of more than or equal to 5% is developed, the MIM forming process is used for manufacturing the metal part with ultrahigh strength, high toughness and complex three-dimensional shape, the requirements of industries such as 3C, tools, automobiles and the like on high-performance parts are met, and the MIM forming process has important technical and economic significance.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the MIM powder of the 1800MPa grade ultrahigh-strength high-toughness steel and the MIM forming process.
In order to solve the technical problems, the invention adopts the technical scheme that: MIM powder of 1800MPa grade ultrahigh-strength high-toughness steel comprises the following metal powder in percentage by weight: 0.0-0.6% of C, 2.0-3.5% of Cr2, 11.0-14.0% of Ni, 14.0-17.0% of Co and 1.5-2.5% of Mo, wherein the grain diameter of the MIM powder is less than or equal to 50 mu m.
The other technical scheme of the invention is as follows: an MIM forming process of 1800 MPa-level ultrahigh-strength high-toughness steel comprises the following steps:
s1: kneading the MIM powder and an adhesive to prepare a feed, and then crushing and/or granulating the feed;
s2: the feed after crushing and/or granulation is molded into a green body by injection molding;
s3: carrying out catalytic degreasing on the green body;
s4: sequentially carrying out thermal degreasing, deoxidation, decarburization and sintering on the green body subjected to catalytic degreasing in an inert gas atmosphere of 0-50 kPa to obtain a sintered piece;
s5: and sequentially carrying out solid solution treatment, subzero treatment and aging treatment on the sintered piece to obtain the ultrahigh-strength high-toughness steel.
The invention has the beneficial effects that: according to the MIM forming process of the 1800 MPa-level ultrahigh-strength high-toughness steel part, the ultrahigh-strength high-toughness steel part with the yield strength of more than or equal to 1800MPa, the elongation of more than or equal to 5% and the hardness of 52-58 HRC is prepared by improving the raw material components and the hot degreasing and sintering processes. The process has the characteristics of simplicity, convenience, economy and high efficiency, and can be used for manufacturing metal parts with ultrahigh strength, high toughness and high hardness and three-dimensional complex shapes in a large scale in a short time. The strength and the hardness of the ultrahigh-strength high-toughness steel part are obviously higher than those of the steel part prepared by the existing MIM process, so that the ultrahigh-strength high-toughness steel part can meet the requirements of industries such as 3C, tools, automobiles and the like on high-performance parts, and is particularly suitable for mass production of metal parts with complex three-dimensional shapes and high performance requirements.
Detailed Description
The following description will be given with reference to the embodiments in order to explain the technical contents, the objects and the effects of the present invention in detail.
The most key concept of the invention is as follows: by improving the raw material components and the hot degreasing and sintering processes, the ultrahigh-strength high-toughness steel part with the yield strength of more than or equal to 1800MPa, the elongation of more than or equal to 5 percent and the hardness of 52-58 HRC is prepared.
The invention relates to an MIM powder of 1800MPa grade ultrahigh strength high toughness steel, which comprises the following metal powder in percentage by weight: 0.0 to 0.6 percent of C, 2.0 to 3.5 percent of Cr, 11.0 to 14.0 percent of Ni, 14.0 to 17.0 percent of Co and 1.5 to 2.5 percent of Mo, and the grain diameter of the MIM powder is less than or equal to 50 mu m.
From the above description, the beneficial effects of the present invention are: co in the MIM powder is an element for improving the strength of steel, and can improve the strength of steel through the synergistic effect with Mo, but has little contribution to toughness; ni is an element for improving the toughness of steel, but Ni element can reduce Ms point of steel and is not beneficial to forming full martensite; therefore, the adoption of Co and Ni metals in a specific ratio is a precondition for ensuring high strength and high toughness of the steel.
Further, the metal powder comprises the following metal powder in percentage by weight: 0.1 to 0.4 percent of C, 2.0 to 3.5 percent of Cr, 11.0 to 13.0 percent of Ni, 15.0 to 17.0 percent of Co and 1.5 to 2.0 percent of Mo, and the grain diameter of the MIM powder is less than or equal to 25 mu m.
From the above description, it can be seen that the strength, toughness and hardness of the resulting steel part can be further improved by more precise control of the individual elements in the raw material composition.
Further comprises 0-2.02 wt% of impurities and the balance of iron.
Further, the weight of each element in the impurities accounts for the weight of the MIM powder as follows: mn is less than or equal to 1.0 percent, si is less than or equal to 1.0 percent, S is less than or equal to 0.01 percent and P is less than or equal to 0.01 percent.
The other technical scheme of the invention is as follows: an MIM forming process of 1800 MPa-level ultrahigh-strength high-toughness steel comprises the following steps:
s1: kneading the MIM powder and the adhesive to prepare a feed, and then crushing and/or granulating the feed;
s2: the feed after crushing and/or granulation is molded into a green body by injection molding;
s3: carrying out catalytic degreasing on the green body;
s4: sequentially carrying out thermal degreasing, deoxidation, decarburization and sintering on the green body subjected to catalytic degreasing in an inert gas atmosphere of 0-50 kPa to obtain a sintered piece;
s5: and (3) sequentially carrying out solid solution treatment, cryogenic treatment and aging treatment on the sintered piece to obtain the ultrahigh-strength high-toughness steel.
From the above description, the beneficial effects of the present invention are: according to the MIM (metal-insulator-metal) forming process of the ultrahigh-strength high-toughness steel part, provided by the invention, a green body is prepared by adopting raw material components in a specific proportion, and then catalytic degreasing, thermal degreasing, deoxidation and decarburization, sintering, solid solution treatment, cryogenic treatment and aging treatment are sequentially carried out, so that components in the alloy can be uniformly dissolved in a matrix to form a uniform solid solution, the effect of improving the elongation is achieved, the ultrahigh-strength high-toughness steel with the yield strength of not less than 1800MPa, the elongation of not less than 5% and the hardness of 52-58 HRC is obtained, the requirements of industries such as 3C, tools, automobiles, aerospace and the like on ultrahigh-strength and wear-resistant parts can be met, and the MIM forming process has the advantages of high production efficiency, low cost, good size consistency and the like.
The catalytic degreasing before sintering can remove most of the binder in the green body, and prevent the green body from cracking, bulging, deforming or collapsing in the sintering process. The metal powder is in the inert atmosphere, so that the metal powder can be prevented from reacting with oxygen in the air to be oxidized.
Further, the thermal degreasing comprises the following specific steps: raising the ambient temperature from room temperature to 250-350 ℃ at a temperature raising rate of 0.1-10 ℃/min, and keeping the temperature for 0-180 min; continuously heating to 400-500 ℃ at the heating rate of 0.1-10 ℃/min, and keeping the temperature for 0-180 min; continuously heating to 550-800 ℃ at the heating rate of 0.1-10 ℃/min, and keeping the temperature for 0-180 min.
From the above description, the high temperature treatment at 500-800 ℃ in the thermal degreasing can decompose the residual binder after the catalytic degreasing by heating, and avoid the binder residue from being cracked into carbon and oxygen in the subsequent high temperature treatment to affect the final performance of the material.
The thermal degreasing is carried out in the inert atmosphere, so that the metal powder can be prevented from reacting with oxygen in the air and being oxidized.
The heating rate in the thermal degreasing process is too low, so that the thermal degreasing time is prolonged, and the thermal degreasing efficiency is reduced; too fast heating rate can lead to severe decomposition and volatilization of the binder, generation of cracks, bulges and other defects, and carbonization of the binder without removal.
The low temperature of the hot degreasing leads to incomplete removal of the binder in the degreased blank, and leads to high carbon content of the material; the high temperature of the thermal degreasing causes the violent decomposition and volatilization of low molecular weight components in the adhesive, and the defects of cracks, bulges and the like are easy to generate.
Further, the specific steps of deoxidation and decarburization are as follows: controlling the gas pressure in the furnace to be less than 10Pa, raising the ambient temperature from 500-800 ℃ to 900-1200 ℃ at the temperature raising rate of 0.1-8 ℃/min, and then preserving the temperature for 10-240 min.
As can be seen from the above description, some oxygen is inevitably present in the metal powder, which is an impurity element in the steel, and is not beneficial to sintering densification and reduces the strength and toughness of the steel, and the removal of oxygen mainly depends on the reaction of carbon and oxygen to generate CO during the sintering process, and the CO is removed in a gas form; carbon in the material is an important strengthening element, and excessive carbon content can cause precipitation of a large amount of carbide at the grain boundary of steel, thereby having adverse effect on the toughness of the steel; too low a carbon content can reduce the strength of the material; therefore, it is necessary to perform the deoxidation and decarburization treatment while controlling the carbon content in the steel material to a suitable range.
Further, the sintering comprises the following specific steps: raising the ambient temperature from 900-1200 ℃ to 1320-1380 ℃ at a temperature raising rate of 0.1-10 ℃/min, then preserving the heat for 30-360 min, and cooling to the room temperature to obtain the sintered piece.
As can be seen from the above description, the sintering temperature is too low and the material fails to densify; the sintering temperature is too high, and the material is over-sintered or fused. The temperature rise rate in the sintering process is too slow, so that the sintering efficiency is reduced; the temperature rise rate is too high, so that air holes in the degreased blank cannot be discharged in time, sintering is not compact, the porosity is increased, and the material performance is influenced.
Further, the solid solution treatment comprises the following specific steps: placing the sintered part in a vacuum environment, preserving heat for 10-180 min at 950-1150 ℃, and then cooling to room temperature, wherein the cooling medium is nitrogen and/or argon, and the cooling rate is more than or equal to 50 ℃/min. The pressure of the cooling medium is 100 to 1000kPa.
As is apparent from the above description, the solution treatment, the cryogenic treatment and the aging treatment are key steps for forming martensite, martensitic transformation and carbide precipitation; the proper temperature and heat preservation time in the solution treatment are matched with rapid cooling, so that the components in the alloy can be uniformly dissolved in the matrix to form uniform solid solution, and the effect of improving the elongation is achieved. The solid solution treatment has requirements on gas pressure in a cooling stage, the higher the gas pressure is, the faster the cooling rate is, and the structure of steel is more uniform.
Further, the cryogenic treatment comprises the following specific steps: and (3) placing the workpiece subjected to the solution treatment at-196 to-150 ℃ for heat preservation for 10 to 180min, and then placing the workpiece in air to heat to room temperature.
As can be seen from the above description, the temperature and the holding time in the cryogenic treatment are suitable, so that the martensite transformation is complete, the reverse transformation austenite is inhibited from forming, the ultrafine carbide is precipitated on the martensite matrix, the structure uniformity is improved, and the full martensite structure of the steel after the cryogenic treatment is ensured.
Further, the aging treatment comprises the following specific steps: and (3) placing the workpiece subjected to cryogenic treatment in a vacuum environment, preserving the heat for 30-960 min at 460-550 ℃, and then cooling to room temperature.
From the above description, the appropriate temperature and holding time in the aging treatment enable carbide to be precipitated, and further improve the hardness, strength and toughness of the material.
Further, the volume ratio of the MIM powder to the binder is 1.30 to 1.85. Preferably, the volume ratio of the MIM powder to the binder is 1. More preferably, the volume ratio of the MIM powder to the binder is 1.59 to 1.65.
From the above description, it can be seen that the addition of the binder can improve the rheological properties of the feedstock while ensuring smooth release of the green body from the mold.
Further, the adhesive comprises, by weight, 80-90% of polyoxymethylene, 5-10% of polyethylene and 0-15% of a compatibilizer.
Further, the adhesive consists of the following components in percentage by weight: 80-90% of polyformaldehyde, 5-10% of polyethylene, 0-4% of paraffin and 3-10% of compatilizer.
The first embodiment of the invention is as follows:
an MIM forming process of 1800 MPa-level ultrahigh-strength high-toughness steel comprises the following steps:
s1: selecting raw materials, wherein the MIM powder consists of the following metal powders in percentage by weight: 0.3% of C, 2.5% of Cr2, 12.5% of Ni, 15.5% of Co, 1.8% of Mo, 0.3% of Mn, 0.2% of Si, 0.002% of S, 0.001% of P and the balance of Fe, wherein the grain diameter of MIN powder is less than or equal to 30 mu m;
the adhesive consists of the following components: 87% of polyoxymethylene, 8% of polyethylene, 3% of paraffin and the balance stearic acid.
S2: adding the MIM powder and the adhesive into an internal mixer according to the volume ratio of 1.60, kneading to prepare a feed, and then granulating the feed;
s3: the granulated feed is injection molded into a green body through an injection molding machine and a mold; the injection temperature is 190 ℃, the screw rotation speed is 60r/min, and the injection pressure is 200MPa.
S4: putting the green body into a degreasing furnace, and performing catalytic degreasing by using nitric acid; the temperature of the catalytic degreasing is 100 ℃, the time is 8h, and the acid passing amount is 4g/min.
S5: placing the green body after catalytic degreasing in a sintering furnace for negative pressure degreasing, introducing argon gas with the flow rate of 40L/min, heating the temperature in the sintering furnace from room temperature to 300 ℃ at the heating rate of 2 ℃/min, and keeping the temperature for 60min; heating the temperature in the sintering furnace from 300 ℃ to 450 ℃ at the heating rate of 1.5 ℃/min, and keeping the temperature for 60min; and (3) raising the temperature in the sintering furnace from 450 ℃ to 600 ℃ at the temperature raising rate of 1 ℃/min, and preserving the temperature for 60min to finish the thermal degreasing.
S6, keeping the pressure in the sintering furnace to be less than 10Pa, raising the temperature in the sintering furnace from 600 ℃ to 1150 ℃ at the temperature raising rate of 4 ℃/min, and then preserving the temperature for 60min to finish the deoxidation and decarburization.
S7: keeping the pressure of argon in the sintering furnace at 20kPa, raising the temperature in the sintering furnace from 1150 ℃ to 1360 ℃ at a temperature raising rate of 5 ℃/min, then preserving the heat for 180min, then cooling to room temperature, and completing sintering to obtain a sintered part.
S8: under the vacuum condition, the sintered piece is kept at 1000 ℃ for 60min, and then is cooled to room temperature, the cooling medium is argon with the pressure of 800kPa, the cooling rate is 300 ℃/min, and the solid solution treatment is completed.
S9: and (3) placing the workpiece subjected to the solution treatment in liquid nitrogen at the temperature of-150 ℃, preserving heat for 60min, taking out, then placing in air, heating to room temperature, and completing the cryogenic treatment.
S10: and (3) under a vacuum condition, preserving the temperature of the workpiece subjected to cryogenic treatment at 480 ℃ for 120min, then cooling to room temperature, and finishing aging treatment to obtain the ultrahigh-strength high-toughness steel part.
The ultrahigh-strength high-toughness steel part has the tensile strength of 2180MPa, the yield strength of 1850MPa, the elongation of 6 percent (the test reference standard GB/T228.1-2010) and the hardness of 57 HRC.
The second embodiment of the invention is as follows:
an MIM forming process of 1800 MPa-level ultrahigh-strength high-toughness steel comprises the following steps:
s1: selecting raw materials, wherein the MIM powder consists of the following metal powders in percentage by weight: 0.15% of C, 2.0% of Cr, 11.5% of Ni, 17.0% of Co, 2.5% of Mo, 0.1% of Mn, 0.3% of Si, 0.005% of S, 0.005% of P and the balance of Fe, wherein the grain diameter of the MIM powder is less than or equal to 25 mu m.
The adhesive consists of the following components: 90% of polyformaldehyde, 7% of polyethylene and the balance of ethylene-vinyl acetate copolymer.
S2: adding the MIM powder and the adhesive into an internal mixer according to the volume ratio of 1.85 to knead to prepare a feed, and crushing the feed.
S3: the crushed feed is injection molded into a green body through an injection molding machine and a mold; the injection temperature is 195 ℃, the screw rotation speed is 80r/min, and the injection pressure is 220MPa.
S4: putting the green body into a degreasing furnace, and performing catalytic degreasing by using nitric acid; the temperature of the catalytic degreasing is 110 ℃, the time is 10h, and the acid passing amount is 2.5g/min.
S5: placing the green body after catalytic degreasing in a sintering furnace for negative pressure degreasing, introducing nitrogen with the flow rate of 50L/min, heating the temperature in the sintering furnace from room temperature to 300 ℃ at the heating rate of 5 ℃/min, and preserving the temperature for 20min; heating the temperature in the sintering furnace from 300 ℃ to 450 ℃ at the heating rate of 1 ℃/min, and preserving the temperature for 20min; and (3) raising the temperature in the sintering furnace from 450 ℃ to 800 ℃ at the temperature raising rate of 0.5 ℃/min, and preserving the temperature for 20min to finish the thermal degreasing.
S6, keeping the pressure in the sintering furnace to be less than 10Pa, raising the temperature in the sintering furnace from 500 ℃ to 1050 ℃ at a temperature raising rate of 1.5 ℃/min, and then preserving the heat for 10min to finish the deoxidation and decarburization.
S7: keeping the pressure of argon in the sintering furnace at 10kPa, raising the temperature in the sintering furnace from 1050 ℃ to 1340 ℃ at a raising rate of 1.5 ℃/min, then preserving the heat for 360min, then cooling to room temperature, and completing sintering to obtain a sintered part.
S8: and (3) in vacuum, preserving the temperature of the sintered part at 1050 ℃ for 60min, and then cooling to room temperature, wherein the cooling medium is nitrogen with the pressure of 400kPa, and the cooling rate is 100 ℃/min, thus completing the solid solution treatment.
S9: and (3) placing the workpiece subjected to the solution treatment in liquid nitrogen at the temperature of-196 ℃, preserving heat for 10min, taking out, then placing in air, and heating to room temperature to complete the cryogenic treatment.
S10: and (3) preserving the temperature of the cryogenic-treated workpiece at 470 ℃ for 240min in vacuum, cooling to room temperature, and finishing aging treatment to obtain the ultrahigh-strength high-toughness steel part.
The ultrahigh-strength high-toughness steel part has the tensile strength of 2260MPa, the yield strength of 1895MPa, the elongation of 5.5% (test reference standard GB/T228.1-2010) and the hardness of 58 HRC.
The third embodiment of the invention is as follows:
an MIM forming process of 1800 MPa-level ultrahigh-strength high-toughness steel comprises the following steps:
s1: selecting raw materials, wherein the MIM powder consists of the following metal powders in percentage by weight: 0.6% of C, 3.5% of Cr3, 11.0% of Ni, 14.0% of Co, 1.5% of Mo, 1.0% of Mn, 0.02% of Si, 0.01% of S, 0.01% of P and the balance of Fe, wherein the grain diameter of the MIM powder is less than or equal to 20 mu m.
The adhesive consists of the following components: 90% of polyformaldehyde, 5% of polyethylene, 3% of ethylene-vinyl acetate copolymer and 2% of paraffin wax.
S2: adding the MIM powder and the adhesive into an internal mixer according to the volume ratio of 1.30, kneading to prepare a feed, and then crushing and granulating the feed in sequence.
S3: the granulated feed is injection molded into a green body through an injection molding machine and a mold; the injection temperature is 185 ℃, the screw rotation speed is 50r/min, and the injection pressure is 240MPa.
S4: putting the green body into a degreasing furnace, and performing catalytic degreasing by using nitric acid; the temperature of catalytic degreasing is 120 ℃, the time is 6h, and the acid passing amount is 3g/min.
S5: placing the green body after catalytic degreasing in a sintering furnace for negative pressure degreasing, introducing nitrogen with the flow of 30L/min, heating the temperature in the sintering furnace from room temperature to 300 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 60min; heating the temperature in the sintering furnace from 300 ℃ to 450 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 60min; and (3) raising the temperature in the sintering furnace from 450 ℃ to 800 ℃ at the temperature raising rate of 2 ℃/min, and preserving the temperature for 60min to finish the thermal degreasing.
S6, keeping the pressure in the sintering furnace to be less than 10Pa, heating the temperature in the sintering furnace from 800 ℃ to 950 ℃ at the heating rate of 1 ℃/min, and then preserving the temperature for 240min to finish the deoxidation and decarburization.
S7: keeping the pressure of argon in the sintering furnace at 20kPa, raising the temperature in the sintering furnace from 900 ℃ to 1350 ℃ at the temperature raising rate of 5 ℃/min, then preserving the temperature for 180min, then cooling to room temperature, and completing sintering to obtain a sintered piece.
S8: and (3) in vacuum, preserving the temperature of the sintered part at 1150 ℃ for 30min, and then cooling to room temperature, wherein the cooling medium is 1000kPa argon, and the cooling rate is 300 ℃/min, so that the solid solution treatment is completed.
S9: and (3) placing the workpiece subjected to the solution treatment in liquid nitrogen at the temperature of-150 ℃, preserving heat for 180min, taking out, then placing in air, heating to room temperature, and completing the cryogenic treatment.
S10: and (3) keeping the temperature of the subzero-treated workpiece at 550 ℃ for 30min in vacuum, cooling to room temperature, and finishing aging treatment to obtain the ultrahigh-strength high-toughness steel part.
The ultrahigh-strength high-toughness steel part has the tensile strength of 2230MPa, the yield strength of 1920MPa, the elongation of 6.0 percent (the test reference standard GB/T228.1-2010) and the hardness of 57 HRC.
The fourth embodiment of the invention is as follows:
an MIM forming process of 1800 MPa-level ultrahigh-strength high-toughness steel comprises the following steps:
s1: selecting raw materials, wherein the MIM powder consists of the following metal powders in percentage by weight: 0.0% of C, 3.0% of Cr3, 14.0% of Ni, 16.5% of Co, 2.0% of Mo, 0.05% of Mn, 1.0% of Si, 0.001% of S, 0.001% of P and the balance of Fe, wherein the grain diameter of the MIM powder is less than or equal to 50 mu m.
The adhesive consists of the following components in percentage by weight: 86% of polyformaldehyde, 7% of polyethylene, 4% of zinc stearate and 3% of paraffin.
S2: adding the MIM powder and the adhesive into an internal mixer according to the volume ratio of 1.70, kneading to prepare a feed, and crushing the feed.
S3: the crushed feed is injection molded into a green body through an injection molding machine and a mold; the injection temperature is 195 ℃, the screw rotation speed is 80r/min, and the injection pressure is 220MPa.
S4: putting the green body into a degreasing furnace, and performing catalytic degreasing by using nitric acid; the temperature of the catalytic degreasing is 110 ℃, the time is 10h, and the acid passing amount is 6g/min.
S5: placing the green body after catalytic degreasing in a sintering furnace for negative pressure degreasing, introducing argon gas, wherein the flow rate of the argon gas is 50L/min, and heating the temperature in the sintering furnace from room temperature to 350 ℃ at the heating rate of 0.1 ℃/min; raising the temperature in the sintering furnace from 350 ℃ to 500 ℃ at a temperature raising rate of 3 ℃/min; the temperature in the sintering furnace is increased from 500 ℃ to 800 ℃ at the heating rate of 0.1 ℃/min, and the thermal degreasing is completed.
S6, keeping the pressure in the sintering furnace to be less than 10Pa, heating the temperature in the sintering furnace from 800 ℃ to 900 ℃ at the heating rate of 1 ℃/min, and then preserving the heat for 10min to finish the deoxidation and decarburization.
S7: keeping the pressure of argon in the sintering furnace at 10kPa, heating the temperature in the sintering furnace from 900 ℃ to 1320 ℃ at the heating rate of 2 ℃/min, then preserving the heat for 360min, then cooling to room temperature, and completing sintering to obtain a sintered piece.
S8: and (3) preserving the temperature of the sintered part at 950 ℃ for 180min in vacuum, and then cooling to room temperature, wherein the cooling medium is nitrogen with the pressure of 100kPa, and the cooling rate is 50 ℃/min, thus completing the solid solution treatment.
S9: and (3) placing the workpiece subjected to the solution treatment in liquid nitrogen at the temperature of-180 ℃, preserving heat for 90min, taking out, then placing in air, heating to room temperature, and completing the cryogenic treatment.
S10: and (3) keeping the temperature of the subzero-treated workpiece at 460 ℃ for 960min in vacuum, cooling to room temperature, and finishing aging treatment to obtain the ultrahigh-strength high-toughness steel part.
The ultra-high strength and high toughness steel part has the tensile strength of 2165MPa, the yield strength of 1840MPa, the elongation of 7.3 percent (the test reference standard GB/T228.1-2010) and the hardness of 52 HRC.
The fifth embodiment of the invention is as follows:
an MIM forming process of 1800 MPa-level ultrahigh-strength high-toughness steel comprises the following steps:
s1: selecting raw materials, wherein the MIM powder consists of the following metal powders in percentage by weight: 0.2% of C, 2.8% of Cr2, 13.0% of Ni, 16.0% of Co, 2.2% of Mo, 0.05% of Mn, 0.05% of Si, 0.008% of S, 0.002% of P and the balance of Fe, wherein the grain diameter of the MIM powder is less than or equal to 20 mu m.
The adhesive consists of the following components in percentage by weight: 80% of polyformaldehyde, 10% of polyethylene, 4% of ethylene-vinyl acetate copolymer, 4% of stearic acid and 2% of paraffin wax.
S2: adding the MIM powder and the adhesive into an internal mixer according to the volume ratio of 1.59, kneading to prepare a feed, and then crushing and granulating the feed in sequence.
S3: the granulated feed is injection molded into a green body through an injection molding machine and a mold; the injection temperature is 185 ℃, the screw rotation speed is 50r/min, and the injection pressure is 240MPa.
S4: putting the green body into a degreasing furnace, and performing catalytic degreasing by using nitric acid; the temperature of catalytic degreasing is 120 ℃, the time is 6h, and the acid passing amount is 3g/min.
S5: placing the green body after catalytic degreasing in a sintering furnace for negative pressure degreasing, introducing argon gas with the flow of 30L/min, heating the temperature in the sintering furnace from room temperature to 250 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 180min; heating the temperature in the sintering furnace from 250 ℃ to 400 ℃ at the heating rate of 8 ℃/min, and keeping the temperature for 180min; and (3) raising the temperature in the sintering furnace from 400 ℃ to 550 ℃ at a temperature raising rate of 3 ℃/min, and preserving the temperature for 180min to finish the thermal degreasing.
S6, keeping the pressure in the sintering furnace to be less than 10Pa, raising the temperature in the sintering furnace from 550 ℃ to 1200 ℃ at a temperature rise rate of 1 ℃/min, and then preserving the temperature for 240min to finish the deoxidation and decarburization.
S7: keeping the pressure of argon in the sintering furnace at 50kPa, raising the temperature in the sintering furnace from 1200 ℃ to 1380 ℃ at the temperature rise rate of 1 ℃/min, then preserving the heat for 30min, then cooling to room temperature, and completing sintering to obtain a sintered piece.
S8: and (3) in vacuum, preserving the temperature of the sintered part at 1150 ℃ for 10min, and then cooling to room temperature, wherein the cooling medium is 1000kPa argon, and the cooling rate is 300 ℃/min, so that the solid solution treatment is completed.
S9: and (3) placing the workpiece subjected to the solution treatment in liquid nitrogen at the temperature of 170 ℃ below zero, preserving the heat for 180min, taking out the workpiece, and then placing the workpiece in air to heat to room temperature to complete the cryogenic treatment.
S10: and (3) preserving the temperature of the workpiece subjected to the cryogenic treatment at 550 ℃ for 30min in vacuum, cooling to room temperature, and finishing aging treatment to obtain the ultrahigh-strength high-toughness steel part.
The ultrahigh-strength high-toughness steel part has the tensile strength of 2205MPa, the yield strength of 1875MPa, the elongation of 5.2 percent (the test reference standard GB/T228.1-2010) and the hardness of 55.8 HRC.
The first comparative example of the present invention is:
the difference between the first comparative example and the first example is that: the weight percentage of Ni in the MIM powder is 10%, and the weight percentage of Co in the MIM powder is 18%. The obtained part has the tensile strength of 2010MPa, the yield strength of 1850MPa, the elongation of 1.5% (test reference GB/T228.1-2010) and the hardness of 59HRC.
The second comparative example of the present invention is:
the difference between the second comparative example and the first example is that: the weight percentage of Ni in the MIM powder is 18%, and the weight percentage of Co in the MIM powder is 10%. The tensile strength of the obtained part is 930MPa, the yield strength is 650MPa, the elongation is 25.0% (test reference standard GB/T228.1-2010), and the hardness is 30HRC.
In conclusion, according to the MIM forming process of the ultrahigh-strength high-toughness steel part, a green body is prepared by adopting Co and Ni metals in a specific ratio, and then catalytic degreasing, thermal degreasing, deoxidation and decarburization, sintering, solid solution treatment, cryogenic treatment and aging treatment are sequentially carried out, so that the ultrahigh-strength high-toughness steel with the yield strength of more than or equal to 1800MPa, the elongation of more than or equal to 5 percent and the hardness of 52-58 HRC can meet the requirements of industries such as 3C, tools, automobiles, aerospace and the like on ultrahigh-strength high-toughness and wear-resistant parts, and has the advantages of high production efficiency, low cost, good size consistency and the like.
Wherein, the solid solution treatment, the cryogenic treatment and the aging treatment are key steps for forming martensite, martensite phase transformation and carbide precipitation; the solid solution treatment can ensure that the components in the alloy can be uniformly dissolved in the matrix to form a uniform solid solution, and the effect of improving the elongation is achieved. The cryogenic treatment enables the martensite to be completely transformed, simultaneously inhibits the formation of reverse transformation austenite, precipitates ultrafine carbide on a martensite matrix, improves the uniformity of the structure and ensures that the steel obtains a full martensite structure after the cryogenic treatment. The aging treatment makes the carbide precipitate, and further improves the hardness, strength and toughness of the material.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical fields are included in the scope of the present invention.
Claims (10)
1. The MIM powder of 1800MPa grade ultrahigh strength high toughness steel is characterized by comprising the following metal powder in percentage by weight: 0.0-0.6% of C, 2.0-3.5% of Cr, 11.0-14.0% of Ni, 14.0-17.0% of Co and 1.5-2.5% of Mo, and the grain diameter of the MIM powder is less than or equal to 50 mu m.
2. The MIM powder of 1800MPa grade ultra-high strength and high toughness steel according to claim 1, further comprising 0-2.02 wt% of impurities and the balance iron.
3. An MIM forming process of 1800 MPa-level ultrahigh-strength high-toughness steel is characterized by comprising the following steps of:
s1: kneading the MIM powder of claim 1 or 2 with a binder to prepare a feed, and then crushing and/or granulating the feed;
s2: the feed after crushing and/or granulation is molded into green bodies by injection;
s3: carrying out catalytic degreasing on the green body;
s4: sequentially carrying out thermal degreasing, deoxidation, decarburization and sintering on the green blank subjected to catalytic degreasing in an atmosphere of inert gas of 0-50 kPa to obtain a sintered piece;
s5: and sequentially carrying out solid solution treatment, subzero treatment and aging treatment on the sintered piece to obtain the ultrahigh-strength high-toughness steel.
4. The MIM forming process of 1800MPa grade ultra-high strength and high toughness steel according to claim 3, wherein the specific steps of the thermal degreasing are as follows: raising the ambient temperature from room temperature to 250-350 ℃ at a temperature raising rate of 0.1-10 ℃/min, and keeping the temperature for 0-180 min; continuously heating to 400-500 ℃ at the heating rate of 0.1-10 ℃/min, and keeping the temperature for 0-180 min; continuously heating to 550-800 ℃ at the heating rate of 0.1-10 ℃/min, and keeping the temperature for 0-180 min.
5. The MIM forming process of 1800MPa grade ultra-high strength and high toughness steel according to claim 3, wherein the specific steps of deoxidation and decarburization are as follows: controlling the gas pressure in the furnace to be less than 10Pa, raising the ambient temperature from 500-800 ℃ to 900-1200 ℃ at the temperature raising rate of 0.1-8 ℃/min, and then preserving the temperature for 10-240 min.
6. The MIM forming process of 1800MPa grade ultra-high strength and high toughness steel according to claim 3, wherein the sintering comprises the following steps: raising the ambient temperature from 900-1200 ℃ to 1320-1380 ℃ at a temperature raising rate of 0.1-10 ℃/min, then preserving the heat for 30-360 min, and cooling to the room temperature to obtain the sintered piece.
7. The MIM forming process for the 1800MPa grade ultra-high strength and high toughness steel according to claim 3, wherein the solution treatment comprises the following specific steps: placing the sintered part in a vacuum environment, preserving heat for 10-180 min at 950-1150 ℃, and then cooling to room temperature, wherein the cooling medium is nitrogen and/or argon, and the cooling rate is more than or equal to 50 ℃/min. The pressure of the cooling medium is 100 to 1000kPa.
8. The MIM forming process of 1800MPa grade ultra-high strength and high toughness steel according to claim 3, wherein the cryogenic treatment comprises the following specific steps: and (3) placing the workpiece subjected to the solution treatment at-196 to-150 ℃ for heat preservation for 10 to 180min, and then placing the workpiece in air to heat to room temperature.
9. The MIM forming process for the 1800MPa grade ultra-high strength and high toughness steel according to claim 3, wherein the aging treatment comprises the following specific steps: and (3) placing the work piece subjected to cryogenic treatment in a vacuum environment, preserving the heat for 30-960 min at 460-550 ℃, and then cooling to room temperature.
10. The MIM forming process for 1800 MPa-level ultrahigh-strength high-toughness steel according to claim 3, wherein the volume ratio of the MIM powder to the binder is 1.30.
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