CN111299600A - Method for producing tool steel powder for 3D printing - Google Patents

Method for producing tool steel powder for 3D printing Download PDF

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Publication number
CN111299600A
CN111299600A CN202010156628.6A CN202010156628A CN111299600A CN 111299600 A CN111299600 A CN 111299600A CN 202010156628 A CN202010156628 A CN 202010156628A CN 111299600 A CN111299600 A CN 111299600A
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gas
nitrogen
tool steel
carbon dioxide
powder
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CN202010156628.6A
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Chinese (zh)
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陈俊孚
吴苏州
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Shenzhen Jinglai New Material Technology Co ltd
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Shenzhen Jinglai New Material Technology Co ltd
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Priority to CN202010156628.6A priority Critical patent/CN111299600A/en
Publication of CN111299600A publication Critical patent/CN111299600A/en
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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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • 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
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • 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
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
    • 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
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • 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
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Nanotechnology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The application provides a method for producing tool steel powder for 3D printing by using mixed gas of carbon dioxide and nitrogen as atomizing gas, which comprises five parts of raw material preparation, off-site gas mixing, gas pressurization, atomization and computer control. The invention uses the mixed gas of carbon dioxide and nitrogen to replace nitrogen as atomization and cooling gas, thereby reducing the nitrogen increase of powder. Meanwhile, the density of carbon dioxide is far greater than that of nitrogen, the outlet kinetic energy of atomized airflow can be improved under the same condition, the atomization of metal particles is facilitated, the one-time yield of atomized tool steel metal powder with the granularity smaller than 20 microns is not less than 50%, the sphericity is not less than 95%, and the development of the tool steel metal powder for 3D printing in China is promoted.

Description

Method for producing tool steel powder for 3D printing
Technical Field
The invention belongs to the field of metal 3D printing, and particularly relates to a preparation method for producing tool steel metal powder for 3D printing by using mixed gas of carbon dioxide and argon as atomizing gas.
Background
The application of the 3D printing technology in the mold, particularly the application in the mold conformal cooling system is one of the most mature fields in the current metal 3D printing business, the tool steel powder can be used for printing a front mold core, a rear mold core, an insert, a slide block, a guide pillar, a hot runner water jacket and the like of an injection mold, and the tool steel powder has the advantages of reducing the molding period, improving the product quality, enabling the temperature field of the mold to be more uniform and the like.
The raw material of tool steel powder belongs to low-carbon martensite age hardening type plastic die steel, and the alloy elements with the time-effect hardening effect in the steel are titanium, aluminum, cobalt and molybdenum. The impurities have obvious influence on the performance of the maraging steel and have more obvious influence on the steel with higher yield strength. This requires that the steel be vacuum smelted to reduce impurities, segregation and gas content in the steel ingot, so as to ensure that the material has good toughness and fatigue resistance.
At present, nitrogen is mostly used as atomizing gas for producing the tool steel powder for 3D printing, but the nitrogen is completely used as the atomizing gas to easily cause nitrogen increase of the tool steel 3D printing powder, so that the toughness of a printed formed part is reduced. Meanwhile, the density of the nitrogen is slightly smaller than that of the air, and the kinetic energy of the nitrogen due to the impact of the outlet is related to the speed and the mass of the gas. The outlet velocity and the volume of the provided impact gas are kept the same, and the gas with high density has better impact kinetic energy. The density of carbon dioxide gas is far higher than that of nitrogen gas, the impact kinetic energy is far higher than that of nitrogen gas, and the impact effect is better than that of nitrogen gas; and as a greenhouse gas, the carbon dioxide gas is utilized to meet the national requirements of energy conservation and emission reduction. However, since carbon dioxide has a certain weak oxidizing property, the mixing ratio of carbon dioxide and nitrogen and the outlet pressure need to be precisely controlled in order to prevent the powder from generating an oxygen increasing phenomenon.
Disclosure of Invention
The invention provides a method for producing tool steel powder for 3D printing by using a mixed gas of carbon dioxide and nitrogen as an atomizing and cooling gas, which solves the problem of nitrogen increase in the production of the tool steel powder for 3D printing by using nitrogen at present, and can also utilize carbon dioxide gas to play a role in energy conservation and emission reduction.
A method for producing tool steel 3D printing powder using a mixed gas of carbon dioxide gas and nitrogen gas as an atomizing gas, comprising the steps of:
the method for producing the tool steel powder comprises five parts of raw material preparation, off-site gas mixing, gas pressurization and atomization and a computer control system,
the preparation of the raw materials comprises the steps of selecting a tool steel bar produced by a billet caster as a raw material, wherein the nitrogen content of the raw material is less than or equal to 70ppm, and the mass fraction of the carbon content is 0.02-0.03%; removing an oxide rust layer on the surface of the tool steel bar by using a polishing method, and cutting the tool steel bar into small sections of 30-50 cm;
the off-site gas mixing comprises the steps of vacuumizing a 100L gas mixing tank to 70-100 pa, introducing nitrogen into the gas mixing tank from the lower part of the gas mixing tank, switching a valve, and introducing purchased liquid carbon dioxide gas from the upper part of the gas mixing tank, wherein the filling proportion of the carbon dioxide gas is less than or equal to 25% (volume fraction). After the nitrogen and the carbon dioxide are mixed, standing in a gas mixing tank for 3-5 minutes to ensure that the gases are uniformly mixed;
and the gas pressurization comprises the step that the mixed gas enters a gas booster pump through a pipeline in a gas mixing tank, and the booster pump increases the pressure of the mixed gas to 2.5-5 MPa.
The atomization and cooling process comprises the steps that pressurized gas is sprayed out through a spray head, metal liquid drops are smashed, metal powder is obtained, and an atomization tower is filled with the metal powder to serve as cooling and protecting gas.
The computer control system comprises a gas mixing system for adding nitrogen and carbon dioxide gas to the computer, so that the automatic operation and the monitoring of the gas flow are facilitated.
Drawings
FIG. 1 is a schematic view showing a carbon dioxide gas and nitrogen gas mixing apparatus in operation of the present application;
FIG. 2 is a control diagram of a nitrogen and carbon dioxide gas mixing system added to a control panel;
FIG. 3 is a microstructure diagram of the powder produced in example 1;
FIG. 4 is a microstructure diagram of the powder produced in example 2;
FIG. 5 is a microstructure diagram of the powder produced in example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples, which are illustrative only and are not intended to limit the present invention.
Example 1:
the tool steel having the composition shown in Table 1 was used, and it was required to select a tool steel bar produced by a billet caster as a raw material. Removing the oxide rust layer on the surface of the raw material by using a polishing method, cutting the raw material into small sections of 30-50 cm, putting the small sections into vacuum atomization powder spraying equipment, setting the power to be 20kw, and heating to ensure that the raw material is completely melted.
TABLE 1 raw materials chemical composition table (%)
C Ti Mn P S Co Mo Ni N
0.02 0.6 ≤0.10 ≤0.01 ≤0.01 8.5 4.6 18 70ppm
Vacuumizing a 100L gas mixing tank to be below 100pa, introducing nitrogen into the gas mixing tank, switching a valve, and introducing purchased liquid carbon dioxide gas into the gas mixing tank, wherein the filling proportion of the carbon dioxide gas is 5%. At the same time, the roots pump of the atomizing tower was turned on to maintain the atomizing tower at a vacuum level of 1000Pa or less.
After the nitrogen and the carbon dioxide are mixed, keeping the mixture in a gas mixing tank for 5 minutes to ensure that the gases are uniformly mixed; the mixed gas is pressurized to 3MPa by a gas booster pump, is sprayed out by a spray head to fill the whole atomizing tower, and the molten and dropped tool steel metal liquid is made into spherical particles by the impact force of the gas.
And (3) cooling the atomized powder in an atomizing tower filled with nitrogen and carbon dioxide, and then treating the powder in grading equipment to obtain the tool steel metal powder for 3D printing in the required particle size range. The metal powder is collected, the one-time yield of the powder with the granularity of less than 20 mu m is 60 percent, and the sphericity is 96 percent. The nitrogen content was 81Pppm, which is much less than the nitrogen content that would easily cause 3D printing of powder on tool steel using nitrogen gas as the atomizing gas completely.
The powder morphology is shown in fig. 3.
Example 2:
1. the tool steels having the compositions shown in Table 2 were used, and it was required to select a bar-shaped tool steel produced by a billet caster as a raw material. Removing the oxide rust layer on the surface of the raw material by using a polishing method, cutting the raw material into small sections of 30-50 cm, putting the small sections into an induction melting furnace of vacuum atomization powder spraying equipment, vacuumizing the induction melting furnace to 200pa, setting the power to be 20kw, heating, and ensuring that the raw material is completely melted.
TABLE 2 chemical composition of raw materials Table
C Ti Mn P S Co Mo Ni N
0.025 0.7 ≤0.10 ≤0.01 ≤0.01 9 4.9 18.5 60ppm
2. Vacuumizing a 100L mixed gas tank to 100Pa, introducing nitrogen into the mixed gas tank, switching a valve, and introducing purchased liquid carbon dioxide gas into the mixed gas tank, wherein the filling proportion of the carbon dioxide gas is 10%. At the same time, the roots pump of the atomizing tower was turned on to maintain the atomizing tower at a vacuum level of 1000Pa or less.
3. After the nitrogen and the carbon dioxide are mixed, keeping the mixture in a gas mixing tank for 5 minutes to ensure that the gases are uniformly mixed; the mixed gas is pressurized to 3.5MPa by a gas booster pump, is sprayed out by a spray head to fill the whole atomizing tower, and the molten and dripped tool steel metal liquid is made into spherical particles by the impact force of the gas.
4. And (3) cooling the atomized powder in an atomizing tower filled with nitrogen and carbon dioxide, and then treating the powder in grading equipment to obtain the tool steel metal powder for 3D printing in the required particle size range. The object is shown in FIG. 4.
Example 3:
1. the tool steels having the compositions shown in Table 3 were used, and it was required to select a bar-shaped tool steel produced by a billet caster as a raw material. Removing the oxide rust layer on the surface of the raw material by using an acid washing or polishing method, cutting the raw material into small sections of 30-50 cm, putting the small sections into an induction melting furnace of vacuum atomization powder spraying equipment, vacuumizing the induction melting furnace to 200pa, setting the power to be 20kw, and heating to ensure that the raw material is completely melted.
TABLE 3 raw material chemical composition Table
C Ti Mn P S Co Mo Ni N
0.01 0.8 ≤0.10 ≤0.01 ≤0.01 10 5.1 18.7 70ppm
2. Vacuumizing a 100L gas mixing tank to 100pa, introducing nitrogen into the gas mixing tank, and switching a valve to introduce purchased liquid carbon dioxide into the gas mixing tank, wherein the filling proportion of the carbon dioxide is 15%. At the same time, the roots pump of the atomizing tower was turned on to maintain the atomizing tower at a vacuum level of 1000Pa or less.
3. After the nitrogen and the carbon dioxide are mixed, keeping the mixture in a gas mixing tank for 5 minutes to ensure that the gases are uniformly mixed; the mixed gas is pressurized to 4MPa by a gas booster pump, is sprayed out by a spray head to fill the whole atomizing tower, and the molten and dropped tool steel metal liquid is made into spherical particles by the impact force of the gas.
4. And (3) cooling the atomized powder in an atomizing tower filled with nitrogen and carbon dioxide, and then treating the powder in grading equipment to obtain the tool steel metal powder for 3D printing in the required particle size range. The object is shown in FIG. 5.
The nitrogen content of the technical powder of the tool steel produced under three conditions is shown in table 4:
TABLE 4 nitrogen content of powder of different example tool steels
Example 1 Example 2 Example 3
90ppm 75ppm 80ppm
Three examples were analyzed to produce tool steel metal powder using a mixed gas of carbon dioxide and nitrogen for nitrogen reduction purposes.

Claims (7)

1. The patent relates to a method for producing 3D printing tool steel powder by using mixed gas of carbon dioxide and nitrogen as atomizing gas.
2. The method related to claim 1 is characterized in that a tool steel bar is used as a raw material, the nitrogen content of the raw material is less than or equal to 70PPM, the carbon content of the raw material is 0.02-0.03%, an oxide rust layer on the surface of the tool steel bar is removed by using a grinding method, and the tool steel bar is cut into small sections of 30-50 cm.
3. Claim 1 uses a mixture of carbon dioxide and nitrogen as the atomizing and cooling gas, the volume content of carbon dioxide in the mixture being 0% to 25%, the remainder being nitrogen.
4. The gas mixture according to claim 3, wherein the carbon dioxide and the nitrogen are introduced after the mixture is sufficiently mixed in a gas mixing tank.
5. The mixed gas as set forth in claim 4 is increased to 2.5 to 5MPa by a gas booster pump.
6. The mixed gas of claim 4 and 5 is controlled by an accessory program added on a computer control panel, and the pressurized gas is sprayed out through a spray head to break up tool steel metal liquid drops to obtain metal powder.
7. The metal powder of claim 7, wherein the yield of the powder with a particle size of less than 20 μm is not less than 50% and the sphericity is not less than 95% by collection.
CN202010156628.6A 2020-03-09 2020-03-09 Method for producing tool steel powder for 3D printing Withdrawn CN111299600A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4762553A (en) * 1987-04-24 1988-08-09 The United States Of America As Represented By The Secretary Of The Air Force Method for making rapidly solidified powder
CN1612781A (en) * 2002-02-13 2005-05-04 梅普拉金属粉有限公司 Method for producing particle-shaped material
US20120156494A1 (en) * 2009-08-20 2012-06-21 Christian Wolfrum Method for producing dispersions having metal oxide nanoparticles and dispersions produced thereby
CN107052352A (en) * 2017-04-01 2017-08-18 北京康普锡威科技有限公司 A kind of CO2The apparatus for preparing metal powder and method of gas shield
CN108115145A (en) * 2017-12-28 2018-06-05 北京康普锡威科技有限公司 A kind of apparatus for preparing metal powder and preparation method
CN108555308A (en) * 2018-07-23 2018-09-21 福州麦辽自动化设备有限公司 A kind of vacuum atomizing device and the method for preparing 3D printing powder
CN108580914A (en) * 2018-07-23 2018-09-28 福州臻美网络科技有限公司 A kind of vacuum atomizing device and the method for preparing 3D printing powder
CN108941587A (en) * 2018-07-23 2018-12-07 深圳市晶特智造科技有限公司 A kind of vacuum atomizing device and the method for preparing 3D printing powder
CN109079149A (en) * 2018-08-30 2018-12-25 深圳市晶莱新材料科技有限公司 A kind of method and apparatus producing Fe-Mn-Pt metal powder

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4762553A (en) * 1987-04-24 1988-08-09 The United States Of America As Represented By The Secretary Of The Air Force Method for making rapidly solidified powder
CN1612781A (en) * 2002-02-13 2005-05-04 梅普拉金属粉有限公司 Method for producing particle-shaped material
US20120156494A1 (en) * 2009-08-20 2012-06-21 Christian Wolfrum Method for producing dispersions having metal oxide nanoparticles and dispersions produced thereby
CN107052352A (en) * 2017-04-01 2017-08-18 北京康普锡威科技有限公司 A kind of CO2The apparatus for preparing metal powder and method of gas shield
CN108115145A (en) * 2017-12-28 2018-06-05 北京康普锡威科技有限公司 A kind of apparatus for preparing metal powder and preparation method
CN108555308A (en) * 2018-07-23 2018-09-21 福州麦辽自动化设备有限公司 A kind of vacuum atomizing device and the method for preparing 3D printing powder
CN108580914A (en) * 2018-07-23 2018-09-28 福州臻美网络科技有限公司 A kind of vacuum atomizing device and the method for preparing 3D printing powder
CN108941587A (en) * 2018-07-23 2018-12-07 深圳市晶特智造科技有限公司 A kind of vacuum atomizing device and the method for preparing 3D printing powder
CN109079149A (en) * 2018-08-30 2018-12-25 深圳市晶莱新材料科技有限公司 A kind of method and apparatus producing Fe-Mn-Pt metal powder

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