CN105648303A - Method for improving sphericity of stainless steel powder prepared by atomization method - Google Patents

Method for improving sphericity of stainless steel powder prepared by atomization method Download PDF

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Publication number
CN105648303A
CN105648303A CN201610118170.9A CN201610118170A CN105648303A CN 105648303 A CN105648303 A CN 105648303A CN 201610118170 A CN201610118170 A CN 201610118170A CN 105648303 A CN105648303 A CN 105648303A
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stainless steel
atomization
powder
sphericity
steel
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CN201610118170.9A
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CN105648303B (en
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杜宇雷
卢晓阳
廖文和
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
    • C22C33/06Making ferrous alloys by melting using master alloys
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y70/00Materials specially adapted for additive manufacturing

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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)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a method for improving the sphericity of stainless steel powder prepared by an atomization method, which is characterized in that the content of elements such as oxygen, nitrogen, sulfur and the like capable of reducing the surface tension in stainless steel is reduced, the content of element silicon capable of increasing the surface tension is controlled to be at the upper limit of a standard component of target stainless steel, and trace element boron capable of increasing the surface tension is added, so that the surface tension of a stainless steel melt liquid drop is obviously improved on the basis of not influencing the performance of the stainless steel, the stainless steel melt liquid drop can be contracted into powder with better sphericity under the action of larger surface tension during atomization, and the purpose of improving the sphericity of the stainless steel powder prepared by the atomization method is realized.

Description

A kind of improve the method that atomization prepares powder of stainless steel sphericity
Technical field
The present invention relates to and a kind of improve the method that atomization prepares 3D printing powder of stainless steel sphericity, belong to 3D printed material and field of powder metallurgy.
Background technology
Atomization is the common method preparing metal dust, mainly includes aerosolization, water atomization, centrifugal atomizing, ultrasonic atomizatio, plasma atomization etc. In general, the pattern of the different metal dusts prepared by atomization is distinguishing. The pattern of metal dust prepared by water atomization is many in irregularly shaped, the poor fluidity of powder; And the atomizations such as aerosolization, centrifugal atomizing, ultrasonic atomizatio, plasma atomization can prepare spherical or subsphaeroidal powder, the mobility of powder is better.
3D prints (increasing material manufacture) and refers to according to mathematical model, by continuous print physical layer superposition, successively increases the mode of material to manufacture the technology of 3D solid object, represents the new trend of world's development of manufacturing. At present, the metal 3D of industrial application prints the raw material used and is mainly all kinds of metal dust, and the automatic powder feeding system that these metals 3D printing technique uses mainly has powder bed powder and the big class of coaxial powder-feeding two. In order to ensure seriality and the high accuracy of print procedure, all require that the sphericity of used metal dust wants height, there is splendid mobility.
Powder of stainless steel is the 3D raw material printing that the class used is important. At present, powder of stainless steel can be atomized preparation by water atomization, aerosolization or plasma, and such as, patent CN201010574595.3 discloses a kind of method that hydraulic atomized method produces spherical stainless steel dusty material; Patent CN200710121435.1 discloses a kind of method adopting aerosolization method to prepare nitrogenous/high nitrogen stainless steel powder; Patent CN201310304846.X discloses a kind of method that plasma spheroidization prepares minute spherical powder of stainless steel. But said method is distinctive in that the atomization method used is different, and prepared powder of stainless steel is all applied for traditional powder metallurgy or metal injection molded field, and the sphericity of powder and mobility can't fully meet the 3D particular/special requirement printed.
Summary of the invention
The invention aims to provide a kind of and can improve the method that atomization prepares powder of stainless steel sphericity further so that the sphericity of prepared powder of stainless steel and mobile performance meet the 3D instructions for use printed.
The technical scheme method realizing the object of the invention is as follows: a kind of improve the method that atomization prepares powder of stainless steel sphericity, comprises the steps:
The first step: first, according to target stainless standard analysis, raw material being carried out proportioning, heating fused raw material also carries out deoxidation, denitrogenation, desulfurization process, wherein, deoxidation adopts addition silicomanganese calcium aluminum barium double deoxidizer in molten steel to carry out, and its addition is less than the 0.1% of molten steel gross mass; Denitrogenation adopts in molten steel one or more that add in a certain amount of Ti, Al, V to carry out, and concrete addition is determined according to nitrogen maxima solubility 0.045% in molten steel and molten steel total; Desulfurization adopts the composite desulfurizing agent added in molten steel containing Ca, Al to carry out, and consumption is the 0.3% of molten steel gross mass, namely obtains oxygen, nitrogen, sulfur content are below the hypoxia of 100ppm, low nitrogen, low-sulfur rustless steel foundry alloy;
Second step: the hypoxia that the first step is obtained, low nitrogen, low-sulfur rustless steel foundry alloy remelting, measure and control the content of silicon in foundry alloy, determine that silicone content reaches the interval upper limit of target stainless steel standard composition, simultaneously, add the boron of trace, its addition with on target stainless steel base, be formed without boracic precipitate for the upper limit, thus obtaining siliceous and the hypoxia of boron, low nitrogen, low-sulfur rustless steel foundry alloy;
3rd step: the rustless steel foundry alloy prepared by second step carries out powder by atomization.
Further, in the first step, silicomanganese calcium aluminum barium double deoxidizer is 40wt%Si, 10wt%Mn, the compositions of 25wt%Ca, 10wt%Al, 15wt%Ba.
Further, in the first step, composite desulfurizing agent is 60wt%CaC2��20wt%CaO��10wt%CaF2, 10wt%Al compositions.
Further, in the 3rd step, powder by atomization include water atomization, aerosolization, centrifugal atomizing, ultrasonic atomizatio, plasma atomization, rotating electrode atomized.
Compared with prior art, the invention have the advantage that
1, the present invention with increase stainless steel melt drop surface tension for target, its composition has been carried out special design and adjustment, the surface tension of the stainless steel melt drop improved is bigger than corresponding standard brand stainless steel watch surface tension, thus sphericity and mobility powder of stainless steel more preferably can be obtained under identical atomization process and atomization plant, it is possible to meet the 3D particular/special requirement printed.
2, the method for the invention is simple, and be all significantly improved effect to existing powder by atomization technology.
Accompanying drawing explanation
Fig. 1 is the SEM figure of aerosolization 430 powder of stainless steel adopting the inventive method to prepare.
Fig. 2 is the SEM figure of the aerosolization 316L powder of stainless steel adopting the inventive method to prepare.
Detailed description of the invention
The principle of institute of the present invention foundation is the content by adjusting impurity element in rustless steel, effect of surface tension is bigger and trace nonmetalloid, stainless steel melt drop increases the surface tension of stainless steel melt drop further, so that can be shrunk to the better powder of sphericity when atomization under bigger surface tension effects. For passing through to reduce in rustless steel the content of the elements such as oxygen, nitrogen and sulfur that surface tension can be made to reduce, meanwhile, control can make content capping in allowed band of the elemental silicon that surface tension increases, and adds the element boron that surface tension can be made to increase of trace; Adjusted by mentioned component, do not affecting the surface tension significantly improving stainless steel melt drop on the basis of rustless steel performance, stainless steel melt drop is enable to be shrunk to the better powder of sphericity under bigger surface tension effects when atomization, it is achieved to improve atomization and prepare the purpose of powder of stainless steel sphericity.
Of the present invention a kind of improve the method that atomization prepares powder of stainless steel sphericity, comprise the steps:
The first step: the purpose of this step is to reduce in rustless steel foundry alloy the content of the elements such as oxygen, nitrogen and sulfur that surface tension can be made to reduce as far as possible, but for nitrogenous rustless steel then with reduce oxygen and sulfur content for target.First, the standard chemical composition of the target rustless steel trade mark according to required preparation carries out proportioning, add heat fusing and carry out deoxidation, denitrogenation, desulfurization process (adopting the deoxidation in tradition process for making, denitrogenation, sulfur removal technology to carry out), wherein, deoxidation adopts the precipitation desoxydation method adding silicomanganese calcium aluminum barium double deoxidizer (addition is less than the 0.1% of molten steel total amount) in molten steel to carry out; Denitrogenation adopts in molten steel one or more that add in a certain amount of Ti, Al, V to carry out (concrete addition is determined, such as 100 kilograms of molten steel interpolation Ti150g) according to nitrogen maxima solubility (0.045%) in molten steel and molten steel total; Desulfurization adopts the composite desulfurizing agent (CaC added in molten steel containing Ca, Al oxide260%+CaO20%+CaF210%+Al10%, consumption is the 0.3% of molten steel total amount) carry out; Thus obtaining hypoxia, low nitrogen, low-sulfur rustless steel foundry alloy. In order to reach to reduce as far as possible the content (content of each element is lower than 100ppm) of oxygen, nitrogen, element sulphur, the deoxidation adopted, denitrogenation, desulfurization process means and include but not limited to method listed above.
Second step: the hypoxia that the first step is obtained, low nitrogen, low-sulfur rustless steel foundry alloy remelting, the upper limit that the composition that the content (being generally adopted ICP or Photometric Determination) measuring and controlling silicon in foundry alloy is standard analysis defined is interval, as lower than higher limit, then again add proper amount of silicon to the composition interval upper limit. Simultaneously, add the boron of trace, addition is with the difference slightly difference (because boron element dissolubility in the rustless steel of heterogeneity is variant) of the prepared rustless steel trade mark, but with the precipitate that is formed without boracic on stainless steel base, for the upper limit, (higher limit is determined by boron element maxima solubility in this composition rustless steel, boron dissolubility in rustless steel is usually no more than 0.03%), thus obtaining siliceous and the hypoxia of boron, low nitrogen, low-sulfur rustless steel foundry alloy.
3rd step: the prepared hypoxia containing proper amount of silicon and boron, low nitrogen, low-sulfur rustless steel foundry alloy are carried out powder by atomization, can adopt water atomization, aerosolization, centrifugal atomizing, ultrasonic atomizatio, plasma atomization, the atomization preparing metal dust such as rotating electrode atomized to carry out. Owing to invention increases the surface tension of stainless steel melt self, therefore, the effect of its sphericity improving prepared powder is not rely on specific atomization.
Embodiment 1
Prepare spherical 430 powder of stainless steel.
(1) according to 430 stainless standard analysis (C :��0.12%, Si :��0.75%, Mn :��1.00%, P :��0.040%, S :��0.030%, Ni :��0.60%, Cr:16.00 ~ 18.00%; Surplus is ferrum; Mass percent, raw metal purity is more than 99.9%) carry out proportioning, each raw-material consumption is determined in mentioned component ratio and prepared stainless total amount, in the present embodiment, prepares 100kg430 rustless steel, each element consumption is as follows: Cr18kg, Ni0.6kg, Mn1kg, Si0.75kg, surplus is that Fe, C, P and S content are less than standard analysis requirement; Add heat fusing, molten steel adds 0.1kg silicomanganese calcium aluminum barium double deoxidizer and carries out precipitation desoxydation, molten steel adds 150gTi and carries out denitrogenation, molten steel adds 0.3kg composite desulfurizing agent (CaC260%+CaO20%+CaF210%+Al10%) carry out desulfurization, thus obtaining hypoxia, low nitrogen, low-sulfur rustless steel foundry alloy.
(2) by prepared rustless steel foundry alloy remelting, adopt ICP to measure and control the content upper limit allowing interval at 430 rustless steel compositions of silicon, i.e. 0.75% (mass fraction is 0.75kg in this example);Add the boron (mass fraction is 0.03kg in this example) of 0.03%, thus obtaining the hypoxia containing proper amount of silicon and boron, low nitrogen, low-sulfur rustless steel foundry alloy.
(3) the prepared hypoxia containing proper amount of silicon and boron, low nitrogen, low-sulfur 430 rustless steel foundry alloy are carried out gas-atomized powder, atomization gas is argon, gas pressure intensity is 6MPa, thus obtaining 430 powder of stainless steel, as shown in Figure 1, it is seen that, the sphericity of 430 powder of stainless steel prepared by employing the inventive method is splendid, substantially without hollow powder and satellite ball phenomenon, good fluidity, it is possible to meet the 3D user demand printed.
Embodiment 2
Prepare spherical 316L powder of stainless steel.
(1) according to the stainless standard analysis of 316L (C :��0.030%, Si :��1.00%, Mn :��2.00%, S :��0.030%, P :��0.045%, Cr:16.00��18.00%, Ni:10.00��14.00%, Mo:2.00��3.0%, mass percent, raw metal purity is more than 99.9%) carry out proportioning, each raw-material consumption is determined in mentioned component ratio and prepared stainless total amount, in the present embodiment, preparation 100kg316L rustless steel, each element consumption is as follows: Cr18kg, Ni14kg, Mn2kg, Mo3kg, Si1kg, surplus is Fe, C, P and S content is less than standard analysis requirement, add heat fusing, molten steel adds 0.1kg silicomanganese calcium aluminium composite deoxidant and carries out precipitation desoxydation, molten steel adds 150gTi and carries out denitrogenation, molten steel adds 0.3kg composite desulfurizing agent (CaC260%+CaO20%+CaF210%+Al10%) carry out desulfurization, thus obtaining hypoxia, low nitrogen, low-sulfur rustless steel foundry alloy.
(2) by prepared rustless steel foundry alloy remelting, adopt ICP measure and control the content upper limit in 316L rustless steel composition allowed band of silicon, i.e. 1%(mass fraction, this example be 1kg)); Add 0.026%(mass fraction, this example be 0.026kg) boron, thus the acquisition hypoxia containing proper amount of silicon and boron, low nitrogen, low-sulfur rustless steel foundry alloy.
(3) the prepared hypoxia containing proper amount of silicon and boron, low nitrogen, low-sulfur 316L rustless steel foundry alloy are carried out gas-atomized powder, atomization gas is argon, gas pressure intensity is 6MPa, thus obtaining 316L powder of stainless steel, as shown in Figure 2, it can be seen that, the sphericity of 316L powder of stainless steel prepared by employing the inventive method is splendid, without hollow powder and satellite ball phenomenon, mobility is splendid, it is possible to meet the 3D user demand printed.

Claims (4)

1. one kind is improved the method that atomization prepares powder of stainless steel sphericity, it is characterised in that comprise the steps:
The first step: raw material is carried out proportioning according to target stainless standard analysis, heating fused raw material also carries out deoxidation, denitrogenation, desulfurization process, wherein, deoxidation adopts addition silicomanganese calcium aluminum barium double deoxidizer in molten steel to carry out, and its addition is less than the 0.1% of molten steel gross mass; Denitrogenation adopts in molten steel one or more that add in a certain amount of Ti, Al, V to carry out, and its addition is determined according to nitrogen maxima solubility 0.045% in molten steel and molten steel total; Desulfurization adopts the composite desulfurizing agent added in molten steel containing Ca, Al to carry out, and consumption is the 0.3% of molten steel gross mass, namely obtains oxygen, nitrogen, sulfur content are below the hypoxia of 100ppm, low nitrogen, low-sulfur rustless steel foundry alloy;
Second step: the hypoxia that the first step is obtained, low nitrogen, low-sulfur rustless steel foundry alloy remelting, measure and control the content of silicon in foundry alloy, determine that silicone content reaches the interval upper limit of target stainless steel standard composition, simultaneously, add the boron of trace, its addition with on target stainless steel base, be formed without boracic precipitate for the upper limit, thus obtaining siliceous and the hypoxia of boron, low nitrogen, low-sulfur rustless steel foundry alloy;
3rd step: the rustless steel foundry alloy prepared by second step carries out powder by atomization.
2. the method that raising atomization as claimed in claim 1 prepares powder of stainless steel sphericity, it is characterised in that in the first step, silicomanganese calcium aluminum barium double deoxidizer is 40wt%Si, 10wt%Mn, the compositions of 25wt%Ca, 10wt%Al, 15wt%Ba.
3. the method that raising atomization as claimed in claim 1 prepares powder of stainless steel sphericity, it is characterised in that in the first step, composite desulfurizing agent is 60wt%CaC2��20wt%CaO��10wt%CaF2, 10wt%Al compositions.
4. as claimed in claim 1 improving the method that atomization prepares powder of stainless steel sphericity, it is characterised in that in the 3rd step, powder by atomization includes water atomization, aerosolization, centrifugal atomizing, ultrasonic atomizatio, plasma atomization, rotating electrode atomized.
CN201610118170.9A 2016-03-02 2016-03-02 Method for improving sphericity of stainless steel powder prepared by atomization method Active CN105648303B (en)

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Cited By (3)

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WO2018075380A1 (en) * 2016-10-17 2018-04-26 Ecole Polytechnique Treatment of melt for atomization technology
CN107999774A (en) * 2017-12-05 2018-05-08 南通金源智能技术有限公司 A kind of method for improving 3D printing powder of stainless steel sphericity
CN112620642A (en) * 2020-12-29 2021-04-09 深圳市福英达工业技术有限公司 Centrifugal atomization device and method for preparing high-temperature high-surface-tension metal powder

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018075380A1 (en) * 2016-10-17 2018-04-26 Ecole Polytechnique Treatment of melt for atomization technology
CN110191776A (en) * 2016-10-17 2019-08-30 综合理工大学 The processing of melt for atomization technique
CN107999774A (en) * 2017-12-05 2018-05-08 南通金源智能技术有限公司 A kind of method for improving 3D printing powder of stainless steel sphericity
CN107999774B (en) * 2017-12-05 2021-01-26 南通金源智能技术有限公司 Method for improving sphericity of 3D printed stainless steel powder
CN112620642A (en) * 2020-12-29 2021-04-09 深圳市福英达工业技术有限公司 Centrifugal atomization device and method for preparing high-temperature high-surface-tension metal powder

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