CN109609864B - High-nitrogen nickel-free stainless steel powder and preparation method thereof - Google Patents

High-nitrogen nickel-free stainless steel powder and preparation method thereof Download PDF

Info

Publication number
CN109609864B
CN109609864B CN201811580413.6A CN201811580413A CN109609864B CN 109609864 B CN109609864 B CN 109609864B CN 201811580413 A CN201811580413 A CN 201811580413A CN 109609864 B CN109609864 B CN 109609864B
Authority
CN
China
Prior art keywords
nitrogen
free
stainless steel
nickel
ball milling
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201811580413.6A
Other languages
Chinese (zh)
Other versions
CN109609864A (en
Inventor
崔晓龙
张峰
靳磊
梁梦媛
翁建寅
鲍贤勇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Feiyada Precision Technology Co ltd
Shenzhen Feiyada Precision Technology Co ltd
Original Assignee
Fiyta Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fiyta Group Co Ltd filed Critical Fiyta Group Co Ltd
Priority to CN201811580413.6A priority Critical patent/CN109609864B/en
Publication of CN109609864A publication Critical patent/CN109609864A/en
Application granted granted Critical
Publication of CN109609864B publication Critical patent/CN109609864B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of manganese
    • 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
    • B22F1/068—Flake-like particles
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • 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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Landscapes

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

Abstract

The invention discloses high-nitrogen nickel-free stainless steel powder and a preparation method thereof. The preparation method comprises the following steps: step S1, preparing a nitrogen-free nickel-free stainless steel ingot, wherein the nitrogen-free nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C less than 0.02%, Si less than 1%, and the balance of Fe; step S2, heating the nitrogen-free and nickel-free stainless steel ingot to a liquid state, and then carrying out atomization powder preparation to obtain nitrogen-free and nickel-free stainless steel powder; and step S3, carrying out plasma-assisted high-energy ball milling on the nitrogen-free and nickel-free stainless steel powder in the atmosphere of nitrogen element-containing gas to obtain the high-nitrogen nickel-free stainless steel powder. The preparation method has the advantages of lower cost, short period, high nitrogen injection efficiency and high powder collection rate. The high-nitrogen nickel-free stainless steel powder disclosed by the invention has the advantages of low impurity content of fine powder, low oxygen content, high powder sphericity and the like.

Description

High-nitrogen nickel-free stainless steel powder and preparation method thereof
Technical Field
The invention relates to the field of application and processing of stainless steel, in particular to high-nitrogen nickel-free stainless steel powder and a preparation method thereof.
Background
Austenitic stainless steels are non-magnetic, have excellent corrosion resistance and excellent surface finish, and have extremely wide application prospects in many fields, particularly in the fields of timepieces and biomedicine. However, the conventional austenitic stainless steel mainly comprises Cr-Ni, and the content of Ni in the stainless steel is high, so that the stainless steel can be leached by body fluids such as sweat, saliva and the like of a human body, and generates allergic reaction on a part of people, so that the problems of swelling, redness, pruritus and the like are caused, and the austenitic stainless steel is continuously limited in the wearable field, the medical field and the like. In addition, Ni is a strategic metal, is expensive, and is especially deficient in resources in China. Therefore, other elements that can replace the Ni element are sought, and development of Ni-free austenitic stainless steel is of great significance.
N is a powerful element for expanding and stabilizing an austenite phase region, and can greatly improve the mechanical property, the corrosion resistance and the biocompatibility of the alloy. In addition, N is widely present in nature, abundant in resources and low in cost, and therefore, N is an optimal element for replacing Ni. This makes the production of high nitrogen nickel-free austenitic stainless steels of great interest.
At present, the main method for preparing the high-nitrogen nickel-free austenitic stainless steel is a pressure smelting method. Although the pressure smelting method can further obtain high N content and high strength and high toughness compared with the high-nitrogen nickel-free austenitic stainless steel prepared by the conventional smelting method, the method has the defects of large production and preparation investment, difficult process and component control, high equipment maintenance cost and the like. In addition, after the high-nitrogen steel plate is prepared by a smelting method, parts need to be punched on the plate, so that the problem of great waste of leftover materials exists, and the requirements of resource conservation and environmental protection are not met.
The development of powder metallurgy technology provides a new approach for the preparation of high nitrogen steel. In the production of high nitrogen steel, the powder metallurgy method can produce a high nitrogen steel product that is difficult to produce by the cast forging method, in near net shape, as compared with the melting method. The powder metallurgy high-nitrogen steel also has the advantages of material saving, less pollution, high quality of produced parts, low capital investment, flexible process and the like. Meanwhile, the powder metallurgy method can also refine grains, eliminate or reduce component segregation and structure segregation, further obtain an alloy with uniformly distributed components, and can easily obtain higher nitrogen content. Therefore, the research of powder high nitrogen steel becomes one of the important research directions of the current high nitrogen nickel-free austenitic stainless steel.
The high-nitrogen nickel-free austenitic stainless steel prepared by adopting the powder metallurgy method is based on obtaining high-nitrogen nickel-free stainless steel powder with high N content, narrow particle size range and uniform distribution. Currently, main methods for preparing high-nitrogen nickel-free austenitic stainless steel powder include an atomization method, a chemical reaction method, a mechanical alloying method, and the like.
Patent application No. CN201110122970.5 provides a method for producing nickel-free high nitrogen stainless steel powder. The method uses soluble FeSO4、CrCl3、MnSO4、(NH3)2MoO3NaOH is used as raw material, firstly precursor powder is obtained by adopting a chemical precipitation method, and then the precursor powder is put into a continuous reaction furnace and placed into N2-H2The continuous reduction and nitridation reactions are carried out under the circulating mixed atmosphere to finally obtain the nickel-free high-nitrogen stainless steel powder. Although the nickel-free high-nitrogen stainless steel powder prepared by the method can reach the nanometer level, the preparation method firstly needs to obtain precursor powder and needs to carry out reduction treatment in a reaction furnace for a long time, and has the defects of long process period, high energy consumption and the like.
In the aspect of preparing the high-nitrogen nickel-free stainless steel powder by adopting a mechanical alloying method, the Cudamai and the like take Fe-Cr-Mn-Mo as raw materials to circulate high-purity N2High-nitrogen nickel-free stainless steel powder is obtained by stirring type high-energy ball milling treatment under the atmosphere (research on preparation of nearly spherical nickel-free high-nitrogen austenitic stainless steel powder by mechanical alloying, powder metallurgy technology, 2008, 26 (4): 265-268). However, this method has the following disadvantages: the simple substance powder is used as the raw material, and the cost is higher. The elements are not fused at high temperature, segregation is easy to exist, the ball milling time is long, the efficiency is low, and impurities are easy to introduce
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of high-nitrogen nickel-free stainless steel powder, which has the advantages of lower cost, short period, high nitrogen injection efficiency and high powder collection rate and aims at overcoming the defects of the prior art.
Another technical problem to be solved by the present invention is to provide a high-nitrogen nickel-free stainless steel powder obtained by the above preparation method, which has the advantages of low impurity content of fine powder, low oxygen content, high sphericity of powder, etc.
In order to solve the technical problems, the invention provides a preparation method of high-nitrogen nickel-free stainless steel powder, which comprises the following steps:
step S1, preparing a nitrogen-free nickel-free stainless steel ingot, wherein the nitrogen-free nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C less than 0.02%, Si less than 1%, and the balance of Fe;
step S2, heating the nitrogen-free and nickel-free stainless steel ingot to a liquid state, and then carrying out atomization powder preparation to obtain nitrogen-free and nickel-free stainless steel powder;
and step S3, carrying out plasma-assisted high-energy ball milling on the nitrogen-free and nickel-free stainless steel powder in the atmosphere of nitrogen element-containing gas to obtain the high-nitrogen nickel-free stainless steel powder.
As a preferable embodiment of the method for preparing the high-nitrogen nickel-free stainless steel powder according to the present invention, in step S1, the ingot of the nitrogen-free nickel-free stainless steel is prepared by vacuum induction melting, plasma arc melting, or electron beam melting.
As a preferable scheme of the method for preparing the high-nitrogen nickel-free stainless steel powder, in step S2, the method for preparing powder by atomization includes a gas atomization method or a plasma rotating electrode method.
As a preferable scheme of the method for preparing the high-nitrogen nickel-free stainless steel powder, in step S2, the method for preparing powder by atomization is a gas atomization method, and the implementation conditions of the powder preparation by atomization include: the melting temperature is 1400-1800 ℃, and the atomizing atmosphere is N2One or more of He and Ar, wherein the atomization air pressure is 2MPa to 50MPa, and the flow rate of the molten steel is 3kg/min to 30 kg/min.
As a preferable scheme of the method for preparing the high-nitrogen nickel-free stainless steel powder, in step S2, the method for preparing powder by atomization is a plasma rotating electrode method, and the conditions for preparing powder by atomization include: electrode rotating speed of8000 r/min-200000 r/min, metal alloy electrode rod diameter of 30 mm-500 mm, length of 50 mm-5000 mm, electrode rod feed rate of 0.5 mm/min-60 mm/min, and inert atmosphere of He, Ar and N2The plasma gun current is 500-10000A.
As a preferable embodiment of the method for preparing the high-nitrogen nickel-free stainless steel powder according to the present invention, the step S3 includes:
step S31, connecting a front cover plate of the ball milling tank which is cleaned cleanly with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the ball milling tank, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
and step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling.
As a preferable scheme of the preparation method of the high-nitrogen nickel-free stainless steel powder, the gas containing the nitrogen element is N2、NH3One or more of the above mixed gases.
As a preferable scheme of the preparation method of the high-nitrogen nickel-free stainless steel powder, the rotation speed of the ball milling driving motor is 600 rpm-1500 rpm, the amplitude of the excitation block of the plasma assisted high-energy ball mill is 4 mm-12 mm, the discharge voltage of the plasma power generator is 10 KV-50 KV, the discharge current is 0.5A-3A, and the mass ratio of the grinding balls to the nitrogen-free nickel-free stainless steel powder is 10: 1-80: 1, the ball milling time is 18-72 h.
In order to solve the technical problems, the invention also provides high-nitrogen nickel-free stainless steel powder which is prepared by the preparation method.
As a preferable embodiment of the high-nitrogen nickel-free stainless steel powder of the present invention, the high-nitrogen nickel-free stainless steel powder comprises the following components by mass percent: cr 15-25%, Mn 10-16%, Mo 2-8%, N0.92-2.83%, C < 0.02%, Si < 1%, and the balance Fe.
Compared with the prior art, the implementation of the invention has the following beneficial effects:
1. the invention provides a preparation method of high-nitrogen nickel-free stainless steel powder, which comprises the steps of preparing nitrogen-free nickel-free stainless steel powder with uniform particle size by atomizing a nitrogen-free stainless steel ingot, and then carrying out plasma-assisted high-energy ball milling on the nitrogen-free nickel-free stainless steel powder in the atmosphere of nitrogen-containing element gas to obtain the high-nitrogen nickel-free stainless steel powder. Therefore, the defects of high cost, easy segregation of component structures and the like caused by directly adopting pure metal powder ball milling are avoided.
2. In the preparation method of the high-nitrogen nickel-free stainless steel powder, provided by the invention, the high-nitrogen nickel-free stainless steel powder with high nitrogen content is quickly refined and activated by adopting plasma-assisted high-energy ball milling, and is obtained. Compared with the common ball milling with simple mechanical stress, the plasma field in the plasma-assisted high-energy ball milling can generate a thermal explosion effect and a high-energy electron bombardment effect, and under the synergistic coupling effect of the thermal explosion effect and the high-energy electron bombardment effect, the powder can be quickly refined and activated, and the N injection effect can be realized in a short time, so that the powder with high nitrogen content can be obtained.
3. In the preparation method of the high-nitrogen nickel-free stainless steel powder, the high-nitrogen nickel-free stainless steel powder with a unique lamellar structure is obtained by adopting plasma-assisted high-energy ball milling, and the high-nitrogen nickel-free stainless steel powder with the lamellar structure has large specific area and high activity and can further promote the improvement of nitrogen content. In addition, the plasma-assisted high-energy ball milling technology also has the function of inhibiting powder agglomeration, and the prepared high-nitrogen nickel-free stainless steel powder is ensured to be uniformly distributed, and the powder particles are small in size and narrow in distribution range.
4. The nitrogen-free and nickel-free stainless steel powder prepared by the preparation method provided by the invention has the advantages of low impurity content of fine powder, low oxygen content, high sphericity of powder and the like.
Drawings
FIG. 1 is a flow chart of the steps of the method for preparing high nitrogen nickel-free stainless steel powder according to the present invention.
Detailed Description
The invention provides high-nitrogen nickel-free stainless steel powder and a preparation method thereof.
The preparation method of the high-nitrogen nickel-free stainless steel powder comprises the following steps:
step S1, preparing a nitrogen-free nickel-free stainless steel ingot, wherein the nitrogen-free nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C less than 0.02%, Si less than 1%, and the balance of Fe;
step S2, heating the nitrogen-free and nickel-free stainless steel ingot to a liquid state, and then carrying out atomization powder preparation to obtain nitrogen-free and nickel-free stainless steel powder;
and step S3, carrying out plasma-assisted high-energy ball milling on the nitrogen-free and nickel-free stainless steel powder in the atmosphere of nitrogen element-containing gas to obtain the high-nitrogen nickel-free stainless steel powder.
In some embodiments, in said step S1, the ingot of nitrogen-free nickel-free stainless steel is prepared by vacuum induction melting. Specifically, the proportioned reactant materials are put into a vacuum induction smelting furnace, so that the prepared components comprise the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C less than 0.02%, Si less than 1%, and the balance Fe. It should be noted that, it is known to those skilled in the art to prepare reactant materials according to the composition requirements of the final nitrogen-free and nickel-free stainless steel ingot, and details are not described herein, and in addition, the vacuum induction melting furnace used herein is a commercially available product.
In some embodiments, in the step S1, the ingot of nitrogen-free and nickel-free stainless steel is prepared by plasma arc melting. Specifically, the proportioned reactant materials are put into a plasma arc melting furnace, so that the prepared components comprise the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C less than 0.02%, Si less than 1%, and the balance Fe. It should be noted that, it is known to those skilled in the art to configure the reactant materials according to the composition requirements of the final nitrogen-free and nickel-free stainless steel ingot, and details are not described herein, and in addition, the plasma arc melting furnace used herein is a commercially available existing product.
In some embodiments, in the step S1, the nitrogen-free and nickel-free stainless steel ingot is prepared by electron beam melting. Specifically, the proportioned reactant materials are put into electron beam melting, so that the prepared components comprise the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C less than 0.02%, Si less than 1%, and the balance Fe. It should be noted that, it is known to those skilled in the art to configure the reactant materials according to the composition requirements of the final nitrogen-free and nickel-free stainless steel ingot, and details are not described herein, and in addition, the electron beam melting furnace used herein is a commercially available existing product.
In some embodiments, in step S2, the method of atomizing to produce powder is a gas atomization method, and the conditions of atomizing to produce powder include: the melting temperature is 1400-1800 ℃, and the atomizing atmosphere is N2One or more of He and Ar, the atomization air pressure is 2MPa to 50MPa, and the flow rate of the molten steel (nitrogen-free nickel-free stainless steel molten steel) is 3kg/min to 30 kg/min.
In some embodiments, in step S2, the method of atomizing powder is a plasma rotating electrode method, and the conditions of atomizing powder include: the rotating speed of the electrode is 8000 r/min-200000 r/min, the diameter of the metal alloy electrode bar is 30 mm-500 mm, the length is 50 mm-5000 mm, and the feeding rate of the electrode bar0.5 mm/min-60 mm/min, and inert atmosphere of He, Ar and N2The plasma gun current is 500-10000A.
In some embodiments, the step S3 includes:
step S31, connecting a front cover plate of the ball milling tank which is cleaned cleanly with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder; the ball-milling medium is made of hard alloy, but in other embodiments, the ball-milling medium is not limited to hard alloy, and other media such as stainless steel and ceramic can be used to obtain the same effect; the total volume of the grinding balls accounts for 40-70% of the volume of the ball milling tank; the volume of the ball milling powder accounts for 20-50% of the space between the grinding balls;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the sealed ball milling tank through a vacuum valve, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
and step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling.
In some embodiments, the nitrogen element-containing gas is N2。
In some embodiments, the gas containing nitrogen is NH3。
In some embodiments, the nitrogen element-containing gas is N2And NH3The mixed gas of (1).
In some embodiments, the rotation speed of the ball mill driving motor is 600rpm to 1500rpm, the amplitude of the vibration block of the plasma assisted high-energy ball mill is 4mm to 12mm, the discharge voltage of the plasma power generator is 10KV to 50KV, the discharge current is 0.5A to 3A, and the mass ratio of the grinding balls to the nitrogen-free and nickel-free stainless steel powder is 10: 1-80: 1, the ball milling time is 18-72 h.
The plasma-assisted high-energy ball mill is a commercially available existing product.
The high-nitrogen nickel-free stainless steel powder obtained by the preparation method provided by the invention comprises the following components in percentage by mass: cr 15-25%, Mn 10-16%, Mo 2-8%, N0.92-2.83%, C < 0.02%, Si < 1%, and the balance Fe.
For a more clear understanding of the technical features, objects and effects of the present invention, embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of high-nitrogen nickel-free stainless steel powder, which specifically comprises the following steps:
and step S1, adding the proportioned smelting materials into a vacuum induction smelting furnace to prepare the nitrogen-free and nickel-free stainless steel liquid. The smelting parameters are set as follows: the initial vacuum degree of smelting is less than 25Pa, the refining vacuum degree is less than 10Pa, the refining time is 20-90 min, and mixed deoxidation is carried out by adopting precipitation deoxidation and diffusion deoxidation, wherein the deoxidation time is 30-90 min. And then pouring the nitrogen-free nickel-free stainless steel liquid into an ingot mold, and cooling to obtain the nitrogen-free nickel-free stainless steel ingot. The obtained nitrogen-free nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C < 0.02%, Si < 1%, and the balance Fe.
And step S2, placing the nitrogen-free and nickel-free stainless steel ingot obtained in the step S1 into an induction melting furnace for melting, and adopting gas atomization for powder preparation. The melting temperature of gas atomization powder preparation is 1400-1800 ℃, the atomization atmosphere is Ar gas, the atomization pressure is 2-50 MPa, and the flow rate of molten steel is 3-30 kg/min. Drying the obtained original nitrogen-free and nickel-free stainless steel powder, and then screening and collecting to obtain the required nitrogen-free and nickel-free stainless steel powder. The desired nitrogen-free and nickel-free stainless steel powder is obtained with an oxygen content of less than 0.04%.
Step S3, specifically including the steps of:
step S31, connecting a front cover plate of the ball milling tank made of the cleaned hard alloy material with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder; the ball-milling medium is made of hard alloy, but in other embodiments, the ball-milling medium is not limited to hard alloy, and other media such as stainless steel and ceramic can be used to obtain the same effect; the total volume of the grinding balls accounts for 40-70% of the volume of the ball milling tank; the volume of the ball milling powder accounts for 20-50% of the space between the grinding balls;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the sealed ball milling tank through a vacuum valve, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling;
wherein the gas containing nitrogen element is NH3And NH3Has a flow rate of 0.4m3The rotating speed of the ball milling driving motor is 600 rpm-1500 rpm, the amplitude of an excitation block of the plasma auxiliary high-energy ball mill is 4 mm-12 mm, the discharge voltage of the plasma power generator is 10 KV-50 KV, the discharge current is 0.5A-3A, and the mass ratio of the grinding balls to the nitrogen-free and nickel-free stainless steel powder is 10: 1, the ball milling time is 18 h.
The high-nitrogen nickel-free stainless steel powder obtained by the method comprises the following components in percentage by mass: 16.8 to 24.8 percent of Cr16, 10.3 to 15.9 percent of Mn10, 2.8 to 7.9 percent of Mo2, 0.92 percent of N, less than 0.02 percent of C, less than 1 percent of Si and the balance of Fe.
Example 2
The embodiment provides a preparation method of high-nitrogen nickel-free stainless steel powder, which specifically comprises the following steps:
and step S1, adding the proportioned smelting materials into a plasma arc smelting furnace to prepare the nitrogen-free and nickel-free stainless steel liquid. The working voltage of the plasma arc smelting furnace is 300-700V, the working current is 10-60 kA, and the smelting time is 10-60 min. The working atmosphere of the plasma arc melting is Ar gas, and the flow of the working gas is 1500-3500L/h. And then pouring the nitrogen-free nickel-free stainless steel liquid into an ingot mold, and cooling to obtain the nitrogen-free nickel-free stainless steel ingot. The obtained nitrogen-free and nickel-free stainless steel ingot comprises the following components in percentage by mass: : cr 18-28%, Mn 13-18%, Mo 4-10%, C < 0.02%, Si < 1%, and the balance Fe.
And step S2, placing the nitrogen-free and nickel-free stainless steel ingot obtained in the step S1 into an induction melting furnace for melting, and adopting gas atomization for powder preparation. The melting temperature of gas atomization powder preparation is 1400-1800 ℃, the atomization atmosphere is Ar gas, the atomization pressure is 2-50 MPa, and the flow rate of molten steel is 3-30 kg/min. Drying the obtained original nitrogen-free and nickel-free stainless steel powder, and then screening and collecting to obtain the required nitrogen-free and nickel-free stainless steel powder. The desired nitrogen-free and nickel-free stainless steel powder is obtained with an oxygen content of less than 0.04%.
Step S3, specifically including the steps of:
step S31, connecting a front cover plate of the ball milling tank made of the cleaned hard alloy material with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder; the ball-milling medium is made of hard alloy, but in other embodiments, the ball-milling medium is not limited to hard alloy, and other media such as stainless steel and ceramic can be used to obtain the same effect; the total volume of the grinding balls accounts for 40-70% of the volume of the ball milling tank; the volume of the ball milling powder accounts for 20-50% of the space between the grinding balls;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the sealed ball milling tank through a vacuum valve, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling;
wherein the gas containing nitrogen element is NH3And NH3Has a flow rate of 0.4m3The rotating speed of the ball milling driving motor is 600 rpm-1500 rpm, the amplitude of an excitation block of the plasma auxiliary high-energy ball mill is 4 mm-12 mm, the discharge voltage of the plasma power generator is 10 KV-50 KV, the discharge current is 0.5A-3A, and the mass ratio of the grinding balls to the nitrogen-free and nickel-free stainless steel powder is 30: 1, the ball milling time is 24 h.
The high-nitrogen nickel-free stainless steel powder obtained by the method comprises the following components in percentage by mass: 16.8 to 24.8 percent of Cr16, 10.3 to 15.9 percent of Mn10, 2.8 to 7.9 percent of Mo2, 1.16 percent of N, less than 0.02 percent of C, less than 1 percent of Si and the balance of Fe.
Example 3
The embodiment provides a preparation method of high-nitrogen nickel-free stainless steel powder, which specifically comprises the following steps:
and step S1, adding the proportioned smelting materials into an electron beam smelting furnace to prepare the nitrogen-free and nickel-free stainless steel liquid. The power of an electron gun for electron beam melting is 50-1200 kW, the air extraction rate is 5000-100000L/s, the vacuum degree in the furnace is less than 5Pa, the melting rate is 90-150 kg/h, and the melting time is 30-120 min. And then pouring the prepared nitrogen-free nickel-free stainless steel liquid into an ingot mold, and cooling to obtain the nitrogen-free nickel-free stainless steel ingot. The obtained nitrogen-free and nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C < 0.02%, Si < 1%, and the balance Fe.
And step S2, placing the nitrogen-free and nickel-free stainless steel ingot obtained in the step S1 into an induction melting furnace for melting, and adopting gas atomization for powder preparation. The melting temperature of gas atomization powder preparation is 1400-1800 ℃, the atomization atmosphere is Ar gas, the atomization pressure is 2-50 MPa, and the flow rate of molten steel is 3-30 kg/min. Drying the obtained original nitrogen-free and nickel-free stainless steel powder, and then screening and collecting to obtain the required nitrogen-free and nickel-free stainless steel powder. The desired nitrogen-free and nickel-free stainless steel powder is obtained with an oxygen content of less than 0.04%.
Step S3, specifically including the steps of:
step S31, connecting a front cover plate of the ball milling tank made of the cleaned hard alloy material with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder; the ball-milling medium is made of hard alloy, but in other embodiments, the ball-milling medium is not limited to hard alloy, and other media such as stainless steel and ceramic can be used to obtain the same effect; the total volume of the grinding balls accounts for 40-70% of the volume of the ball milling tank; the volume of the ball milling powder accounts for 20-50% of the space between the grinding balls;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the sealed ball milling tank through a vacuum valve, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling;
wherein the gas containing nitrogen element is N2And N is2Has a flow rate of 0.4m3The rotating speed of the ball milling driving motor is 600 rpm-1500 rpm, the amplitude of an excitation block of the plasma auxiliary high-energy ball mill is 4 mm-12 mm, the discharge voltage of the plasma power generator is 10 KV-50 KV, the discharge current is 0.5A-3A, and the mass ratio of the grinding balls to the nitrogen-free and nickel-free stainless steel powder is 40: 1, the ball milling time is 36 h.
The high-nitrogen nickel-free stainless steel powder obtained by the method comprises the following components in percentage by mass: 16.8 to 24.8 percent of Cr16, 10.3 to 15.9 percent of Mn10, 2.8 to 7.9 percent of Mo2, 1.67 percent of N, less than 0.02 percent of C, less than 1 percent of Si and the balance of Fe.
Example 4
The embodiment provides a preparation method of high-nitrogen nickel-free stainless steel powder, which specifically comprises the following steps:
and step S1, adding the proportioned smelting materials into a vacuum induction smelting furnace to prepare the nitrogen-free and nickel-free stainless steel liquid. The smelting parameters are set as follows: the initial vacuum degree of smelting is less than 25Pa, the refining vacuum degree is less than 10Pa, the refining time is 20-90 min, and mixed deoxidation is carried out by adopting precipitation deoxidation and diffusion deoxidation, wherein the deoxidation time is 30-90 min. And then pouring the nitrogen-free nickel-free stainless steel liquid into an ingot mold, and cooling to obtain the nitrogen-free nickel-free stainless steel ingot. The obtained nitrogen-free nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C < 0.02%, Si < 1%, and the balance Fe.
And step S2, placing the nitrogen-free and nickel-free stainless steel ingot obtained in the step S1 into an induction melting furnace for melting, and adopting a plasma rotating electrode method for preparing powder. The electrode rotating speed is 8000 r/min-200000 r/min, the diameter of the metal alloy electrode bar is 30 mm-500 mm, the length is 50 mm-5000 mm, the electrode bar feeding speed is 0.5 mm/min-60 mm/min, the plasma gun current is 500A-10000A, and the inert atmosphere is He gas. And collecting the nitrogen-free and nickel-free stainless steel powder after the powder preparation process, wherein the oxygen content of the obtained nitrogen-free and nickel-free stainless steel powder is lower than 0.04 percent.
Step S3, specifically including the steps of:
step S31, connecting a front cover plate of the ball milling tank made of the cleaned hard alloy material with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder; the ball-milling medium is made of hard alloy, but in other embodiments, the ball-milling medium is not limited to hard alloy, and other media such as stainless steel and ceramic can be used to obtain the same effect; the total volume of the grinding balls accounts for 40-70% of the volume of the ball milling tank; the volume of the ball milling powder accounts for 20-50% of the space between the grinding balls;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the sealed ball milling tank through a vacuum valve, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling;
wherein the gas containing nitrogen element is N2And N is2Has a flow rate of 0.4m3The rotating speed of the ball milling driving motor is 600 rpm-1500 rpm, the amplitude of an excitation block of the plasma auxiliary high-energy ball mill is 4 mm-12 mm, the discharge voltage of the plasma power generator is 10 KV-50 KV, the discharge current is 0.5A-3A, and the mass ratio of the grinding balls to the nitrogen-free and nickel-free stainless steel powder is 50: 1, the ball milling time is 48 h.
The high-nitrogen nickel-free stainless steel powder obtained by the method comprises the following components in percentage by mass: 16.8 to 24.8 percent of Cr16, 10.3 to 15.9 percent of Mn10, 2.8 to 7.9 percent of Mo2, 2.16 percent of N, less than 0.02 percent of C, less than 1 percent of Si and the balance of Fe.
Example 5
The invention provides a preparation method of high-nitrogen nickel-free stainless steel powder, which specifically comprises the following steps:
the embodiment provides a preparation method of high-nitrogen nickel-free stainless steel powder, which specifically comprises the following steps:
and step S1, adding the proportioned smelting materials into a plasma arc smelting furnace to prepare the nitrogen-free and nickel-free stainless steel liquid. The working voltage of the plasma arc smelting furnace is 300-700V, the working current is 10-60 kA, and the smelting time is 10-60 min. The working atmosphere of the plasma arc melting is Ar gas, and the flow of the working gas is 1500-3500L/h. And then pouring the nitrogen-free nickel-free stainless steel liquid into an ingot mold, and cooling to obtain the nitrogen-free nickel-free stainless steel ingot. The obtained nitrogen-free and nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C < 0.02%, Si < 1%, and the balance Fe.
And step S2, placing the nitrogen-free and nickel-free stainless steel ingot obtained in the step S1 into an induction melting furnace for melting, and adopting a plasma rotating electrode method for preparing powder. The electrode rotating speed is 8000 r/min-200000 r/min, the diameter of the metal alloy electrode bar is 30 mm-500 mm, the length is 50 mm-5000 mm, the electrode bar feeding speed is 0.5 mm/min-60 mm/min, the plasma gun current is 500A-10000A, and the inert atmosphere is He gas. And collecting the nitrogen-free and nickel-free stainless steel powder after the powder preparation process, wherein the oxygen content of the obtained nitrogen-free and nickel-free stainless steel powder is lower than 0.04 percent.
Step S3, specifically including the steps of:
step S31, connecting a front cover plate of the ball milling tank made of the cleaned hard alloy material with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder; the ball-milling medium is made of hard alloy, but in other embodiments, the ball-milling medium is not limited to hard alloy, and other media such as stainless steel and ceramic can be used to obtain the same effect; the total volume of the grinding balls accounts for 40-70% of the volume of the ball milling tank; the volume of the ball milling powder accounts for 20-50% of the space between the grinding balls;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the sealed ball milling tank through a vacuum valve, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling;
wherein the gas containing nitrogen element is NH3And NH3Has a flow rate of 0.4m3The rotating speed of the ball milling driving motor is 600 rpm-1500 rpm, the amplitude of an excitation block of the plasma auxiliary high-energy ball mill is 4 mm-12 mm, the discharge voltage of the plasma power generator is 10 KV-50 KV, the discharge current is 0.5A-3A, and the mass ratio of the grinding balls to the nitrogen-free and nickel-free stainless steel powder is 60: 1, the ball milling time is 60 h.
The high-nitrogen nickel-free stainless steel powder obtained by the method comprises the following components in percentage by mass: 16.8 to 24.8 percent of Cr16, 10.3 to 15.9 percent of Mn10, 2.8 to 7.9 percent of Mo2, 2.48 percent of N, less than 0.02 percent of C, less than 1 percent of Si and the balance of Fe.
Example 6
The embodiment of the invention provides a preparation method of high-nitrogen nickel-free stainless steel powder, which specifically comprises the following steps:
and step S1, adding the proportioned smelting materials into an electron beam smelting furnace to prepare the nitrogen-free and nickel-free stainless steel liquid. The power of an electron gun for electron beam melting is 50-1200 kW, the air extraction rate is 5000-100000L/s, the vacuum degree in the furnace is less than 5Pa, the melting rate is 90-150 kg/h, and the melting time is 30-120 min. And then pouring the prepared nitrogen-free nickel-free stainless steel liquid into an ingot mold, and cooling to obtain the nitrogen-free nickel-free stainless steel ingot. The obtained nitrogen-free and nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C < 0.02%, Si < 1%, and the balance Fe.
And step S2, placing the nitrogen-free and nickel-free stainless steel ingot obtained in the step S1 into an induction melting furnace for melting, and adopting a plasma rotating electrode method for preparing powder. The electrode rotating speed is 8000 r/min-200000 r/min, the diameter of the metal alloy electrode bar is 30 mm-500 mm, the length is 50 mm-5000 mm, the electrode bar feeding speed is 0.5 mm/min-60 mm/min, the plasma gun current is 500A-10000A, and the inert atmosphere is He gas. And collecting the nitrogen-free and nickel-free stainless steel powder after the powder preparation process, wherein the oxygen content of the obtained nitrogen-free and nickel-free stainless steel powder is lower than 0.04 percent.
Step S3, specifically including the steps of:
step S31, connecting a front cover plate of the ball milling tank made of the cleaned hard alloy material with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder; the ball-milling medium is made of hard alloy, but in other embodiments, the ball-milling medium is not limited to hard alloy, and other media such as stainless steel and ceramic can be used to obtain the same effect; the total volume of the grinding balls accounts for 40-70% of the volume of the ball milling tank; the volume of the ball milling powder accounts for 20-50% of the space between the grinding balls;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the sealed ball milling tank through a vacuum valve, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling;
wherein the gas containing nitrogen element is N2And N is2Has a flow rate of 0.4m3The rotating speed of the ball milling driving motor is 600 rpm-1500 rpm, the amplitude of an excitation block of the plasma auxiliary high-energy ball mill is 4 mm-12 mm, the discharge voltage of the plasma power generator is 10 KV-50 KV, the discharge current is 0.5A-3A, and the mass ratio of the grinding balls to the nitrogen-free and nickel-free stainless steel powder is 80: 1, the ball milling time is 72 h.
The high-nitrogen nickel-free stainless steel powder obtained by the method comprises the following components in percentage by mass: 16.8 to 24.8 percent of Cr16, 10.3 to 15.9 percent of Mn10, 2.8 to 7.9 percent of Mo2, 2.83 percent of N, less than 0.02 percent of C, less than 1 percent of Si and the balance of Fe.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (5)

1. A preparation method of high-nitrogen nickel-free stainless steel powder is characterized by comprising the following steps:
step S1, preparing a nitrogen-free nickel-free stainless steel ingot, wherein the nitrogen-free nickel-free stainless steel ingot comprises the following components in percentage by mass: cr 18-28%, Mn 13-18%, Mo 4-10%, C less than 0.02%, Si less than 1%, and the balance of Fe;
step S2, heating the nitrogen-free and nickel-free stainless steel ingot to a liquid state, and then carrying out atomization powder preparation to obtain nitrogen-free and nickel-free stainless steel powder;
step S3, carrying out plasma-assisted high-energy ball milling on the nitrogen-free and nickel-free stainless steel powder in the atmosphere of nitrogen element-containing gas to obtain the high-nitrogen nickel-free stainless steel powder;
in step S2, the atomized powder is prepared by a plasma rotating electrode method, and the conditions of the atomized powder include: the rotating speed of the electrode is 8000 r/min-200000 r/min, the diameter of the metal alloy electrode rod is 30 mm-500 mm, the length is 50 mm-5000 mm, the feeding rate of the electrode rod is 0.5 mm/min-60 mm/min, and the inert atmosphere adopted is He, Ar and N2The plasma gun current is 500-10000A;
the step S3 includes:
step S31, connecting a front cover plate of the ball milling tank which is cleaned cleanly with an electrode rod;
step S32, filling the ball milling tank with proportioned grinding balls and the nitrogen-free and nickel-free stainless steel powder;
step S34, mounting the cleaned rear cover plate of the ball milling tank to the ball milling tank;
step S35, vacuumizing the ball milling tank, and continuously introducing nitrogen-containing gas into the ball milling tank at a certain flow rate to fill the ball milling tank with the flowing nitrogen-containing gas;
step S36, fixing the ball milling tank on a plasma-assisted high-energy ball mill;
step S37, connecting the iron core in the electrode bar with the positive pole of a plasma power generator, and connecting the rear cover plate with the negative pole of the plasma power generator;
step S38, switching on the plasma power generator, setting discharge voltage and discharge current, starting a ball milling driving motor of the plasma-assisted high-energy ball mill, and performing plasma-assisted high-energy ball milling;
the rotating speed of the ball milling driving motor is 600 rpm-1500 rpm, the amplitude of an excitation block of the plasma auxiliary high-energy ball mill is 4 mm-12 mm, the discharge voltage of the plasma power generator is 10 KV-50 KV, the discharge current is 0.5A-3A, and the mass ratio of the grinding balls to the nitrogen-free and nickel-free stainless steel powder is 10: 1-80: 1, the ball milling time is 18-72 h.
2. The method for preparing a high-nitrogen nickel-free stainless steel powder according to claim 1, wherein in the step S1, the ingot of the nitrogen-free nickel-free stainless steel is prepared by vacuum induction melting, plasma arc melting, or electron beam melting.
3. The method for preparing a high-nitrogen nickel-free stainless steel powder according to claim 1, wherein the nitrogen element-containing gas is N2、NH3One or more of the above mixed gases.
4. A high nitrogen nickel-free stainless steel powder, characterized in that it is produced by the production method according to any one of claims 1 to 3.
5. The high-nitrogen nickel-free stainless steel powder according to claim 4, comprising the following components in percentage by mass: cr 15-25%, Mn 10-16%, Mo 2-8%, N2.16-2.83%, C < 0.02%, Si < 1%, and the balance Fe.
CN201811580413.6A 2018-12-24 2018-12-24 High-nitrogen nickel-free stainless steel powder and preparation method thereof Active CN109609864B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811580413.6A CN109609864B (en) 2018-12-24 2018-12-24 High-nitrogen nickel-free stainless steel powder and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811580413.6A CN109609864B (en) 2018-12-24 2018-12-24 High-nitrogen nickel-free stainless steel powder and preparation method thereof

Publications (2)

Publication Number Publication Date
CN109609864A CN109609864A (en) 2019-04-12
CN109609864B true CN109609864B (en) 2021-07-13

Family

ID=66011305

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811580413.6A Active CN109609864B (en) 2018-12-24 2018-12-24 High-nitrogen nickel-free stainless steel powder and preparation method thereof

Country Status (1)

Country Link
CN (1) CN109609864B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111570808A (en) * 2020-05-28 2020-08-25 Oppo（重庆）智能科技有限公司 Non-magnetic 17-4PH stainless steel material, preparation method thereof and shell of electronic equipment
CN111560564B (en) * 2020-06-09 2021-07-13 江苏省海洋资源开发研究院(连云港) Resource-saving high-nitrogen duplex stainless steel and near-net forming method thereof
CN112723872B (en) * 2021-02-04 2022-10-14 三桥惠(佛山)新材料有限公司 Manganese-zinc ferrite pre-sintering material and preparation process thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100333835C (en) * 2005-07-29 2007-08-29 华南理工大学 High energy ball mill method with plasma aid
CN103374685B (en) * 2012-04-23 2016-06-08 钢铁研究总院 A kind of stainless material and manufacture method thereof
CN105618776A (en) * 2016-04-11 2016-06-01 西安欧中材料科技有限公司 Preparation method of high-nitrogen stainless steel spherical powder

Also Published As

Publication number Publication date
CN109609864A (en) 2019-04-12

Similar Documents

Publication Publication Date Title
CN108907210B (en) Method for preparing solid spherical metal powder for additive manufacturing
CN108103381B (en) High-strength FeCoNiCrMn high-entropy alloy and preparation method thereof
CN109609864B (en) High-nitrogen nickel-free stainless steel powder and preparation method thereof
CN102717086B (en) Method for preparing high-niobium titanium-aluminum alloy spherical micro powder in short process
CN102280241B (en) Manufacturing process for iron-silicon-aluminum soft magnetic powder
CN108588582A (en) 3D printing high strength stainless steel powder and preparation process under low temperature Service Environment
CN110093548B (en) Ultrafine-grained high-toughness high-entropy alloy containing rare earth Gd and preparation method thereof
CN105950944B (en) A kind of high-melting-point high-entropy alloy NbMoTaWVTi and preparation method thereof
CN110014158A (en) A kind of method that aerosolization prepares spherical chromium powder
CN102277525A (en) Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel
CN112981231B (en) High-manganese-nitrogen austenitic stainless steel powder and preparation method thereof
CN102101174A (en) Water atomization diffusion alloy powder and preparation method thereof
CN113136531B (en) Powder metallurgy stainless steel
CN109518027B (en) Preparation method and application of fine-grain Mg-Al-Ti-C intermediate alloy
CN103752837A (en) Method for producing water atomized alloy powder by using reduced iron of smelting slag
CN109609863B (en) High-nitrogen nickel-free stainless steel powder and preparation method thereof
CN108977719B (en) A kind of preparation method of low-carbon alloy steel
CN114734044B (en) High-nitrogen nickel-free stainless steel powder and preparation method and application thereof
CN110732801A (en) Cu-Ni-Mn alloy solder powder and its preparing process
CN102373359B (en) Method for producing alloy steel powder special for automobile engines
CN114367669A (en) Preparation method of TaW10 alloy spherical powder for 3D printing
CN110499463A (en) A kind of method that microwave reduction iron ore prepares 316L stainless steel 3D printing metal powder
KR20140001530A (en) Producing method of fe-tic composite powder by mechanically activation process
CN113510246A (en) Preparation method of Ti-6Al-4V alloy powder and Ti-6Al-4V alloy powder prepared by same
CN111250721A (en) Method for producing Fe-Mn-Pt-based medical 3D printing metal material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CP01 Change in the name or title of a patent holder

Address after: 518034 Guangdong city of Shenzhen province Nanshan District Gao Xin Road Fiyta Technology Building

Patentee after: Feiyada Precision Technology Co.,Ltd.

Address before: 518034 Guangdong city of Shenzhen province Nanshan District Gao Xin Road Fiyta Technology Building

Patentee before: FIYTA HOLDINGS Ltd.

CP01 Change in the name or title of a patent holder
TR01 Transfer of patent right

Effective date of registration: 20210802

Address after: 518034 Guangdong city of Shenzhen province Nanshan District Gao Xin Road Fiyta Technology Building

Patentee after: Feiyada Precision Technology Co.,Ltd.

Patentee after: Shenzhen feiyada Precision Technology Co.,Ltd.

Address before: 518034 Guangdong city of Shenzhen province Nanshan District Gao Xin Road Fiyta Technology Building

Patentee before: Feiyada Precision Technology Co.,Ltd.

TR01 Transfer of patent right