CN106735266B - The preparation method of increasing material manufacturing powder of stainless steel, stainless steel and the stainless steel - Google Patents
The preparation method of increasing material manufacturing powder of stainless steel, stainless steel and the stainless steel Download PDFInfo
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- CN106735266B CN106735266B CN201611072289.3A CN201611072289A CN106735266B CN 106735266 B CN106735266 B CN 106735266B CN 201611072289 A CN201611072289 A CN 201611072289A CN 106735266 B CN106735266 B CN 106735266B
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- stainless steel
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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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- 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
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
Abstract
The invention discloses a kind of increasing material manufacturing powder of stainless steel, and by what is obtained after stainless steel raw material powder progress ingredient, melting, powder processed, sub-sieve, aging strengthening model, the mass content of copper is 1wt%-10wt% in the stainless steel raw material powder.Preparation method of the invention: powder of stainless steel is first prepared；Increasing material manufacturing is carried out after carrying out a timeliness to powder of stainless steel, then the alloy that increasing material manufacturing is obtained solution treatment 0.5-3h at 1050-1200 DEG C carries out secondary ageing heat treatment again to get stainless steel is arrived.The stainless steel of method preparation of the invention is all improved relative to traditional stainless steel, room temperature lower yield strength and tensile strength, elongation percentage.
Description
Technical field
The invention belongs to stainless steel material field more particularly to a kind of increasing material manufacturing powder of stainless steel, stainless steel and it is somebody's turn to do
The preparation method of stainless steel.
Background technique
Metal increasing material manufacturing includes selective laser melting technology, direct metal laser sintering forming technique, selectively swashs
Light sintering technology and electron-beam melting forming technique are the mainstream metal rapid prototyping technologies occurred in recent years, are rapid prototyping manufacturings
One of latest development form.Metal increasing material manufacturing is melted moulding material using high energy laser beam or electron beam, and material melts
After change under software program driving, the solidification of each slice is completed by design technology automatically, material is recombined and forms gold
Belong to part.
The caking power of increasing material manufacturing course powder determines the performance of final alloy or component.The prior art usually exists
On the basis of the conventional cast alloying component having been commercialized, by different flouring technologies adjusted powder size, size distribution,
The parameters such as oxygen content, sphericity are suitable for the alloy powder of increasing material manufacturing to research and develop.However, general alloy such as ferrous alloy, by
, large specific surface area small in granularity, powder surface are usually to exist in the form of alloyed oxide, since oxide generally relatively causes
It is close, need higher energy to destroy the sintering and densification for being just able to achieve powder to it at high temperature.Material system is increased for electron beam
Process is made, due to the charge buildup effect of oxide on surface, process adjustments are improper also to cause so-called " haze phenomenon ", not only
Increase increasing material manufacturing alloy defect, can also destroy the vacuum system of equipment or electron gun.As shown in Figure 1, conventional powder is increasing material
In manufacturing process, electron beam or laser sintered limited to the irradiation of powder or sintering time, due to the presence of surface film oxide,
It is difficult to form liquid phase between particle, hinders the expanding of element between powder, cause sintering insufficient, component has a large amount of sintering defect
Or hole, reduce the mechanical property or service life of component.Therefore, suitable powdered ingredients, structure how are developed, particle is made
Between preferentially form liquid phase, promoting the quick diffusion of element between particle is the key that one of current increases material manufacturing technology of solution.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
The preparation method of kind increasing material manufacturing powder of stainless steel, stainless steel and the stainless steel.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
A kind of increasing material manufacturing powder of stainless steel carries out ingredient, melting, powder processed, sub-sieve, timeliness by stainless steel raw material powder
It is obtained after heat treatment, the mass content of copper is 1wt%-10wt% in the stainless steel raw material powder.Applicant is by repeatedly
Research and experimental verification discovery are difficult after ageing treatment in particle surface when copper content is lower than 1wt% in powder of stainless steel
To enough copper, the sintering character of powder of stainless steel is promoted little；As the high 10wt% of copper content, copper amount of precipitation is too many, breaks
Bad particle surface pattern, causes powder flowbility to decline, unfavorable to increasing material manufacturing；Meanwhile copper content be higher than 10wt% when, increase material
Copper can largely be precipitated in manufacturing process, and precipitate meeting agglomeration, unobvious to the performance facilitation of stainless steel, or even meeting
Deteriorate stainless Steel Properties.
Above-mentioned powder of stainless steel, it is preferred that the stainless steel raw material powder is on the component base of 316L stainless steel
It is obtained after addition copper.
Above-mentioned powder of stainless steel, it is preferred that the aging heat treatment temperature is 300-700 DEG C, time 0.5-5h.
Applicant is by research repeatedly and experimental verification discovery, by the ageing treatment of suitable temperature and right times, can make a large amount of
Copper is precipitated in the crystal boundary and other fault locations of particle surface, difficult since the diffusion coefficient of copper is very low when temperature is lower than 300 DEG C
It, can be due between the copper of precipitation between powder when temperature is higher than 700 DEG C to form the copper of sufficient amount in powder particle surface
Diffusion bonds, and powder flowbility is caused to decline.
The inventive concept total as one, the present invention also provides a kind of preparation methods of stainless steel, comprising the following steps:
(1) stainless steel raw material powder is first subjected to ingredient, melting, powder processed, sub-sieve, an aging strengthening model, obtained stainless
Powdered steel；Aging heat treatment temperature is 300-700 DEG C, time 0.5-5h；In the stainless steel raw material powder
The mass content of copper is 1wt%-10wt%；
(2) increasing material manufacturing is carried out to the powder of stainless steel, the alloy that increasing material manufacturing is obtained is solid at 1000-1200 DEG C
Then molten processing 0.5-3h carries out secondary ageing heat treatment again to get the stainless steel is arrived；Wherein, at the secondary ageing heat
The temperature of reason is 300-600 DEG C, time 0.5-5h.Applicant passes through repeatedly the study found that solid solution temperature is lower than 1000
DEG C when, elements diffusion is slow, and the required solution treatment time is longer, and is difficult to ensure whole extraneous copper element solid solutions in not
In steel matrix of becoming rusty；Simultaneously it has also been found that stainless steel base softens when solid solubility temperature is higher than 1200 DEG C, parts of stainless steel may result in
Deformation；Wherein, the temperature of the secondary ageing heat treatment is 200-600 DEG C, time 0.5-5h；Applicant by studying repeatedly
It was found that the diffusion rate of copper is very low when secondary ageing temperature is lower than 200 DEG C, it is precipitated and hydrodynamics effect is unobvious, work as temperature
When degree is higher than 600 DEG C, the copper Yi Chang great of precipitation, mechanical property and corrosion resistance to stainless steel have deterioration to be inclined to.Timeliness temperature
When spending lower (400 DEG C or less), aging time can be appropriately extended 3-5 hours, and when aging temp is higher, aging time is appropriate
Shortening is advisable (0.5-2 hours), and the time, the too long precipitate copper that will lead to was grown up.I.e. the present invention first passes through solution treatment and makes between particle
Copper be solid-solubilized in matrix again, handling using secondary ageing can make copper Dispersed precipitate in alloy substrate, to improve not
The intensity of rust steel.
Above-mentioned preparation method a, it is preferred that aging strengthening model and secondary ageing heat treatment are in vacuum or lazy
It is carried out under property gas shield.
Above-mentioned preparation method, it is preferred that copper content is 3wt%-8wt% in the stainless steel raw material powder.
Above-mentioned preparation method, it is preferred that the pulverizing process uses argon gas aerosolization, nitrogen aerosolization or plasma
Rotation electrode powder.
Above-mentioned preparation method, it is preferred that the stainless steel raw material powder carries out an aging heat treatment temperature and is
400-600 DEG C, time 2-4h.
Above-mentioned preparation method, it is preferred that the temperature of the secondary ageing heat treatment is 350-450 DEG C, time 3-4h.
Above-mentioned preparation method, it is preferred that the stainless steel raw material powder is to add copper on the component base of stainless steel
It obtains afterwards, copper is uniformly solid-solution in powdered base in the stainless steel raw material powder；Wherein, the stainless steel is selected as
316L stainless steel.
The inventive concept total as one, the present invention also provides a kind of stainless steels, are prepared by above-mentioned preparation method.
Compared with the prior art, the advantages of the present invention are as follows:
(1) powder of stainless steel of the invention has a large amount of copper segregation, increasing material manufacturing process through an ageing treatment rear surface
Copper can be solid-solution in stainless steel base after middle temperature increases, can be by real again after solution treatment after the completion of increasing material manufacturing
Row ageing treatment (secondary ageing), making copper, Dispersed precipitate reaches alloy strengthening effect in stainless steel base again, further mentions
The mechanical property of high stainless steel.
(2) suitable solid solution copper, Powder during Sintering Process schematic diagram excessively are added in stainless steel of the invention sees Fig. 2 institute
Show, a large amount of copper can be made to be precipitated in the crystal boundary of particle surface and other fault locations, due to table by the aging strengthening model to powder
The copper in face can melt at compared with the lower temperature of matrix, while its liquid phase and matrix have preferable wetability, may act as high temperature
The quick diffusion admittance of matrix stainless steel in sintering process, to greatly improve the sintering character of powder.
(3) suitable solid solution copper excessively is added in stainless steel of the invention, can be made by the aging strengthening model to powder
A large amount of copper is precipitated in the crystal boundary and other fault locations of particle surface, due to the fusing point of copper is low and good conductivity etc., can have
Effect avoid conventional powder surface be oxidized object surround caused by caking power is low, during electron beam increasing material manufacturing haze it is existing
As the problems such as, to reduce increasing material manufacturing cost, improve the performance of increasing material manufacturing stainless steel.
(4) for the stainless steel of method of the invention preparation relative to traditional stainless steel, room temperature lower yield strength and stretching are strong
Degree, elongation percentage are all improved.
Detailed description of the invention
Fig. 1 is powder of stainless steel Powder during Sintering Process schematic diagram during increasing material manufacturing in the prior art.
Fig. 2 is Powder during Sintering Process schematic diagram during stainless steel increasing material manufacturing of the present invention.
Fig. 3 is the phasor that the present invention adds 0-10% copper in 316L stainless steel.
Specific embodiment
To facilitate the understanding of the present invention, invention herein is done below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment:
The present embodiment selection tool steel powder be in the stainless composition of steel of 316L add copper carry out ingredient, melting, powder processed,
It is obtained after sub-sieve, aging strengthening model；The ingredient and content minute mark of the tool steel powder are as follows: 316L stainless steel alloy powder:
Fe-17Cr-13Ni-2.5Mo-2.1Mn-0.5Si-0.01C-(1-10)Cu。
The phasor of copper is added in 316L stainless steel primitive component as shown in Figure 3, from the figure 3, it may be seen that former in 316L stainless steel
After adding copper in beginning ingredient, when high temperature, copper can be solid-solution in completely in 316L stainless steel base, pass through argon gas aerosolization, nitrogen gas
Atomization or plasma rotating electrode are quickly cooled down the powder of preparation, and since copper has little time to spread, copper was solid solution condition, and uniformly
It is distributed in 316L stainless steel base, after aging strengthening model, copper is precipitated from iron matrix, and is preferentially precipitated at crystal boundary position,
And form continuous copper networks；Copper is made to be segregated in the grain boundaries that energy is higher, unstable by aging strengthening model, and crystal boundary is exactly
The position that powder preferential oxidation occurs, these effectively prevent the generation of increasing material manufacturing Powder Oxidation along the copper of crystal boundary distribution；
Simultaneously as the copper fusing point of particle surface is low, during increasing material manufacturing, liquid phase can be preferentially formed, enhances the member between particle
The diffusion of element, improves the sintering character of powder.
The preparation method of the stainless steel of following embodiments, comprising the following steps:
(1) stainless steel raw material powder is subjected to ingredient, melting, powder processed (argon gas aerosolization, nitrogen aerosolization or plasma rotation
Turn electrode rapid cooling and prepare powder), sub-sieve, under inert gas protection carry out an aging strengthening model；According to copper content
Difference, the variation in 300-700 DEG C, 0.5-5 hours ranges of aging heat treatment condition and range；
(2) increasing material manufacturing is carried out to the raw material after an aging strengthening model, the alloy that increasing material manufacturing is obtained is in 1000-
Secondary ageing heat treatment is carried out at 1200 DEG C after solution treatment 0.5-3h, obtains stainless steel；Secondary ageing heat treatment temperature be
300-600 DEG C, time 0.5-5h, secondary ageing heat treatment also carries out under inert gas protection.At increasing material manufacturing and solid solution
After reason, the copper of particle surface is all solid-solution in matrix again, guarantees that each element is uniformly divided in stainless steel alloy after solution treatment
Cloth carries out ageing treatment (secondary ageing) again, copper Dispersed precipitate is made to reach alloy strengthening effect in stainless steel alloy matrix,
Further increase the mechanical property of alloy.
Stainless steel alloy performance is shown in Table 1 He after the ingredient of nitrogen aerosolization powder of stainless steel and increasing material manufacturing in the present embodiment
Shown in table 2.
(draw direction is parallel to paving to the 316L stainless steel alloy ingredient and room-temperature property of each embodiment and comparative example of table 1
Powder)
Increasing material manufacturing stainless steel in 2 different embodiments of the invention of the table mechanical property after timeliness at different temperatures
By the experimental data of table 1- table 2 it is found that the stainless steel (comparative example) of stainless steel of the invention compared with the prior art,
Room temperature lower yield strength and tensile strength improve 20-60MPa, and elongation percentage improves 2-6%.It can be seen that the present invention tradition not
It becomes rusty on the basis of steel, by adding suitable Cu element, and by the suitable ageing treatment of carry out to powder, improves stainless
The sintering character of steel improves the mechanical property of alloy and elongation percentage, ensure that the mechanical property of stainless steel.
Claims (6)
1. a kind of preparation method of stainless steel, which comprises the following steps:
(1) stainless steel raw material powder is first subjected to ingredient, melting, powder processed, sub-sieve, an aging strengthening model, obtains stainless steel powder
End；Aging heat treatment temperature is 300-700 DEG C, time 0.5-5h；Copper in the stainless steel raw material powder
Mass content is 1wt%-10wt%；The stainless steel raw material powder is obtained after adding copper on the component base of 316L stainless steel
It arrives, copper is uniformly solid-solution in powdered base in the stainless steel raw material powder；
(2) increasing material manufacturing is carried out to the powder of stainless steel, the alloy that increasing material manufacturing is obtained is at 1000-1200 DEG C at solid solution
0.5-3h is managed, carries out secondary ageing heat treatment again then to get stainless steel is arrived；Wherein, the temperature of the secondary ageing heat treatment
It is 300-600 DEG C, time 0.5-5h.
2. preparation method as described in claim 1, which is characterized in that the pulverizing process uses argon gas aerosolization, nitrogen gas
Atomization or plasma rotating electrode powder.
3. preparation method as described in claim 1, which is characterized in that an aging strengthening model and secondary ageing heat treatment
Carried out under vacuum or inert gas shielding.
4. preparation method as described in claim 1, which is characterized in that copper content is 3wt%- in the stainless steel raw material powder
8wt%.
5. preparation method as described in claim 1, which is characterized in that the stainless steel raw material powder carries out a timeliness heat
The temperature of processing is 400-600 DEG C, time 2-4h；The temperature of the secondary ageing heat treatment is 350-450 DEG C, time 3-
4h。
6. a kind of stainless steel, which is characterized in that be prepared by the described in any item preparation methods of the claims 1-5.
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| CN101381868A (en) * | 2008-10-27 | 2009-03-11 | 徐洪 | High-hardness stainless steel alloy powder for laser remelted and technique of preparing the same |
| CN105537582A (en) * | 2016-03-03 | 2016-05-04 | 上海材料研究所 | 316L stainless steel powder for 3D printing technology and preparation method thereof |
| CN105648175A (en) * | 2015-12-31 | 2016-06-08 | 无锡透平叶片有限公司 | Heat treatment method capable of increasing first pass yield of 0Cr17Ni4Cu4Nb stainless steel material and application thereof |
| CN106048382A (en) * | 2016-06-08 | 2016-10-26 | 山东大学（威海） | Powder metallurgy stainless steel and preparation method thereof |
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2016
- 2016-11-29 CN CN201611072289.3A patent/CN106735266B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676654A (en) * | 2005-04-14 | 2005-10-05 | 华南理工大学 | Stainless steel powder composite material and its warm-pressing method |
| CN101381868A (en) * | 2008-10-27 | 2009-03-11 | 徐洪 | High-hardness stainless steel alloy powder for laser remelted and technique of preparing the same |
| CN105648175A (en) * | 2015-12-31 | 2016-06-08 | 无锡透平叶片有限公司 | Heat treatment method capable of increasing first pass yield of 0Cr17Ni4Cu4Nb stainless steel material and application thereof |
| CN105537582A (en) * | 2016-03-03 | 2016-05-04 | 上海材料研究所 | 316L stainless steel powder for 3D printing technology and preparation method thereof |
| CN106048382A (en) * | 2016-06-08 | 2016-10-26 | 山东大学（威海） | Powder metallurgy stainless steel and preparation method thereof |
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