CN108555285A - A kind of high-nitrogen nickel-free powder of stainless steel and preparation method thereof, application - Google Patents
A kind of high-nitrogen nickel-free powder of stainless steel and preparation method thereof, application Download PDFInfo
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- CN108555285A CN108555285A CN201810818526.9A CN201810818526A CN108555285A CN 108555285 A CN108555285 A CN 108555285A CN 201810818526 A CN201810818526 A CN 201810818526A CN 108555285 A CN108555285 A CN 108555285A
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/04—Removing impurities by adding a treating agent
- C21C7/06—Deoxidising, e.g. killing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
- C22C33/06—Making ferrous alloys by melting using master alloys
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Abstract
The present invention provides a kind of preparation methods of high-nitrogen nickel-free powder of stainless steel, include the following steps：(A) after chromic carbide iron, pure iron being mixed heating vacuum pumping, molten steel is obtained；(B) by molten steel it is melting down after, under the conditions of nitrogen protection, successively add alloy material, killer, nitro-alloy carry out alloying operate to obtain aluminium alloy；(C) by after the aluminium alloy water atomization, pigment separation is dry.The method that the preparation method of the high-nitrogen nickel-free powder of stainless steel of the embodiment of the present invention utilizes nitrogen protection; optimize the technological parameter in smelting process; it is uniform to prepare ingredient; dense structure; nitrogen content is higher than 0.6% high-nitrogen austenitic, and entire method operating procedure is simple, and operating condition is mild; easy to operate, should be widely promoted application.
Description
Technical field
Apply manufacture field the present invention relates to stainless steel, in particular to a kind of high-nitrogen nickel-free powder of stainless steel and
Preparation method, application.
Background technology
Austenitic stainless steel refers to the stainless steel at normal temperatures with austenite structure.Contain Cr about 18%, Ni in steel
When 8%-10%, C about 0.1%, there is stable austenite structure.Austenitic chromium nickel stainless steel includes famous 18Cr-8Ni steel
Increase Cr, Ni content on this basis and the high Cr-Ni Series Steels that the elements such as Mo, Cu, Si, Nb, Ti grow up are added.It is difficult to understand
Family name's body stainless steel is nonmagnetic and has high tenacity and plasticity, but intensity is relatively low, it is impossible to be allowed to strengthen by phase transformation, be only capable of leading to
It crosses cold working to be strengthened, S, Ca, Se is such as added, the elements such as Te then have good free-cutting machinability.
As it can be seen that austenitic stainless steel has lower hardness, wears no resistance at present, it to be used for Ovshinsky when body implant
Nickel in body stainless steel can be leached by body fluid such as the sweat of human body, salivas, and generate human allergy's reaction to part population, be caused
The problems such as swelling, rubescent, itch.
In view of this, special propose the present invention.
Invention content
The first object of the present invention is to provide a kind of preparation method of high-nitrogen nickel-free powder of stainless steel, preparation method profit
With the method for nitrogen protection, and optimize the technological parameter in smelting process, it is uniform to prepare ingredient, dense structure, and nitrogen content is high
In 0.6% high-nitrogen austenitic, entire method operating procedure is simple, and operating condition is mild, easy to operate, should be widely promoted and answers
With.
The second object of the present invention is to provide the high-nitrogen nickel-free powder of stainless steel that above-mentioned preparation method is prepared, the powder
Last quality is uniform, has excellent performance, mechanical property and corresponding corrosion resistance show it is excellent, further to expand the marketization
Possibility is provided, due to not containing nickel in the powder of stainless steel, the allergic reaction that people will not be caused any improves
The safety coefficient of stainless steel application.
The third object of the present invention is to provide the further application of above-mentioned high-nitrogen nickel-free powder of stainless steel, application field
Widely, it can be widely applied to injection moulding, body implant's manufacture etc., particularly with for easy allergic human population
The manufacture view of implant be more suitable for.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme：
An embodiment of the present invention provides a kind of preparation methods of high-nitrogen nickel-free powder of stainless steel, include the following steps：
(A) after chromic carbide iron, pure iron being mixed heating vacuum pumping, molten steel is obtained；
(B) by molten steel it is melting down after, under the conditions of nitrogen protection, add alloy material, killer successively, nitro-alloy closed
Aurification operates to obtain aluminium alloy；
(C) by after the aluminium alloy water atomization, pigment separation is dry.
Preparation method operating procedure itself is simple, and operating condition is mild, using the method for nitrogen protection, and optimizes smelting
Technological parameter in the process, it is uniform to prepare ingredient, dense structure, and nitrogen content is higher than 0.6% high-nitrogen austenitic, the stainless steel
Nickel element is not contained in powder, is reduced the allergic reaction of people when preparing body implant, is further expanded applicable surface.
Preferably, it in the step (A), is evacuated down between 10Pa-0.1MPa, is more preferably 10Pa.
Preferably, in the step (B), the alloy material is one or more of iron, molybdenum, violent element.
Preferably, in the step (B), the killer is aluminium element or element silicon；
Preferably, the additive amount of the killer is 1-2kg/t molten steel.
Preferably, in the step (B), the temperature of alloying controls between 1530-1550 DEG C.
The present invention also provides a kind of high-nitrogen nickel-free powder of stainless steel being prepared using above-mentioned preparation method.
Preferably, the particle size distribution law of above-mentioned high-nitrogen nickel-free powder of stainless steel is：Particle accounting more than 180 μm
0.027wt%, the particle accounting 34.8wt% between 74 μm -180 μm, the particle accounting 11.6wt% between 53 μm -74 μm,
Particle accounting 13.8wt% between 38.5 μm -53 μm is less than 38.5 μm of particle accounting 39.8wt%.
Preferably, the mobility of the powder of stainless steel controls between (20-21s)/50g.
Preferably, the nitrogen content of powder of stainless steel is more than 0.6wt%, and carbon content is less than 0.05wt%, and oxygen content is less than
0.04wt%.
Above-mentioned high-nitrogen nickel-free powder of stainless steel all has very good answer in injection moulding, body implant's manufacture view
With.
Compared with prior art, beneficial effects of the present invention are：
(1) method that the preparation method of high-nitrogen nickel-free powder of stainless steel of the invention utilizes nitrogen protection, and optimize smelting
Technological parameter in the process, it is uniform to prepare ingredient, dense structure, and nitrogen content is higher than 0.6% high-nitrogen austenitic, entire method
Operating procedure is simple, and operating condition is mild, easy to operate, and should be widely promoted application.
(2) the high-nitrogen nickel-free powder of stainless steel quality being prepared is uniform, has excellent performance, mechanical property and corresponding resistance to
Corrosive nature show it is excellent, for further expand the marketization provide possibility, due in the powder of stainless steel do not contain nickel,
Therefore the allergic reaction that people will not be caused any improves the safety coefficient of stainless steel application.
(3) above-mentioned its application field of high-nitrogen nickel-free powder of stainless steel of the present invention is very extensive, can be widely applied to note
Molding, body implant's manufacture etc. are penetrated, is more suitable for particularly with the manufacture view of the implant for easy allergic human population.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
An embodiment of the present invention provides a kind of preparation methods of high-nitrogen nickel-free powder of stainless steel, include the following steps：
(A) after chromic carbide iron, pure iron being mixed heating vacuum pumping, molten steel is obtained；
(B) by molten steel it is melting down after, under the conditions of nitrogen protection, add alloy material, killer successively, nitro-alloy closed
Aurification operates to obtain aluminium alloy；
(C) by after the aluminium alloy water atomization, pigment separation is dry.
Preparation method operating procedure itself is simple, and operating condition is mild, using the method for nitrogen protection, and optimizes smelting
Technological parameter in the process, it is uniform to prepare ingredient, dense structure, and nitrogen content is higher than 0.6% high-nitrogen austenitic, the stainless steel
Nickel element is not contained in powder, is reduced the allergic reaction of people when preparing body implant, is further expanded powder of stainless steel
Applicable surface.
Preferably, it in the step (A), is evacuated down between 10Pa-0.1MPa, is more preferably 10Pa.
Preferably, in the step (B), the alloy material is one or more of iron, molybdenum, violent element.
Preferably, in the step (B), the killer is aluminium element or element silicon；
Preferably, the additive amount of the killer is 1-2kg/t molten steel.
Preferably, in the step (B), the temperature of alloying controls between 1530-1550 DEG C.
The present invention also provides a kind of high-nitrogen nickel-free powder of stainless steel being prepared using above-mentioned preparation method.
Preferably, the particle size distribution law of above-mentioned high-nitrogen nickel-free powder of stainless steel is：Particle accounting more than 180 μm
0.027wt%, the particle accounting 34.8wt% between 74 μm -180 μm, the particle accounting 11.6wt% between 53 μm -74 μm,
Particle accounting 13.8wt% between 38.5 μm -53 μm is less than 38.5 μm of particle accounting 39.8wt%.In such granularity point
It can ensure the homogeneity of the powder under cloth rule, and there is excellent performance.
Preferably, the indices of the powder of stainless steel are preferably controlled in following range：Mobility is controlled in (20-
Between 21s)/50g.
Preferably, the nitrogen content of powder of stainless steel is more than 0.6wt%, and carbon content is less than 0.05wt%, and oxygen content is less than
0.04wt%.
Above-mentioned high-nitrogen nickel-free powder of stainless steel all has very good answer in injection moulding, body implant's manufacture view
With.When as body implant due to direct body contact, higher want is proposed for the security performance of its material therefor
It asks, the high-nitrogen nickel-free powder of stainless steel that the present invention is prepared can just meet application requirement.
The high-nitrogen nickel-free powder of stainless steel that the present invention is prepared has been established very good for a series of subsequent operation of development
Good basis：
1, by the analysis of the thermodynamic behavior of nitrogen alloying process, establish in molten steel the solubility of nitrogen and alloy at
Divide, the quantitative calculation of temperature and nitrogen partial pressure, and discusses temperature, nitrogen partial pressure and alloying component to nitrogen using the computation model
The affecting laws of dissolving；
2, nitrogen nitrogen solubility model in solid phase (delta ferrite phase and x austenite phases) stainless steel system is established, and analyzes conjunction
Golden ingredient, nitrogen partial pressure are to the affecting laws of nitrogen solubility in solid phase stainless steel system；It is solidifying in high-nitrogen austenitic stainless steel using nitrogen
Microsegregation during Gu and precipitation mathematical model, the influence factor that analyzing influence nitrogen is segregated and is precipitated in process of setting；
3, by the metallurgy theory analysis smelted to high-nitrogen austenitic stainless steel, optimize smelting process parameter, utilize nitrogen
The vaccum sensitive stove and nitrogen protection electroslag remelting smelting technology of gas shielded prepare uniform ingredient, dense structure, nitrogen content height
In 0.6% high-nitrogen austenitic stainless steel；
4, tensile Properties are carried out to the high-nitrogen austenitic stainless steel of preparation, obtains nitrogen content, crystallite dimension, experiment temperature
Degree, tensile speed are to the affecting laws of high-nitrogen austenitic stainless steel mechanical property；And by high-nitrogen austenitic stainless steel not
Impact experiment research under synthermal, the tough Transition of Brittleness behavior of research high-nitrogen austenitic stainless steel and freezing crack mechanism, and
Go out affecting laws of the nitrogen content in high-nitrogen austenitic stainless steel to its tough brittle transition temperature；
5, to the corrosion resistance of the high-nitrogen austenitic stainless steel of preparation, especially resistance to local corrosion performance conducts a research,
Such as spot corrosion, crevice corrosion, intercrystalline corrosion obtain influence factor and its influence of high-nitrogen austenitic stainless steel corrosion resistance
Rule, to develop the high-nitrogen austenitic stainless steel based theoretical of high corrosion resistance.
The solution of the present invention is further described below by specific embodiment：
Embodiment 1
1) chromic carbide iron, ingot iron are mixed after being added, be powered heating, is evacuated down to 10Pa or so, obtains molten steel；
2) by molten steel it is melting down after, be passed through nitrogen protection gas, and add alloy material (manganese metal and metallic iron)；
3) killer of 1-2kg/t molten steel is added, killer selects aluminium；
4) control bath temperature is added nitro-alloy progress alloying and obtains aluminium alloy between 1530-1550 DEG C；
5) by after the aluminium alloy water atomization, pigment separation is finally dried in vacuo, obtains high-nitrogen nickel-free powder of stainless steel.
The high-nitrogen nickel-free powder of stainless steel the key technical indexes is as follows after testing：
The powder size regularity of distribution is：Particle accounting 0.027wt% more than 180 μm, the particle between 74 μm -180 μm
Accounting 34.8wt%, the particle accounting 11.6wt% between 53 μm -74 μm, the particle accounting between 38.5 μm -53 μm
13.8wt% is less than 38.5 μm of particle accounting 39.8wt%.
Mobility is controlled in 20s/50g.
Nitrogen content 0.6wt%.
Carbon content 0.05wt%.
Oxygen content 0.04wt%.
Embodiment 2
1) chromic carbide iron, ingot iron are mixed after being added, be powered heating, is evacuated down to 50KPa or so, obtains molten steel；
2) by molten steel it is melting down after, be passed through nitrogen protection gas, and add alloy material (manganese metal and metal molybdenum)；
3) killer of 1-2kg/t molten steel is added, killer selects silicon；
4) control bath temperature is added nitro-alloy progress alloying and obtains aluminium alloy between 1530-1550 DEG C；
5) by after the aluminium alloy water atomization, pigment separation is finally dried in vacuo, obtains high-nitrogen nickel-free powder of stainless steel.
The high-nitrogen nickel-free powder of stainless steel the key technical indexes is as follows after testing：
The powder size regularity of distribution is：Particle accounting 0.027wt% more than 180 μm, the particle between 74 μm -180 μm
Accounting 34.8wt%, the particle accounting 11.6wt% between 53 μm -74 μm, the particle accounting between 38.5 μm -53 μm
13.8wt% is less than 38.5 μm of particle accounting 39.8wt%.
Mobility is controlled in 21s/50g.
Nitrogen content 0.7wt%.
Carbon content 0.04wt%.
Oxygen content 0.03wt%.
Embodiment 3
1) chromic carbide iron, ingot iron are mixed after being added, be powered heating, is evacuated down to 90KPa or so, obtains molten steel；
2) by molten steel it is melting down after, be passed through nitrogen protection gas, and add alloy material (manganese metal, metallic iron and metal molybdenum)；
3) killer of 1-2kg/t molten steel is added, killer selects silicon；
4) control bath temperature is added nitro-alloy progress alloying and obtains aluminium alloy between 1530-1550 DEG C；
5) by after the aluminium alloy water atomization, pigment separation is finally dried in vacuo, obtains high-nitrogen nickel-free powder of stainless steel.
The high-nitrogen nickel-free powder of stainless steel the key technical indexes is as follows after testing：
The powder size regularity of distribution is：Particle accounting 0.027wt% more than 180 μm, the particle between 74 μm -180 μm
Accounting 34.8wt%, the particle accounting 11.6wt% between 53 μm -74 μm, the particle accounting between 38.5 μm -53 μm
13.8wt% is less than 38.5 μm of particle accounting 39.8wt%.
Mobility is controlled in 20s/50g.
Nitrogen content 0.6wt%.
Carbon content 0.05wt%.
Oxygen content 0.04wt%.
Comparative example 1
The key technical indexes of austenitic stainless steel is as follows：
The powder size regularity of distribution is：- 22 μm >=80%.
Carbon content 0.03wt%, oxygen content 0.05wt%.
The each embodiment of the present invention by using Fe-Cr-Mn-Mo-N systems high-nitrogen austenitic stainless steel as main study subject,
By the metallurgy basic research to nitrogen basic act and influence factor in molten steel, process of setting, made under high pressure or normal pressure
It is standby go out ingredient uniformly, the high-nitrogen austenitic stainless steel of dense structure, and to the mechanical property and corrosion resistant of high-nitrogen austenitic stainless steel
Corrosion can be studied, and lay the foundation in Chinese large-scale industrial production for high nitrogen stainless steel.
Compared with prior art, beneficial effects of the present invention are：
(1) method that the preparation method of high-nitrogen nickel-free powder of stainless steel of the invention utilizes nitrogen protection, and optimize smelting
Technological parameter in the process, it is uniform to prepare ingredient, dense structure, and nitrogen content is higher than 0.6% high-nitrogen austenitic, entire method
Operating procedure is simple, and operating condition is mild, easy to operate, and should be widely promoted application.
(2) the high-nitrogen nickel-free powder of stainless steel quality being prepared is uniform, has excellent performance, mechanical property and corresponding resistance to
Corrosive nature show it is excellent, for further expand the marketization provide possibility, due in the powder of stainless steel do not contain nickel,
Therefore the allergic reaction that people will not be caused any improves the safety coefficient of stainless steel application.
(3) above-mentioned its application field of high-nitrogen nickel-free powder of stainless steel of the present invention is very extensive, can be widely applied to note
Molding, body implant's manufacture etc. are penetrated, is more suitable for particularly with the manufacture view of the implant for easy allergic human population.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of preparation method of high-nitrogen nickel-free powder of stainless steel, which is characterized in that include the following steps：
(A) after chromic carbide iron, pure iron being mixed heating vacuum pumping, molten steel is obtained；
(B) by molten steel it is melting down after, under the conditions of nitrogen protection, successively add alloy material, killer, nitro-alloy carry out alloying
Operation obtains aluminium alloy；
(C) by after the aluminium alloy water atomization, pigment separation is dry.
2. preparation method according to claim 1, which is characterized in that in the step (A), be evacuated down to 10Pa-
It is more preferably 10Pa between 0.1MPa.
3. preparation method according to claim 1, which is characterized in that in the step (B), the alloy material be iron, molybdenum,
One or more of violent element.
4. preparation method according to claim 1, which is characterized in that in the step (B), the killer is aluminium member
Element or element silicon；
Preferably, the additive amount of the killer is 1-2kg/t molten steel.
5. preparation method according to claim 1, which is characterized in that in the step (B), the temperature control of alloying exists
Between 1530-1550 DEG C.
6. the high-nitrogen nickel-free powder of stainless steel that claim 1-5 any one of them preparation methods are prepared.
7. high-nitrogen nickel-free powder of stainless steel according to claim 6, which is characterized in that the granularity of the powder of stainless steel point
Cloth rule is：Particle accounting 0.027wt% more than 180 μm, the particle accounting 34.8wt% between 74 μm -180 μm, 53 μm -
Particle accounting 11.6wt% between 74 μm, the particle accounting 13.8wt% between 38.5 μm -53 μm, is less than 38.5 μm of particle
Accounting 39.8wt%.
8. high-nitrogen nickel-free powder of stainless steel according to claim 6, which is characterized in that the mobility of the powder of stainless steel
Control is between (20-21s)/50g.
9. high-nitrogen nickel-free powder of stainless steel according to claim 6, which is characterized in that the nitrogen content of the powder of stainless steel
More than 0.6wt%, carbon content is less than 0.05wt%, and oxygen content is less than 0.04wt%.
10. claim 6-9 any one of them high-nitrogen nickel-free powder of stainless steel is in injection moulding, body implant's manufacture view
Application.
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| CN111500942A (en) * | 2020-05-11 | 2020-08-07 | 湖南恒基粉末科技有限责任公司 | High-nitrogen-content non-magnetic stainless steel powder and preparation method thereof |
| CN112222416A (en) * | 2020-09-11 | 2021-01-15 | 广州有研粉体材料科技有限公司 | Preparation method of high-nitrogen non-magnetic nickel-free stainless steel ultrafine powder and metal powder |
| CN113604094A (en) * | 2021-06-30 | 2021-11-05 | 信和新材料（苏州）有限公司 | Filler, preparation method thereof and epoxy coating comprising filler |
| CN114734044A (en) * | 2022-04-02 | 2022-07-12 | 广州纳联材料科技有限公司 | High-nitrogen nickel-free stainless steel powder and preparation method and application thereof |
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| CN111500942A (en) * | 2020-05-11 | 2020-08-07 | 湖南恒基粉末科技有限责任公司 | High-nitrogen-content non-magnetic stainless steel powder and preparation method thereof |
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| CN112222416A (en) * | 2020-09-11 | 2021-01-15 | 广州有研粉体材料科技有限公司 | Preparation method of high-nitrogen non-magnetic nickel-free stainless steel ultrafine powder and metal powder |
| CN113604094A (en) * | 2021-06-30 | 2021-11-05 | 信和新材料（苏州）有限公司 | Filler, preparation method thereof and epoxy coating comprising filler |
| CN113604094B (en) * | 2021-06-30 | 2022-11-08 | 信和新材料（苏州）有限公司 | Filler, preparation method thereof and epoxy coating comprising filler |
| CN114734044A (en) * | 2022-04-02 | 2022-07-12 | 广州纳联材料科技有限公司 | High-nitrogen nickel-free stainless steel powder and preparation method and application thereof |
| CN114734044B (en) * | 2022-04-02 | 2024-04-23 | 广州纳联材料科技有限公司 | High-nitrogen nickel-free stainless steel powder and preparation method and application thereof |
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Application publication date: 20180921 |