CN108031851A - A kind of preparation method of austenitic stainless steel alloy - Google Patents
A kind of preparation method of austenitic stainless steel alloy Download PDFInfo
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- CN108031851A CN108031851A CN201711464460.XA CN201711464460A CN108031851A CN 108031851 A CN108031851 A CN 108031851A CN 201711464460 A CN201711464460 A CN 201711464460A CN 108031851 A CN108031851 A CN 108031851A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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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
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- 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
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F2003/145—Both compacting and sintering simultaneously by warm compacting, below debindering temperature
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- 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
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a kind of preparation method of austenitic stainless steel alloy, will be ground after iron powder, chromium powder and manganese uniformly mixing in the case where pressure is the blanket of nitrogen of 5MPa, drying and grinding product, obtains alloying Fe Cr Mn N powder；Alloying Fe Cr Mn N powder hot-pressings are sintered, is cooled to room temperature and can obtain the high-strength hard nickel-less austenitic stainless steel of height.Alloying element that the present invention uses is simple and relative low price, and preparation process is simple, easy to operate, its core procedure includes mechanical alloying powder and powder sintered, and mechanical alloying is powder sintered into bulk, obtains the high-strength hard nickel-less austenitic stainless steel of height.High-strength high hard nickel-less austenitic stainless steel prepared by this method has excellent mechanical property and preferable corrosion resisting property, has reached the requirement of high-strength high hard nickel-less austenitic stainless steel.
Description
Technical field
The invention belongs to materials processing technology field, and in particular to a kind of high-strength high hard nickel-less austenitic stainless steel and its system
Preparation Method.
Background technology
Stainless steel has good corrosion resisting property and comprehensive mechanical property, obtains fast development in many fields, especially
Austenitic stainless steel, because with good plasticity, weldability, high corrosion-resistant, toughness and low-temperature flexibility, nonmagnetic, workability
The advantages that, it is used widely in industries such as oil, chemical industry, food and medical instruments.But 304 and 316 traditional austenites are not
Rust steel has good plasticity, but low strength at room temperature, it is difficult to meets increasing performance requirement.Add into stainless steel
Add nitrogen to improve the intensity and corrosion resistance of stainless steel, and nickel resources can be saved, also solve current nickeliferous stainless
" nickel is quick " of human organ is endangered when steel is used as biologic medical material.Nitrogen has the following advantages as the element of substitution nickel：Nitrogen
It is a kind of formation and stable austenite phase p-block element p strongly, ferrite content in steel can be reduced and expand austenite phase
Area；Nitrogen can significantly improve hardness of steel at the same time, and not reduce its plasticity and toughness；Nitrogen can significantly improve the pitting potential of stainless steel,
1% nitrogen effect is suitable with 30%Cr.The conventional preparation techniques of high nitrogen steel are high pressure smelting processes, but device therefor is complicated, investment
It is huge, its industrial development and application is limited, and mechanical alloying has benefited from its energy height, powder is in machinery in preparation process
A large amount of fresh surfaces that solid-gas reaction occurs available for nitrogen and powder are formd under collision, can be relatively easy to be dissolved nitrogen
Into iron-based body, sintering bulk can obtain high nitrogen, even tissue, the stainless steel of crystal grain refinement, more application prospect.
The content of the invention
The purpose of the present invention is providing a kind of preparation method of high-strength high hard nickel-less austenitic stainless steel alloy, party's legal system
Standby high-strength high hard nickel-less austenitic stainless steel alloy has excellent mechanical property and preferable corrosion resistance, has reached height
The requirement of strong high hard nickel-less austenitic stainless steel.
To reach above-mentioned purpose, technology of preparing scheme that the present invention uses for：
A kind of preparation method of high-strength high hard nickel-less austenitic stainless steel alloy, comprises the following steps：
A kind of preparation method of austenitic stainless steel alloy, comprises the following steps：
1) it is 70 in mass ratio:18:12 by iron powder, chromium powder and manganese powder after mixing pressure be 4-6Mpa blanket of nitrogen
1~12h of lower grinding；Then the product after grinding is taken out, it is dry, alloying Fe-Cr-Mn-N powder is obtained, Vacuum Package is protected
Deposit；
2) by alloying Fe-Cr-Mn-N solid-solution powders made from step 1) pressure be 180-200MPa, temperature be
900~1000 DEG C, and 0.5~1h of hot pressed sintering under conditions of the protection of the argon gas with flowing；Naturally cooled to after the completion of sintering
Room temperature and release, obtain sintering bulk；
3) step 2) is made to the Fe-Cr-Mn-N bulks after sintering and carries out solution treatment, argon gas, temperature in flowing are
1.4h -1.6h is kept the temperature under conditions of 1150 DEG C ± 10 DEG C, then with distilled water water cooling, that is, obtains the high-strength hard nickel-less austenitic of height
Stainless steel.
The purity of the iron powder, chromium powder and manganese powder is >=99.8%, and granularity is 200 mesh with thin.
Grinding in the step 1) carries out in vibration rod mill, is first vacuumized before grinding and is re-filled with nitrogen gas progress
Protection against oxidation and alloying nitrogen source is used as, the rotating speed for setting vibration rod mill is 900~1000rmp/min, the vibration used
Rod is stainless steel, and bar ratio is 25:1~30:1.
In the step 1) after the completion of grinding, first vibration rod mill is vacuumized, is then filled with absolute ethyl alcohol thereto,
Continue it is wet after 30~35min of grinding take product, supernatant liquor is filtered off after product is stood, then be dried；The nothing being wherein filled with
The volume of water-ethanol is 15~18% of rod milling tank volume in vibration rod mill.
Drying in the step 1) is that powder to be dried is placed in vacuum drying chamber, it is evacuated to -0.8~-
0.95MPa, then heats to 70~75 DEG C of dry 10~12h.
The step) in nitrogen of the pressure for 5MPa is filled with into the mixture of every 300g iron, chromium and manganese powder end in grinding
Gas.
The Fe-Cr-Mn-N solid-solution powders after mechanical alloying are loaded inner surface lay in the step 2) graphite
In the sintered-carbide die of paper, jolt ramming, places into and hot pressed sintering is carried out in atmosphere protection hot-pressed sintering furnace.
In the step 2) when carrying out hot pressed sintering, 620--640MPa and pressurize 10- are first boosted at room temperature
20min, then reduces pressure and is warming up to 900~1000 DEG C to 180~200MPa, then with the programming rate of 8~10 DEG C/min, and
During be passed through the argon gas of flowing as protective gas, and 0.5~1h of hot pressed sintering under this condition.
Solution treatment in the step 3) carries out in vacuum tube furnace, and 10 are first evacuated to before solution treatment-3Pa, then
The argon gas of flowing is passed through as protective gas, then 1150 DEG C ± 10 DEG C of condition is warming up to the programming rate of 8~10 DEG C/min
Lower insulation 1.4h -1.6h, whole process are continually fed into the argon gas of flowing, after insulation it is rapid take out be put into distilled water into
Row water-cooled process.
Relative to the prior art, the invention has the advantages that：
The preparation method of high-strength high hard nickel-less austenitic stainless steel provided by the invention, iron powder, chromium powder and manganese are uniformly mixed
Ground after conjunction in the case where pressure is the blanket of nitrogen of 5MPa, drying and grinding product, obtains alloying Fe-Cr-Mn-N powder；By alloying
Fe-Cr-Mn-N powder hot-pressings sinter, and are cooled to room temperature and can obtain the high-strength hard nickel-less austenitic stainless steel of height.The present invention uses
Alloying element is simple and relative low price, preparation process is simple, easy to operate, its core procedure includes mechanical alloying system
Powder and powder sintered, mechanical alloying is powder sintered into bulk, obtain the high-strength hard nickel-less austenitic stainless steel of height.Party's legal system
Standby high-strength high hard nickel-less austenitic stainless steel has excellent mechanical property and preferable corrosion resisting property, has reached high-strength high hard
The requirement of nickel-less austenitic stainless steel.
High strength and high hardness austenite prepared by the present invention, tensile strength are 1178.63~1300.69MPa, and density is
7.60g/cm3 or so, its relative density are 873.75~915.50MPa up to 99% or so, 2% yield strength, and hardness is
480.76~487.96HV, density are 7.56~7.63g/cm3, elongation after fracture is 8.17~9.57%.Keeping preferably prolonging
While stretching rate, there is excellent mechanical property, disclosure satisfy that the use demand of special occasions.
The present invention has further the advantage that：
1) replace traditional reinforced iron-base element of volume such as nickel, molybdenum with the less expensive manganese of price and nitrogen and carry out alloying, reduce into
This is avoided harm of the nickel for human body at the same time.
2) pass through mechanical alloying using vibration rod mill, realize manganese and nitrogen that conventional method can not realize in iron
Over-saturation is dissolved, and can realize alloying process at a lower temperature for melting.
3) mode for carrying out hot pressed sintering using mould is taken to prepare bulk, including pressing technology and sintering temperature, technique
Simply, it is easy to operate, precipitation strength is achieveed the purpose that in sintering process, improves intensity and hardness.
4) mechanical alloying is combined with powder metallurgy, realizes that mechanical alloying powder is sintered in lower temperature, save
Financial cost.
5) nitride produced during mechanical alloying and hot pressed sintering, further enhancing are eliminated using solution treatment
Energy.
6) prepare high strength and high hardness austenite bulk tensile strength much larger than 304 stainless steels requirement (σ b >=
520MPa), while preferable elongation percentage is kept.
Embodiment
1) it is 70 in mass ratio:18:12 by iron powder, chromium powder and manganese powder after mixing pressure be 5Mpa blanket of nitrogen under
Grind 1~12h；Then the product after grinding is taken out, it is dry, alloying Fe-Cr-Mn-N powder is obtained, Vacuum Package preserves；
2) by obtained alloying Fe-Cr-Mn-N solid-solution powders pressure be 180-200MPa, temperature be 900~
1000 DEG C, and 0.5~1h of hot pressed sintering under conditions of the protection of the argon gas with flowing；Cooled to room temperature is simultaneously after the completion of sintering
Release, obtains sintering bulk；
3) the Fe-Cr-Mn-N bulks after obtained sintering are subjected to solution treatment, the argon gas, temperature in flowing are 1150 DEG C
Under conditions of keep the temperature 1.5h, then with distilled water water cooling, that is, obtain the high-strength hard nickel-less austenitic stainless steel of height.
The purity of the iron powder, chromium powder and manganese powder is >=99.8%, and granularity is 200 mesh with thin.
Grinding in the step 1) carries out in vibration rod mill, is first vacuumized before grinding and is re-filled with nitrogen gas progress
Protection against oxidation and alloying, the rotating speed for setting vibration rod mill are 900~1000rmp/min, and the vibrating head used is stainless
Steel material, bar ratio are 25:1~30:1.
In the step 1) after the completion of grinding, first vibration rod mill is vacuumized, is then filled with absolute ethyl alcohol thereto,
Continue it is wet after 30~35min of grinding take product, supernatant liquor is filtered off after product is stood, then be dried；The nothing being wherein filled with
The volume of water-ethanol is 15~18% of rod milling tank volume in vibration rod mill.
Drying in the step 1) is that powder to be dried is placed in vacuum drying chamber, it is evacuated to -0.8~-
0.95MPa, then heats to 70~75 DEG C of dry 10~12h.
It is filled with the nitrogen that pressure is 5MPa in the step 1) into the mixture of every 300g iron, chromium and manganese powder end in grinding
Gas.
The Fe-Cr-Mn-N solid-solution powders after mechanical alloying are loaded inner surface lay in the step 2) graphite
In the sintered-carbide die of paper, jolt ramming, places into and hot pressed sintering is carried out in atmosphere protection hot-pressed sintering furnace.
Hot pressed sintering middle progress in atmosphere protection hot-pressed sintering furnace in the step 2), when carrying out hot pressed sintering,
630MPa and pressurize 15min are first boosted at room temperature, then reduce pressure to 180~200MPa, then with 8~10 DEG C/min's
Programming rate is warming up to 900~1000 DEG C, and during be passed through the nitrogen of flowing as protective gas, and hot pressing under this condition
Sinter 0.5~1h.
Solution treatment in the step 3) carries out in vacuum tube furnace, and 10 are first evacuated to before solution treatment-3Pa, then
The argon gas of flowing is passed through as protective gas, then is warming up to 1150 DEG C with the programming rate of 8~10 DEG C/min and keeps the temperature 1.5h, it is whole
A process is continually fed into the argon gas of flowing, and rapid taking-up, which is put into distilled water, after insulation carries out water-cooled process.
High-strength high hard nickel-less austenitic made from the preparation method of the high-strength high hard nickel-less austenitic stainless steel is stainless
Steel alloy, its tensile strength are 1178.63~1300.69MPa, and 2% yield strength is 873.75~915.50MPa, and hardness is
480.76~487.96HV, density 7.60g/cm3Left and right, elongation after fracture are 8.17~9.57%.
The high-strength hard nickel-less austenitic stainless steel of height prepared by the present invention, its key are alloy element species and content,
The core of preparation method is to be combined mechanical alloying with powder metallurgy, and chromium, manganese element are realized by mechanical alloying
With solid solution of the nitrogen in iron, by the copper powders sinter molding of alloying and analysis is dissolved using the hot pressed sintering of powder metallurgy
Go out, so that obtaining high intensity has preferably moulding stainless steel bulk again.The preparation method include machinery powder, hot pressed sintering and
Solution treatment three parts, wherein the technology point of machinery powder processed is：
1) it is 70 in mass ratio:18:Iron powder, chromium powder and the common 300g of manganese powder are added vibration rod mill by 12 after mixing
In, the wherein iron powder of commodity in use, chromium powder and manganese powder, purity to analyze pure (purity >=99.8%), granularity for 200 mesh with
Carefully.It is 25 by bar ratio:1~30:1 adds the vibrating head of stainless steel, and every about 215g, first vacuumizes before rod milling and be filled with afterwards
Nitrogen sets vibration rod mill rotating speed as 900~1000rmp/min, is shut down after grinding 1~12h as nitrogen source and protective gas.
2) vibration rod mill is vacuumized after grinding, is then filled with the absolute ethyl alcohol (volume of absolute ethyl alcohol thereto
For 15~18% of rod milling tank volume in vibration rod mill, continue it is wet after 30~35min of grinding take product, filtered after product is stood
Remove supernatant liquor, be placed in vacuum drying chamber, be evacuated to -0.8~-0.95MPa, then heat to 70~75 DEG C of dryings 10~
12h, obtains alloying Fe-Cr-Mn-N solid-solution powders, and Vacuum Package preserves.
The technology point of hot pressed sintering is：
One layer of graphite paper first is laid in sintered-carbide die cavity inner surface, reproducibility environment is formed, avoids powder from burning
Oxidation during knot, while be conducive to sample after the completion of sintering.Then the Fe-Cr-Mn-N solid-solution powders of alloying are seated in
In sintered-carbide die, jolt ramming, is placed in hot-pressed sintering furnace, while is passed through the nitrogen of flowing as protective gas.Rise at room temperature
300MPa and pressurize 15min are depressed into, reduces pressure to 180~200MPa, 900 are warming up to the programming rate of 10 DEG C/min~
1000 DEG C, 0.5~1h of hot pressed sintering under this condition；Cooled to room temperature and release, are removed from the molds after the completion of sintering,
Obtain alloy cube matherial.Atmosphere protection hot-pressed sintering furnace is made of 200t hydraulic presses and open type burner hearth, can atmosphere protection, highest adds
Hot temperature is up to 1200 DEG C, it is ensured that middle pressure sintering process parameter is realized.
The technology point of powder solution treatment is：
Fe-Cr-Mn-N bulks after obtained sintering are put into vacuum tube furnace, are first evacuated to vacuum tube furnace
10-3Pa, then the argon gas of flowing is passed through as protective gas, then be warming up to 1150 DEG C with the programming rate of 8~10 DEG C/min and protect
Warm 1.5h, whole process are continually fed into the argon gas of flowing, and rapid taking-up, which is put into distilled water, after insulation carries out water-cooled process.
Solution treatment can be eliminated since nitrogen is not dissolved the nitride of generation completely, nitrogen is dissolved into completely in iron matrix lattice.
The tensile strength of high-strength high hard nickel-less austenitic stainless steel produced by the present invention is 1178.63~1300.69MPa
MPa, 2% yield strength are 873.75~915.50MPa, strong far more than the surrenders of 304 stainless steel tensile strength >=520Mpa and 2%
The requirement of degree >=205Mpa.Stainless steel density (presses Fe=7.86g/cm3, Cr up to 7.60g/cm3 or so with theoretical density
=7.20g/cm3, Mn=7.44g/cm3 are calculated) compare, its relative density is up to 99% or so.Hardness number up to 480.76~
487.96HV is 304 stainless steel hardness (200HV) of market more than twice.Elongation percentage, which also reaches prior powder metallurgy, at the same time to reach
9% or so arrived, while preferable elongation percentage is kept, has excellent mechanical property, disclosure satisfy that the use of special occasions
Demand.
Elaborated below with embodiment to the present invention, described is explanation of the invention, and unrestricted.
Embodiment 1：
1) it is 70 in mass ratio:18:Iron powder, chromium powder and the common 300g of manganese powder are added vibration rod mill by 12 after mixing
In, wherein the iron powder of commodity in use, chromium powder and manganese powder, purity are that analysis is pure, and granularity is 200 mesh with thin.It is 30 by bar ratio:
1 adds the stainless steel bar that 42 quality are 215g, is first vacuumized before rod milling and is filled with nitrogen gas afterwards as nitrogen source and protective gas, if
It is 900rmp/min to determine vibration rod mill rotating speed, is shut down after grinding 4h.
2) vibration rod mill is vacuumized after grinding, is then filled with the absolute ethyl alcohol (volume of absolute ethyl alcohol thereto
For in vibration rod mill rod milling tank volume 15%), continue grind 50min after it is wet take product, filter off upper strata after product is stood
Clear liquid, is placed in vacuum drying chamber, is evacuated to -0.8MPa, then heats to 75 DEG C of dry 10h, obtains alloying Fe-Cr-
Mn-N solid-solution powders, Vacuum Package preserve.
3) one layer of graphite paper is laid in sintered-carbide die cavity inner surface, reproducibility environment is formed, by mechanical alloying
Fe-Cr-Mn-N solid-solution powders afterwards are seated in sintered-carbide die, and jolt ramming, is placed in hot-pressed sintering furnace, while are passed through stream
Dynamic argon gas forms protective atmosphere.Boost to 630MPa and pressurize 15min at room temperature, reduce pressure to 200MPa, with 10 DEG C/
The programming rate of min is warming up to 900~1000 DEG C, under this condition hot pressed sintering 1h；Cooled to room temperature after the completion of sintering
And release, it is removed from the molds, obtains Fe-Cr-Mn-N solid solution bulks.
4) Fe-Cr-Mn-N solid solution bulks are put into vacuum tube furnace, vacuum tube furnace is first evacuated to 10-3Pa,
Then pass to that the argon gas of flowing is anti-oxidation, then 1150 DEG C are risen to the programming rate of 10 DEG C/min, and keep the temperature 1.5h, whole process
It is continually fed into argon gas and forms protection atmosphere, insulation terminates to take out to be put into distilled water rapidly to carry out water cooling, that is, obtains high-strength high hard
Nickel-less austenitic stainless steel.
Embodiment 2：
1) it is 70 in mass ratio:18:Iron powder, chromium powder and the common 300g of manganese powder are added vibration rod mill by 12 after mixing
In, wherein the iron powder of commodity in use, chromium powder and manganese powder, purity are that analysis is pure, and granularity is 200 mesh with thin.It is 30 by bar ratio:
1 adds the stainless steel bar that 42 quality are 215g, is first vacuumized before rod milling and is filled with nitrogen gas afterwards as nitrogen source and protective gas, if
It is 900rmp/min to determine vibration rod mill rotating speed, is shut down after grinding 8h.
2) vibration rod mill is vacuumized after grinding, is then filled with the absolute ethyl alcohol (volume of absolute ethyl alcohol thereto
For in vibration rod mill rod milling tank volume 15%), continue grind 50min after it is wet take product, filter off upper strata after product is stood
Clear liquid, is placed in vacuum drying chamber, is evacuated to -0.85MPa, then heats to 75 DEG C of dry 10h, obtains alloying Fe-Cr-
Mn-N solid-solution powders, Vacuum Package preserve.
3) one layer of graphite paper is laid in sintered-carbide die cavity inner surface, reproducibility environment is formed, by mechanical alloying
Fe-Cr-Mn-N solid-solution powders afterwards are seated in sintered-carbide die, and jolt ramming, is placed in hot-pressed sintering furnace, while are passed through stream
Dynamic argon gas forms protective atmosphere.Boost to 630MPa and pressurize 15min at room temperature, reduce pressure to 200MPa, with 10 DEG C/
The programming rate of min is warming up to 900~1000 DEG C, under this condition hot pressed sintering 1h；Cooled to room temperature after the completion of sintering
And release, it is removed from the molds, obtains Fe-Cr-Mn-N solid solution bulks.
4) Fe-Cr-Mn-N solid solution bulks are put into vacuum tube furnace, vacuum tube furnace is first evacuated to 10-3Pa,
Then pass to that the argon gas of flowing is anti-oxidation, then 1150 DEG C are risen to the programming rate of 10 DEG C/min, and keep the temperature 1.5h, whole process
It is continually fed into argon gas and forms protection atmosphere, insulation terminates to take out to be put into distilled water rapidly to carry out water cooling, that is, obtains high-strength high hard
Nickel-less austenitic stainless steel.
Embodiment 3：
1) it is 70 in mass ratio:18:Iron powder, chromium powder and the common 300g of manganese powder are added vibration rod mill by 12 after mixing
In, wherein the iron powder of commodity in use, chromium powder and manganese powder, purity are that analysis is pure, and granularity is 200 mesh with thin.It is 30 by bar ratio:
1 adds the stainless steel bar that 42 quality are 215g, is first vacuumized before rod milling and is filled with nitrogen gas afterwards as nitrogen source and protective gas, if
It is 900rmp/min to determine vibration rod mill rotating speed, is shut down after grinding 12h.
2) vibration rod mill is vacuumized after grinding, is then filled with the absolute ethyl alcohol (volume of absolute ethyl alcohol thereto
For in vibration rod mill rod milling tank volume 15%), continue grind 50min after it is wet take product, filter off upper strata after product is stood
Clear liquid, is placed in vacuum drying chamber, is evacuated to -0.9MPa, then heats to 75 DEG C of dry 10h, obtains alloying Fe-Cr-
Mn-N solid-solution powders, Vacuum Package preserve.
3) one layer of graphite paper is laid in sintered-carbide die cavity inner surface, reproducibility environment is formed, by mechanical alloying
Fe-Cr-Mn-N solid-solution powders afterwards are seated in sintered-carbide die, and jolt ramming, is placed in hot-pressed sintering furnace, while are passed through stream
Dynamic argon gas forms protective atmosphere.Boost to 630MPa and pressurize 15min at room temperature, reduce pressure to 200MPa, with 10 DEG C/
The programming rate of min is warming up to 900~1000 DEG C, under this condition hot pressed sintering 1h；Cooled to room temperature after the completion of sintering
And release, it is removed from the molds, obtains Fe-Cr-Mn-N solid solution bulks.
4) Fe-Cr-Mn-N solid solution bulks are put into vacuum tube furnace, vacuum tube furnace is first evacuated to 10-3Pa,
Then pass to that the argon gas of flowing is anti-oxidation, then 1150 DEG C are risen to the programming rate of 10 DEG C/min, and keep the temperature 1.5h, whole process
It is continually fed into argon gas and forms protection atmosphere, insulation terminates to take out to be put into distilled water rapidly to carry out water cooling, that is, obtains high-strength high hard
Nickel-less austenitic stainless steel.
Embodiment 4：
1) it is 70 in mass ratio:18:Iron powder, chromium powder and the common 300g of manganese powder are added vibration rod mill by 12 after mixing
In, wherein the iron powder of commodity in use, chromium powder and manganese powder, purity are that analysis is pure, and granularity is 200 mesh with thin.It is 30 by bar ratio:
1 adds the stainless steel bar that 42 quality are 215g, is first vacuumized before rod milling and is filled with nitrogen gas afterwards as nitrogen source and protective gas, if
It is 900rmp/min to determine vibration rod mill rotating speed, is shut down after grinding 8h.
2) vibration rod mill is vacuumized after grinding, is then filled with the absolute ethyl alcohol (volume of absolute ethyl alcohol thereto
For in vibration rod mill rod milling tank volume 15%), continue grind 50min after it is wet take product, filter off upper strata after product is stood
Clear liquid, is placed in vacuum drying chamber, is evacuated to -0.8MPa, then heats to 75 DEG C of dry 10h, obtains alloying Fe-Cr-
Mn-N solid-solution powders, Vacuum Package preserve.
3) one layer of graphite paper is laid in sintered-carbide die cavity inner surface, reproducibility environment is formed, by mechanical alloying
Fe-Cr-Mn-N solid-solution powders afterwards are seated in sintered-carbide die, and jolt ramming, is placed in hot-pressed sintering furnace, while are passed through stream
Dynamic argon gas forms protective atmosphere.Boost to 630MPa and pressurize 15min at room temperature, reduce pressure to 180MPa, with 10 DEG C/
The programming rate of min is warming up to 900~1000 DEG C, under this condition hot pressed sintering 1h；Cooled to room temperature after the completion of sintering
And release, it is removed from the molds, obtains Fe-Cr-Mn-N solid solution bulks.
4) Fe-Cr-Mn-N solid solution bulks are put into vacuum tube furnace, vacuum tube furnace is first evacuated to 10-3Pa,
Then pass to that the argon gas of flowing is anti-oxidation, then 1150 DEG C are risen to the programming rate of 10 DEG C/min, and keep the temperature 1.5h, whole process
It is continually fed into argon gas and forms protection atmosphere, insulation terminates to take out to be put into distilled water rapidly to carry out water cooling, that is, obtains high-strength high hard
Nickel-less austenitic stainless steel.
Embodiment 5
1) it is 70 in mass ratio:18:Iron powder, chromium powder and the common 300g of manganese powder are added vibration rod mill by 12 after mixing
In, wherein the iron powder of commodity in use, chromium powder and manganese powder, purity are that analysis is pure, and granularity is 200 mesh with thin.It is 30 by bar ratio:
1 adds the stainless steel bar that 42 quality are 215g, is first vacuumized before rod milling and is filled with nitrogen gas afterwards as nitrogen source and protective gas, if
It is 900rmp/min to determine vibration rod mill rotating speed, is shut down after grinding 8h.
2) vibration rod mill is vacuumized after grinding, is then filled with the absolute ethyl alcohol (volume of absolute ethyl alcohol thereto
For in vibration rod mill rod milling tank volume 15%), continue grind 50min after it is wet take product, filter off upper strata after product is stood
Clear liquid, is placed in vacuum drying chamber, is evacuated to -0.8MPa, then heats to 75 DEG C of dry 10h, obtains alloying Fe-Cr-
Mn-N solid-solution powders, Vacuum Package preserve.
3) one layer of graphite paper is laid in sintered-carbide die cavity inner surface, reproducibility environment is formed, by mechanical alloying
Fe-Cr-Mn-N solid-solution powders afterwards are seated in sintered-carbide die, and jolt ramming, is placed in hot-pressed sintering furnace, while are passed through stream
Dynamic argon gas forms protective atmosphere.Boost to 630MPa and pressurize 15min at room temperature, reduce pressure to 190MPa, with 10 DEG C/
The programming rate of min is warming up to 900~1000 DEG C, under this condition hot pressed sintering 1h；Cooled to room temperature after the completion of sintering
And release, it is removed from the molds, obtains Fe-Cr-Mn-N solid solution bulks.
4) Fe-Cr-Mn-N solid solution bulks are put into vacuum tube furnace, vacuum tube furnace is first evacuated to 10-3Pa,
Then pass to that the argon gas of flowing is anti-oxidation, then 1150 DEG C are risen to the programming rate of 10 DEG C/min, and keep the temperature 1.5h, whole process
It is continually fed into argon gas and forms protection atmosphere, insulation terminates to take out to be put into distilled water rapidly to carry out water cooling, that is, obtains high-strength high hard
Nickel-less austenitic stainless steel.
The preparation method of high strength and high hardness Austria formula body stainless steel provided by the invention, its hot pressed sintering under different pressure
The copper alloy bulk of acquisition, its performance data is as follows after tested：
The properties of the high-strength high hard nickel-less austenitic stainless steel produced by the present invention of table 1
Through experiment test, high strength and high hardness Austria formula body stainless steel provided by the invention, utilizes mechanical alloying and hot pressing
Sintering processing prepares, and possesses excellent mechanical property, while keeps preferable elongation percentage, disclosure satisfy that special occasions needs
Will.
Claims (9)
1. a kind of preparation method of austenitic stainless steel alloy, it is characterised in that comprise the following steps：
1) it is 70 in mass ratio:18:12 grind iron powder, chromium powder and manganese powder in the case where pressure is the blanket of nitrogen of 4-6Mpa after mixing
Grind 1~12h；Then the product after grinding is taken out, it is dry, alloying Fe-Cr-Mn-N powder is obtained, Vacuum Package preserves；
2) by alloying Fe-Cr-Mn-N solid-solution powders made from step 1) pressure be 180-200MPa, temperature be 900~
1000 DEG C, and 0.5~1h of hot pressed sintering under conditions of the protection of the argon gas with flowing；Cooled to room temperature is simultaneously after the completion of sintering
Release, obtains sintering bulk；
3) step 2) is made to the Fe-Cr-Mn-N bulks after sintering and carries out solution treatment, argon gas, temperature 1150 in flowing
1.4h -1.6h is kept the temperature under conditions of DEG C ± 10 DEG C, then with distilled water water cooling, that is, it is stainless to obtain high-strength high hard nickel-less austenitic
Steel.
A kind of 2. preparation method of austenitic stainless steel alloy according to claim 1, it is characterised in that：The iron
The purity of powder, chromium powder and manganese powder is >=99.8%, and granularity is 200 mesh with thin.
A kind of 3. preparation method of austenitic stainless steel alloy according to claim 1, it is characterised in that：The step 1)
In grinding carried out in vibration rod mill, grinding before first vacuumize be re-filled with nitrogen gas carry out protection against oxidation and as conjunction
Aurification nitrogen source, the rotating speed for setting vibration rod mill are 900~1000rmp/min, and the vibrating head used is stainless steel, bar
Than for 25:1~30:1.
A kind of 4. preparation method of austenitic stainless steel alloy according to claim 1, it is characterised in that：The step 1)
In after the completion of grinding, first vibration rod mill is vacuumized, is then filled with absolute ethyl alcohol thereto, continues 30~35min of grinding
It is wet afterwards to take product, supernatant liquor is filtered off after product is stood, then be dried；The volume for the absolute ethyl alcohol being wherein filled with is vibration
The 15~18% of rod milling tank volume in rod mill.
A kind of 5. preparation method of austenitic stainless steel alloy according to claim 1, it is characterised in that：The step 1)
In drying be that powder to be dried is placed in vacuum drying chamber, be evacuated to -0.8~-0.95MPa, then heat to 70
~75 DEG C of dry 10~12h.
A kind of 6. preparation method of austenitic stainless steel alloy according to claim 1, it is characterised in that：The step)
In nitrogen of the pressure for 5MPa is filled with into the mixture of every 300g iron, chromium and manganese powder end in grinding.
A kind of 7. preparation method of austenitic stainless steel alloy according to claim 1, it is characterised in that：The step 2)
The middle Fe-Cr-Mn-N solid-solution powders by after mechanical alloying, which are fitted into inner surface lay, to be had in the sintered-carbide die of graphite paper,
Jolt ramming, places into and hot pressed sintering is carried out in atmosphere protection hot-pressed sintering furnace.
A kind of 8. preparation method of austenitic stainless steel alloy according to claim 1, it is characterised in that：The step 2)
In when carrying out hot pressed sintering, first boost to 620--640MPa and pressurize 10-20min at room temperature, then reduce pressure extremely
180~200MPa, then 900~1000 DEG C are warming up to the programming rate of 8~10 DEG C/min, and during be passed through the argon gas of flowing
As protective gas, and 0.5~1h of hot pressed sintering under this condition.
A kind of 9. preparation method of austenitic stainless steel alloy according to claim 1, it is characterised in that：The step 3)
In solution treatment carried out in vacuum tube furnace, 10 are first evacuated to before solution treatment-3Pa, then it is passed through the argon gas conduct of flowing
Protective gas, then 1.4h -1.6h is kept the temperature under conditions of being warming up to 1150 DEG C ± 10 DEG C with the programming rate of 8~10 DEG C/min, it is whole
A process is continually fed into the argon gas of flowing, and rapid taking-up, which is put into distilled water, after insulation carries out water-cooled process.
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