CN103801691A - Nitrogenous stainless steel product with manner of solid of revolution and manufacturing method thereof - Google Patents
Nitrogenous stainless steel product with manner of solid of revolution and manufacturing method thereof Download PDFInfo
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- CN103801691A CN103801691A CN201410016941.4A CN201410016941A CN103801691A CN 103801691 A CN103801691 A CN 103801691A CN 201410016941 A CN201410016941 A CN 201410016941A CN 103801691 A CN103801691 A CN 103801691A
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Abstract
The invention discloses a nitrogenous stainless steel product with a manner of a solid of revolution and a manufacturing method of the nitrogenous stainless steel product. The method includes the following steps that a package casing with the manner of the solid of revolution is designed; the package casing with the manner of the solid of revolution is manufactured, powder filling is carried out, degassing is carried out, hot isostatic pressure is exerted. In the step of manufacturing the package casing with the manner of the solid of revolution, the package casing is manufactured by means of a flow forming technology. The flow forming process is divided into six to fifteen passes to be carried out, the deformation of each pass is 7%-17% and the annealing treatment is carried out on a package casing blank between all the passes. A blank body obtained through the method is close to the shape of a final product, the raw material utilization rate is improved and the subsequent machining difficulty is lowered.
Description
Technical field
The invention belongs to field of powder metallurgy, particularly a kind of nitrogen-contained stainless steel goods with revolving body form and preparation method thereof.
Background technology
The thirties in 20th century and the later stage forties, the in short supply stimulation with nitrogen of nickel resources prepared stainless research for nickel.Researcher's discovery, nitrogen can not only improve the intensity of Steel material, and to improving the corrosion resistance of material, especially also there is material impact anti-chlorine ion spot corrosion aspect.The preparation technology of nitrogen-contained stainless steel product mainly contains: pressurized Induction Melting, high temperature insostatic pressing (HIP) melting, high pressure plasma melting, pressurization electroslag melting, back-pressure casting, the nitriding of electroslag heating-high pressure, powder metallurgy etc.Compare with melting nitrogen-contained stainless steel, powder metallurgic method is prepared nitrogen-contained stainless steel and is had many merits, the product that for example can obtain evening chemical composition and microstructure, can add nitrogen in different phase, has and reaches the advantages such as possibility, the technique of high nitrogen-containing is very flexible.Therefore, the method is just being widely used in the research of nitrogen-contained stainless steel.
At present, the main method that powder metallurgy is prepared nitrogen-contained stainless steel powder has: high pressure nitrogen melting-nitrogen atomization method; Fluid bed nitriding method; Mechanical alloying method etc.Obtaining after nitrogen-contained stainless steel, a crucial step is the shaping of powder, because nitrogen-contained stainless steel powder surface is coated with the nitride that hardness is larger, hinder the distortion of powder particle in pressing process, thereby made formability and the agglutinating property variation of nitrogen-contained stainless steel powder.
Mainly comprise preparing the powder forming method using in powder metallurgy nitrogen-contained stainless steel:
(1) injection molding method, for example, the utilization Powder Injection Molding Technologies such as Rawers are made nitrogenous 316L stainless steel (Rawers J., Croydon F., Krabbe R., Duttinger N.Tensile Characteristics of Nitrogen Enhanced Powder Injection Moulded316L Stainless Steel.Powder Metallurgy, 1996,39:125-129.).
(2) hot extrusion method: the people such as Simmons are contained in a certain amount of nitrogenous powder compacting in the carbon steel pipes of certain size, dry, then steel pipe are heated to and the corresponding temperature of nitrogenous steel solution heat treatment.After insulation a period of time; under certain extruding force, hot extrude is pressed onto required size, heat-treats (Simmons J.W., Kemp W.E. after finishing; Dunning J.S.The P/M Processing of High-Nitrogen Stainless Steel.JOM, 1996; (4): 20).
(3) powder forging rolling method: ASP company of Sweden utilizes powder forging rolling technology to make the nitrogenous high-speed steel that performance is very excellent, and put into production (ASP intra-company of Sweden data).
(4) Aeroform method: Zhou Candong etc. utilize Aeroform method prepare nitrogenous 35CrMoV steel (Zhou Candong. the preparation of nitrogenous 35CrMoV steel and research [D]. Shanghai: publishing house of Shanghai University, 2002:52.).
(5) hot isostatic pressing method: Crucible company of the U.S. adopts this method to produce powder metallurgy nitrogen-contained stainless steel material, its technological parameter adopting is 1130 ℃, 100MPa, be incubated 4 hours (G.O.Rhodes, W.B.Eisen. " High Nitrogen Corrosion Resistant Austenitic Stainless Steels Produced by HIP P/M Processing; " Materials Science Forum1999, pp.635-648.).
For the shaping of nitrogen-contained stainless steel powder, all there are some shortcomings in said method.Injection molding method shortcoming is: the mobility to powder, particle size require strict, and in powder, nitrogen content is wayward, easily causes nitriding or denitrogenation, and sample compactness is poor; Hot extrusion shortcoming is that energy consumption is high, sample size is little, cannot prepare the goods that contain spill, the complicated shape such as hollow; Powder forging rolling method shortcoming is general to be only generally no more than 10mm for the production of Strip and thickness of strip, cannot production large scale, complex-shaped sample; Aeroform method shortcoming is industrialization difficulty.
Hot isostatic pressing method is convenient to large-scale industrial production, but different heat and other static pressuring processes parameters exerts an influence the performance to nitrogen-contained stainless steel and tissue, and wherein technological parameter mainly comprises sintering temperature, sintering pressure and temperature retention time.Crucible company of the U.S. adopts hot isostatic pressing method to have that sintering temperature is low, sintering pressure is low while preparing nitrogen-contained stainless steel material and the problem such as temperature retention time is long.
Therefore, applicable heat and other static pressuring processes parameter can make nitrogen-contained stainless steel obtain good mechanics and microstructure, also can enhance productivity simultaneously, reduces production costs, thereby makes nitrogen-contained stainless steel product more competitive.
In addition, while adopting heat and other static pressuring processes to prepare stainless steel parts, the prismatic cylindrical or cuboid jacket of general employing, after powder is densified by high temperature insostatic pressing (HIP), also need larger processing capacity could obtain final part product, utilization rate of raw materials is low, and particularly high for cost of material and be difficult to mach stainless steel material, traditional jacket form restricts its application and popularization.
Summary of the invention
For the defect of prior art, the object of the present invention is to provide a kind of preparation method of the nitrogen-contained stainless steel goods with revolving body form.This preparation method adopts heat and other static pressuring processes, can solve nitrogen-contained stainless steel powder forming difficulty, nitrogen content is wayward, goods compactness is poor, size is little, industrialization is difficult, production efficiency is low shortcoming.And the present invention also adopts near-net-shape technology, approach the revolving body jacket of product net shape by employing, can improve stock utilization, reduce follow-up amount of machining, reduce costs.
Another object of the present invention is to provide a kind of nitrogen-contained stainless steel goods with revolving body form that adopt said method to prepare.
In order to achieve the above object, the present invention is achieved in that
A preparation method with the nitrogen-contained stainless steel goods of revolving body form, comprises the following steps: the jacket of design revolving body form, the jacket of preparing revolving body form, dress powder, degassed and high temperature insostatic pressing (HIP) step, wherein:
In the described jacket step of preparing revolving body form, described jacket adopts spinning process preparation, and wherein, described spinning process is divided into 6-15 passage to carry out, and the deflection of each passage is 7-17%, and all jacket base is carried out to annealing in process between each passage.
In above-mentioned preparation method, exemplarily, described spinning process is divided into 6,8,10,13 or 15 passages to carry out, and the deflection of each passage is 7%, 10%, 12% or 16%.
In above-mentioned preparation method, as a kind of preferred embodiment, in the described jacket step of preparing revolving body form, temperature when described annealing in process is 500 ℃-1200 ℃, and temperature retention time is 0.25-3 hour.Exemplarily, temperature when described annealing in process is 500 ℃, 600 ℃, 750 ℃, 800 ℃, 900 ℃, 1050 ℃, 1160 ℃ or 1200 ℃, and temperature retention time is 0.5h, 0.h8,1h, 1.5h, 2.0h, 2.5h or 2.8h.More preferably, temperature when described annealing in process is 600 ℃-700 ℃, and temperature retention time is 1-2 hour.
The jacket that adopts above-mentioned spinning process to prepare has the advantages that wall thickness is even and thickness is controlled, has avoided the appearance of work hardening simultaneously, has retained plasticity and the welding characteristic of jacket.The jacket that adopts above-mentioned spinning process to prepare, its diameter of section can increase continuously or reduce, and unconventional fixed diameter.
In above-mentioned preparation method, as a kind of preferred embodiment, in the jacket step of described design revolving body form, according to the jacket of numerical model design revolving body form, powder yield function is following formula:
Wherein, σ
yfor single shaft yield stress, σ ' is deviatoric stress component tensor, and P is hydrostatic pressure, γ=ρ
a, β=(1-ρ)
b2, wherein ρ is relative density, be that 1-3.5(is such as the value of a is 1,1.2,1.5,1.8,2.0,2.1,2.3,2.4,2.5,2.7,2.9,3.1,3.2,3.4 according to the different a spans of material composition), b span is that 0.2-1(is such as the value of b is 0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9,1.0).
Preferably, described jacket diameter range is 100mm～1500mm, and altitude range is 200mm～2000mm.
In above-mentioned preparation method, as a kind of preferred embodiment, the material of described jacket is mild steel, stainless steel, nickel or molybdenum.
In above-mentioned preparation method, as a kind of preferred embodiment, described dress powder step refers to nitrogen-contained stainless steel powder packed in described jacket and sealing jacket, preferably, the particle of described nitrogen-contained stainless steel powder is less than or equal to 250 μ m, this nitrogen-contained stainless steel powder is made up of following chemical composition according to mass percent: Cr20.0～35%, Mn0.1～10%, Mo0.1～6%, Si0.1～1.0%, N0.4～1.5%, Ni5～25%, all the other are Fe and inevitable impurity.
In above-mentioned preparation method, as a kind of preferred embodiment, described degassed step refers to degassed vacuum in jacket to≤10
-3pa.Avoid in jacket powder oxidized in order to make in jacket vacuum reach above-mentioned requirements simultaneously, whole degassed step is preferably carried out in two steps: the first step, jacket is placed in to room temperature degassed to vacuum < 10Pa, because at room temperature degassed, in jacket, powder is difficult for oxidized, and when in jacket when vacuum < 10Pa, oxygen content is little, can avoid in follow-up jacket heat de-airing powder oxidized; Second step, it is degassed under the condition of 100～800 ℃ that jacket is placed in to temperature, finally makes vacuum≤10 in jacket
-3pa because jacket heated after, inner residual gas expands, and carries out degassed residual gas content in jacket further being reduced simultaneously, finally reaches production requirement, vacuum≤10
-3pa.
In above-mentioned preparation method, as a kind of preferred embodiment, in described high temperature insostatic pressing (HIP) step, jacket cold charge after degassed is entered in high temperature insostatic pressing (HIP) cylinder body, to carry out hip treatment, wherein: sintering temperature is 1135～1350 ℃, sintering pressure is 110～180MPa, and temperature retention time is 0.5～3h.Preferably, the pressure medium of described high temperature insostatic pressing (HIP) is helium or argon gas.When sintering temperature declines lower than the sintered density of 1135 ℃ of materials, higher than 1350 ℃ of abnormal grain growths, make processing cost improve simultaneously; Sintering pressure is lower than 110MPa, and the sintered density of material declines, and higher than 180MPa, be favourable, but pressure is higher to improving material density, and the requirement of equipment is also higher, and material manufacturing cost significantly improves; When temperature retention time is less than 0.5h, material can not reach complete densification, and exceedes 3h, makes material grains grow up, the production efficiency that simultaneously increased Energy Intensity Reduction.
Nitrogen-contained stainless steel goods with revolving body form that adopt said method to prepare, the product after high temperature insostatic pressing (HIP) possesses nearly end form; Preferably, the diameter range of described goods is 100mm～1500mm, and altitude range is 200mm～2000mm; More preferably, described nitrogen-contained stainless steel goods are cone cartridge type.
The stainless steel products obtaining by said method at least has one of following performance: nitrogen content is high, density >=99.9%, and tensile strength is 980～1040MPa, yield strength is 625～675MPa, percentage elongation is 28.5～49.0%, and the contraction percentage of area is 27.5～60.0%, and ballistic work is 24～89J.
The principle of the invention is: according to the jacket of numerical model design revolving body form, adopt spinning to prepare the jacket of revolving body form in conjunction with Technology for Heating Processing, take nitrogen-contained stainless steel powder as raw material, powder carries out high temperature insostatic pressing (HIP) in the jacket with revolving body form, the stainless steel products crystal grain that adopts above-mentioned technique to obtain is tiny, and eliminated the intergranular defect of material internal and hole, improved density and the intensity of material, the base substrate after high temperature insostatic pressing (HIP) approaches end article shape.
Compared with prior art, beneficial effect of the present invention is:
1) can make density >=99.9%, approach the final revolving body nitrogen-contained stainless steel part that uses profile, improve utilization rate of raw materials, reduce following process difficulty.
2), compared with existing heat and other static pressuring processes, by improving sintering temperature and sintering pressure, shorten sintering time, thereby improved operating efficiency in obtaining high-performance nitrogen-contained stainless steel goods.
Accompanying drawing explanation
Fig. 1 is part section schematic diagram prepared by embodiment 3.
The specific embodiment
Following examples are used for further illustrating the present invention, and non-limiting its scope.
Embodiment 1
The particle mean size that the present embodiment is chosen is that the nitrogenous super austenitic powder of stainless steel of 178 μ m is raw material, and the composition of this powder according to mass percent is: 28.15%Cr, and 6.22%Mn, 2.11%Mo, 0.5%Si, 0.76%N, 10.12%Ni, all the other are Fe.
Adopt above-mentioned raw materials preparation to have the part of cone cartridge type, this part is of a size of: bottom surface internal diameter 210mm, external diameter 390mm, end face internal diameter 80mm, external diameter 135mm, height 340mm.
Preparation method is as follows:
1) jacket design: according to the jacket of numerical model design revolving body form, powder yield function is following formula:
Wherein, σ
yfor single shaft yield stress, σ ' is deviatoric stress component tensor, and P is hydrostatic pressure, γ=ρ
a, β=(1-ρ)
b2, wherein ρ is relative density, and a is that 2.4, b is 0.4.
First design jacket original shape, simulate on computers in hot isostatic pressing, under isostatic pressure, there is the yield function that the condition of plastic deformation obtains by above formula and determined in the powder aggregate in jacket, rear relative density is shunk in the plastic deformation of powder aggregate to be increased, until no longer to there is plastic deformation in powder completely densified, the monnolithic case size of actual required goods and jacket after the final appearance and size of jacket more at this moment obtaining and high temperature insostatic pressing (HIP) (being sintered body and outer jacket thereof after actual required high temperature insostatic pressing (HIP)), change initial jacket shape design if inconsistent, repeat said process, until the monnolithic case consistent size of actual required goods and jacket after the jacket appearance and size of calculating and high temperature insostatic pressing (HIP), obtain the design jacket of end article, jacket is specifically of a size of: bottom surface internal diameter 220mm, external diameter 420mm, end face internal diameter 80mm, external diameter 150mm, be highly 380mm, the material of jacket is mild steel.
2) jacket preparation: adopt spinning process to prepare the mild steel jacket of the barrel-shaped formula of above-mentioned cone, spinning process is divided into 6 passages to carry out, and each pass deformation is 15-17%, and between passage, annealing temperature is 650 ℃, and temperature retention time is 1h.
3) dress powder and degassed: nitrogen-contained stainless steel powder is packed in the jacket of the barrel-shaped formula of above-mentioned low-carbon (LC) steel pricker and ram-jolt, sealing jacket, then that jacket is degassed in two steps: the first step, jacket is placed in to room temperature degassed, degassed to vacuum be 8Pa; Second step, by jacket be heated to 650 ℃ degassed, degassed to vacuum 10
-3pa;
4) high temperature insostatic pressing (HIP): enter in high temperature insostatic pressing (HIP) cylinder body through the jacket cold charge of degassed sealing, intensification is carried out densified, and pressure medium is argon gas, and technological parameter is: 1135 ℃ of sintering temperatures, sintering pressure 130MPa, temperature retention time 3h, then cooling with stove, after coming out of the stove, recording bottom surface internal diameter is 204mm, external diameter 395mm, end face internal diameter 76mm, external diameter 138mm, height 346mm.Remove jacket and carry out following process, nitrogen content is 0.76% after testing, and tensile strength is 980MPa, and yield strength is 675MPa, percentage elongation 28.5%, the contraction percentage of area 27.5%, normal temperature ballistic work 24J.
Embodiment 2
The particle mean size that the present embodiment is chosen is that the nitrogenous super austenitic powder of stainless steel of 200 μ m is raw material, and the composition of this powder according to mass percent is: 25.00%Cr, and 5.00%Mn, 2.10%Mo, 0.5%Si, 0.76%N, 10.00%Ni, all the other are Fe.
Adopt above-mentioned raw materials to prepare the part of solid-cone cartridge type, this part is of a size of: bottom surface diameter 500mm, end face diameter 300mm, height 1500mm.
Preparation method is as follows:
1) jacket design: according to the jacket of numerical model design revolving body form, powder yield function is following formula:
Wherein, σ
yfor single shaft yield stress, σ ' is deviatoric stress component tensor, and P is hydrostatic pressure, γ=ρ
a, β=(1-ρ)
b2, wherein ρ is relative density, and a is that 2.5, b is 0.5.
The yield function obtaining by above formula and the size of end article, according to the analog form design jacket of embodiment 1, jacket is specifically of a size of: bottom surface diameter 620mm, end face diameter 335mm, height 1720mm, jacket material is 304 stainless steels.
2) jacket preparation: adopt spinning process to prepare the stainless steel jacket of above-mentioned cone form, spinning process is divided into 10 passages to carry out, and each pass deformation is 8-12%, and between passage, annealing temperature is 1050 ℃, and temperature retention time is 0.5h.
3) dress powder and degassed same example 1;
4) heat and other static pressuring processes, parameter is: 1135 ℃ of temperature, pressure 190MPa, temperature retention time 3h, cooling with stove, after coming out of the stove, record bottom surface diameter 530mm, end face diameter 311mm, height 1520mm, removes jacket and carries out following process, nitrogen content is 0.76% after testing, tensile strength is 1040MPa, and yield strength is 670MPa, percentage elongation 47.5%, the contraction percentage of area 50.0%, normal temperature ballistic work 67J.
Embodiment 3
The particle mean size that the present embodiment is chosen is that the nitrogenous super austenitic powder of stainless steel of 150 μ m is raw material, and nitrogen-contained stainless steel powder composition according to mass percent is: 20.10%Cr, and 5.50%Mn, 1.80%Mo, 0.5%Si, 0.76%N, 9.00%Ni, all the other are Fe.
Adopt above-mentioned raw materials to prepare part as shown in Figure 1, this accessory size is: D1=300mm, D2=200mm, D3=700mm, H1=150mm, H2=1200mm.
Preparation method is as follows:
1) jacket design: according to the jacket of numerical model design revolving body form, powder yield function is following formula:
Wherein, σ
yfor single shaft yield stress, σ ' is deviatoric stress component tensor, and P is hydrostatic pressure, γ=ρ
a, β=(1-ρ)
b2, wherein ρ is relative density, and a is that 2.3, b is 0.5.
The yield function obtaining by above formula and the size of end article, according to the analog form design jacket of embodiment 1, jacket is specifically of a size of: D1=360mm, D2=225mm, D3=850mm, H1=180mm, H2=1460mm, jacket material is mild steel.
2) jacket preparation: adopt spinning process to prepare the stainless steel jacket of above-mentioned cone form, spinning process is divided into 8 passages to carry out, and each pass deformation is 10-15%, and between passage, annealing temperature is 650 ℃, and temperature retention time is 1h.
3) dress powder and degassed same example 1;
4) heat and other static pressuring processes, parameter is: 1160 ℃ of temperature, pressure 190MPa, temperature retention time 3h, cooling with stove, come out of the stove and record D1=306mm, D2=209mm, D3=730mm, H1=157mm, H2=1245mm, removes jacket and carries out following process, and nitrogen content is 0.76% after testing, tensile strength is 1030MPa, and yield strength is 660MPa, percentage elongation 49.0%, the contraction percentage of area 50.5%, normal temperature ballistic work 78J.
Claims (10)
1. a preparation method with the nitrogen-contained stainless steel goods of revolving body form, is characterized in that, comprises the following steps: the jacket of design revolving body form, the jacket of preparing revolving body form, dress powder, degassed and high temperature insostatic pressing (HIP) step, wherein:
In the described jacket step of preparing revolving body form, described jacket adopts spinning process preparation, and wherein, described spinning process is divided into 6-15 passage to carry out, and the deflection of each passage is 7-17%, and all jacket base is carried out to annealing in process between each passage.
2. preparation method according to claim 1, is characterized in that, in the described jacket step of preparing revolving body form, temperature when described annealing in process is 500 ℃-1200 ℃, and temperature retention time is 0.25-3 hour.
3. preparation method according to claim 2, is characterized in that, temperature when described annealing in process is 600 ℃-700 ℃, and temperature retention time is 1-2 hour.
4. preparation method according to claim 1, is characterized in that, in the jacket step of described design revolving body form, according to the jacket of numerical model design revolving body form, powder yield function is following formula:
Wherein, σ
yfor single shaft yield stress, σ ' is deviatoric stress component tensor, and P is hydrostatic pressure, γ=ρ
a, β=(1-ρ)
b2, wherein ρ is relative density, is 1-3.5 according to the different a spans of material composition, and b span is 0.2-1.
5. preparation method according to claim 4, is characterized in that, described jacket diameter range is 100mm～1500mm, and altitude range is 200mm～2000mm.
6. preparation method according to claim 1, is characterized in that, the material of described jacket is mild steel, stainless steel, nickel or molybdenum.
7. preparation method according to claim 1, it is characterized in that, described dress powder step refers to nitrogen-contained stainless steel powder packed in described jacket and sealing jacket, preferably, the particle of described nitrogen-contained stainless steel powder is less than or equal to 250 μ m, this nitrogen-contained stainless steel powder is made up of following chemical composition according to mass percent: Cr20.0～35%, Mn0.1～10%, Mo0.1～6%, Si0.1～1.0%, N0.4～1.5%, Ni5～25%, all the other are Fe and inevitable impurity.
8. preparation method according to claim 1, is characterized in that, described degassed step refers to degassed vacuum in jacket to≤10
-3pa; Described degassed step is preferably carried out in two steps: the first step, is placed in room temperature by jacket degassed to vacuum < 10Pa; Second step, it is degassed under the condition of 100～800 ℃ that jacket is placed in to temperature, finally makes vacuum≤10 in jacket
-3pa.
9. preparation method according to claim 1, it is characterized in that, in described high temperature insostatic pressing (HIP) step, jacket cold charge after degassed is entered in high temperature insostatic pressing (HIP) cylinder body, to carry out hip treatment, wherein: sintering temperature is 1135～1350 ℃, sintering pressure is 110～180MPa, and temperature retention time is 0.5～3h.Preferably, the pressure medium of described high temperature insostatic pressing (HIP) is helium or argon gas.
10. adopt the nitrogen-contained stainless steel goods with revolving body form that prepared by method described in claim 1-8, it is characterized in that, the product after high temperature insostatic pressing (HIP) possesses nearly end form; Preferably, the diameter range of described goods is 100mm～1500mm, and altitude range is 200mm～2000mm; More preferably, described nitrogen-contained stainless steel goods are cone cartridge type.
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| JP7242344B2 (en) | 2018-02-27 | 2023-03-20 | ロールス・ロイス・ピーエルシー | Method for producing austenitic iron alloy |
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