CN103706793A - Preparation method of low-nickel high-nitrogen austenitic stainless steel product - Google Patents
Preparation method of low-nickel high-nitrogen austenitic stainless steel product Download PDFInfo
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Abstract
The invention provides a preparation method of a low-nickel high-nitrogen austenitic stainless steel product. The method comprises the steps of mixing 200-mesh iron powder, chromium powder, manganese powder and manganese powder as raw materials, with the purity of not less than 99.0%, and 200-mesh graphite powder according to the mass ratio of (66-72): (16-18): (10-12): (2.0-3.5): (0.1-0.3), grinding the above powder in a nitrogen environment, mixing with an adhesive, and then performing mixing and injection molding, catalytic debinding, residual adhesive desorption, sintering densification and sintering densification to obtain the low-nickel high-nitrogen austenitic stainless steel product. The low-nickel high-nitrogen austenitic stainless steel product provided by the invention has the characteristics of higher sintered density, nitrogen content and dimensional precision, excellent mechanical property and decay resistance and the like, thereby being suitable for large-scale industrial manufacturing.
Description
Technical field
The invention belongs to stainless steel manufacturing technology field, relate in particular to a kind of preparation method who saves nickel high-nitrogen austenitic stainless steel goods.
Background technology
The preparation method of nickel-saving type high nitrogen stainless steel mainly contains high pressure smelting process and powder metallurgic method at present.High pressure melting comprises the techniques such as high temperature insostatic pressing (HIP) melting, pressurized Induction Melting, pressurization plasma melting, pressurization electroslag remelting, though can obtain high nitrogen content and obdurability, but equipment needed thereby is complicated, it is huge to invest, and technology controlling and process is more difficult, has hindered their industrialization development and application.Compare with high pressure melting, powder metallurgy is produced high nitrogen steel and is had a lot of advantages, as simple in equipment, cost is low, material property has been strengthened in refined crystalline strengthening, dispersion strengthening etc., the solid solubility of nitrogen in solid-state austenitic stainless steel be much larger than the solubility in liquid state in addition, thereby powder metallurgy solid State Nitriding technique has become one of focus of current high nitrogen steel preparation field.But traditional powder metallurgy mold pressing-sintering process can only be suppressed the simple stainless steel parts of shape matching, and its density, mechanics and corrosion resisting property are not high, thereby and are not suitable for the preparation of complex-shaped high performance nickel saving high nitrogen stainless steel goods.
Metal injection moulding is as current state-of-the-art powder metallurgy Near net Shaping Technology, there is unique advantage producing low-costly and in high volume to have aspect 3 D complex geometry, high-performance, high-precision product, can also realize automation completely and work continuously, be considered to one of the most potential high nitrogen steel preparation of industrialization technology in future.The general technology route that metal current injection moulding is prepared high indole nickel and stainless steel is: first by inert gas atomizer technology, obtain spherical stainless steel material powder, then powder of stainless steel and binding agent are mixed and made into feeding and carry out injection moulding and obtain preform, after degreasing, in blanket of nitrogen, carry out sintering and nitrogenize obtains high nitrogen stainless steel goods.Yet the shortcoming of above-mentioned technique is that the cost of gas-atomized powder is higher, fine powder output capacity is low, the granularity of powder is difficult to accurate control, in this externally sintered nitridation process owing to being subject to the impact of nitrogen-atoms kinetics of diffusion, the distribution of nitrogen is often even not, and be difficult to obtain very high sintered density, thereby affect stainless tissue and performance.
Ball grinding technique is an effective way of the high indole nickel and stainless steel powder of preparation, by starting powder with containing nitrogen medium (as nitrogen, ammoniacal liquor, nitride etc.) between there is solid-gas, solid-liquid or solid-solid reaction, the high nitrogen supersaturated solid solution superfines of formation nonequilibrium state is manocrystalline powders even, because powder inside exists a large amount of distortions of lattice and crystal defect, sintering activity is higher, easily obtains high sintered density and performance.In recent years, utilize ball grinding technique to prepare the high nitrogen powdered steel of multiple ultra-fine, over-saturation nitrogen, yet its grain shape mostly is irregular sheet or polygonal, top layer oxygen content and hardness are high, powder flowbility and tap density are very low, and formability is poor, can not meet the technique needs of follow-up metal injection moulding, can only adopt the technique of the complex and expensive such as high temperature insostatic pressing (HIP), hot extrusion, powder forging rolling to form, be difficult to realize large-scale industrialization and produce.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who saves nickel high-nitrogen austenitic stainless steel goods, the preparation method who is intended to solve existing nickel-saving type high nitrogen stainless steel exists that equipment requirement is high, nitrogen skewness, the problem such as poor is shaped.
The present invention is achieved in that a kind of preparation method who saves nickel high-nitrogen austenitic stainless steel goods, comprises the following steps:
(1) raw material are used under nitrogen environment the steel ball of Φ 7～Φ 9mm with 400～500r/min rotating speed ball milling, 12～72h, obtained spherical powder, wherein, the ratio of grinding media to material of described raw material and steel ball is (10: 1)～(14: 1);
(2) high indole nickel and stainless steel spherical powder step (1) being obtained and adhesive be (54～60) by volume: (40～46) are mixing in mixing roll after mixing obtains injecting feeding, wherein, melting temperature is 175～185 ℃, and mixing time is 60～90min; Described injection feeding is carried out to injection moulding in injection machine, obtain the flawless shaping base of shape, wherein, injection temperature is 180～190 ℃, and injection pressure is 80～120MPa;
(3) shaping base step (2) being obtained is in catalysis degreasing stove and at nitrogen and HNO
3under gaseous environment, carry out degreasing, obtain degreasing blank, wherein, skimming temp is 120 ℃～130 ℃, and degreasing time is 4～6h;
(4) degreasing blank step (3) being obtained is placed in vacuum tube furnace order and carries out the processing that removes of remaining adhesive, and sintering densification is processed, and solution heat treatment, obtains saving nickel high-nitrogen austenitic stainless steel goods.
Preferably, in step (1), described raw material are iron powder, chromium powder, manganese powder, molybdenum powder and graphite powder (66～72) (16～18) in mass ratio: (10～12): (2.0～3.5): (0.1～0.3) obtains after mixing.
Preferably, the granularity of described iron powder, chromium powder, manganese powder, molybdenum powder and graphite powder is 200 orders.
Preferably, in step (1), described ratio of grinding media to material is 10: 1; In step (1), the purity of described iron powder, chromium powder, manganese powder and molybdenum powder is all not less than 99.0%; In step (1), described nitrogen flow is 1.0～1.5L/min.
Preferably, in step (2), described adhesive comprises following by each component of mass parts:
Preferably, in step (3), the speed that passes into of described nitrogen is 400～500mL/min, described HNO
3it is 0.05～0.10mL/min that gas passes into speed.
Preferably, the processing that removes of described remaining adhesive comprises the following steps:
Under vacuum >=10Pa, when starting to be warmed up to 350 ℃ with 5 ℃/min speed, room temperature is incubated 30min, continuation is warming up to after 420 ℃ of when insulation 40min with 2 ℃/min speed, continuation is incubated after 40min while being heated to 500 ℃ with 2 ℃/min heating rate, continues to be warmed up to 550 ℃ of insulation 60min with 2 ℃/min speed.
Preferably, described sintering densification is processed and is comprised the following steps:
Described remaining adhesive remove step after, adjust vacuum>=1.0 * 10
-2pa, continues to be warmed up to after 1150 ℃ of insulation 30min with 8 ℃/min speed, when the speed that continues to take 5 ℃/min is warmed up to 1270 ℃, close vacuum and nitrogen flow under 1.0～1.2L/min environment after sintering 90min with the cooling sintered article that obtains of stove.
Preferably, described solution heat treatment comprises the following steps: described sintered article is reheated to 1100 ℃ of insulation 60min, and then shrend is cooling.
The present invention overcomes the deficiencies in the prior art, a kind of preparation method who saves nickel high-nitrogen austenitic stainless steel goods is provided, for the high indole nickel and stainless steel powder that in the past prepared by ball grinding technique, be generally irregular sheet, mobility and tap density are low, cannot meet follow-up this shortcoming of metal injection moulding technological requirement, the present invention be take pure element powder as primary raw material, explore best stirring ball-milling process route and prepared good sphericity, nitrogen content is high, particle is tiny, can better meet the high nitrogen stainless steel powder of follow-up injection moulding requirement, utilize subsequently metal injection moulding to obtain and there is higher sintered density and nitrogen content, good mechanical property, the high indole austenitic stainless steel goods that decay resistance and dimensional accuracy are high, thereby realized the combination of ball milling and two kinds of technologies of preparing of powder injection forming.
In addition, for injection moulding high nitrogen stainless steel in the past, mainly adopt solvent degreasing+hot degreasing two step degreasing process, there is complex procedures, degreasing speed is slow, generation defect is many, consume energy high, the shortcomings such as contaminated environment, the present invention also provides a kind of adhesive of catalysis degreasing type, implement advanced catalysis degreasing technique, greatly shorten degreasing time, improved production efficiency, reduced the production cost of injection forming product, and the skimming temp using is low, during degreasing, there is not liquid phase, avoided product to deform and the weakness such as dimension control difficulty, degreasing base quality is good, there is no open defect.
Finally, oxygen content for ball milling high nitrogen stainless steel powder is in the past high, cause in its injection sintered article oxide many and be difficult to reduction, thereby affect the problem of sintering character, the present invention adopts and in ball milling material powder, adds appropriate graphitic carbon as interior reducing agent, under high vacuum condition, injection moulding degreasing base is carried out to presintering, utilizes the carbothermic reduction reaction of vacuum-sintering to carry out deoxidation, effectively reduce the oxide in sintered body, improved every serviceability of sintered article comprehensively.
Accompanying drawing explanation
Fig. 1 is the spherical powder SEM shape appearance figure that in the embodiment of the present invention prepared by stirring ball-milling;
Fig. 2 is the SEM shape appearance figure of injecting green compact photo in kind and inner fracture in the embodiment of the present invention;
Fig. 3 is that in the embodiment of the present invention, removing of remaining adhesive processed and densification process curve figure;
Fig. 4 is the photo in kind that saves nickel high-nitrogen austenitic stainless steel sintered article in the embodiment of the present invention;
Fig. 5 is the SEM photo saving in the embodiment of the present invention after the solution treatment of nickel high-nitrogen austenitic stainless steel.
The specific embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment
A preparation method who saves nickel high-nitrogen austenitic stainless steel goods, comprises the following steps:
(1) stirring ball-milling is prepared high indole nickel and stainless steel spherical powder
Selecting granularity is 200 orders, (66～72) mass parts iron powder of purity >=99.0%, (16～18) mass parts chromium powder, (10～12) mass parts manganese powder, (2.0～3.5) mass parts molybdenum powder is as raw material, and add the 200 order graphite powders of (0.1～0.3) mass parts as lubricant and deoxidization reducer, after being mixed, all powder is placed in together with abrading-ball in the ball grinding cylinder of high-energy stirring formula ball mill, ball milling 12～72h under the High Purity Nitrogen atmosphere of circulation, ball cylinder volume is 10L, abrading-ball is selected the bearing steel ball of Φ 7～Φ 9mm, rotating speed is 400～500r/min, ratio of grinding media to material is 10: 1～14: 1, nitrogen flow is 1.0～1.5L/min.In order to reduce the adverse effect of other impurity, not use procedure controlling agent in mechanical milling process.
At rotating speed, be 400r/min, ratio of grinding media to material 10: 1, under ball radius Φ 7mm condition, the key property of ball milling different time powder is as shown in table 1:
The characteristic of table 1 ball milling different time powder
As can be seen from Table 1, along with the prolongation of Ball-milling Time, the nitrogen content sustainable growth of body of powder, particle mean size constantly reduces, it is large that specific area becomes, apparent density and the tap density of powder improve gradually, and when ball milling reaches 60h, the fragmentation of powder and cold welding have reached the dynamic equilibrium stage, particle size becomes the most tiny (5～20 μ m), specific area is maximum, nitrogen content very high (1.32%), tap density higher (be about solid density 59.1%); The powder of ball milling 72h is compared with the powder of ball milling 60h, powder size is alligatoring to some extent, tap density changes little, the now cold welding effect that the illustrates powder of preponderating has been difficult to by refinement, continue ball milling and only can bring the undue reunion of body of powder and the rising of impurity content, the final performance of alloy causes harmful effect.
As shown in Figure 1, wherein, Fig. 1 is spherical powder SEM shape appearance figure prepared by stirring ball-milling to the ESEM pattern of ball milling 60h powder particle, and a figure is the powder particle under low power, and b figure is the powder particle under high power.From Fig. 1, can find that powder particle is very tiny evenly, shape very convergence is spherical, high tap density contributes to improve the useful load of injection feeding, bigger serface can improve the sintering activity of powder, good sphericity is conducive to improve the mobility of powder, this shows that ball milling has significantly improved shape and the granularity of powder, improved the operational characteristic of powder, it is high that stirring ball-milling 60h has prepared nitrogen content, particle is tiny, the compound powder of high-nitrogen nickel-free stainless steel of good sphericity, there is good mobility, high useful load and sintering activity, the very injection of suitable metal powder injection forming and the needs of sintering process.
(2) preparation and the injection molding process of injection feeding
In embodiments of the present invention, the adhesive adopting is mainly comprised of polyformaldehyde (POM), high density polyethylene (HDPE) (HDPE), vinyl-vinyl acetate copolymer (EVA) and stearic acid (SA), its mass parts meter respectively consists of: 85～90 parts of POM, 5～8 parts of HDPE, 2～5 parts of EVA, 1～3 part of SA.Than common binding agent, adhesive of the present invention has that the speed of removing is fast, good fluidity, conformality feature high, with low cost, be well suited for, for making the feeding of METAL INJECTION MOLDING OF STAINLESS STEELS goods, realizing the quick zero defect degreasing of product, and guaranteeing the dimensional accuracy that it is high.
By the high nitrogen spherical powder of adhesive and ball milling 60h according to volume ratio (40～46): (54～60) after mixing, on banbury, carry out mixing make be evenly distributed, granular injection feeding that rheological property is good, melting temperature is 175～185 ℃, and the time is 60～90min.Feeding is carried out on injection machine to injection moulding, 180～190 ℃ of injection temperatures, injection pressure is 80～120MPa, obtains the zero defect shaping base of required form.
Fig. 2 be the feeding of powder volume mark while being 58% at 185 ℃, the injection green compact photo in kind obtaining under the injection parameters of 110MPa and the SEM shape appearance figure of inner fracture, wherein, a figure is pictorial diagram, b figure is that a schemes fracture SEM shape appearance figure in kind.Injection base substrate mainly comprises following three kinds: a kind of for injection moulding MPIF35 standard tensile sample, for the tensile mechanical properties of test material; Another kind is the disk of Φ 20mm * 5mm, for the decay resistance of test material; The third is a kind of ball-screw reverser part base substrate of complicated shape, for testing the dimensional accuracy of sintered article.As can be seen from Figure 2, injection base any surface finish is smooth, does not occur filling the defects such as type deficiency, face crack, distortion, hole, can see that the inner adhesive of base substrate mixes with powder, and do not produce the segregation phenomenon of powder from fracture photo.
(3) catalysis degreasing technique
Injection moulding green compact are positioned in catalysis degreasing stove and carry out degreasing, and degreasing process is as follows: 120 ℃～130 ℃ of skimming temps, and degreasing time 4～6h, it is 400～500mL/min that protective gas N2 passes into speed, catalytic gas HNO
3the speed of passing into is 0.05～0.10mL/min.Because the main constituent element polyformaldehyde in adhesive is very sensitive to acid atmosphere, under the catalytic action of nitric acid vapor, be cracked into formaldehyde gas rapidly and remove, shaping base is after 4～6h catalysis degreasing, the always amount of removing of adhesive has reached more than 85%, wherein main adhesive polyformaldehyde substantially decomposes and removes completely, and catalysis degreasing process completes.The degreasing effect of catalysis degreasing is better, not only degreasing time is far shorter than hot degreasing time, and catalytic reaction temperature is lower than the fusing point of acetal resin, in whole skimming processes, do not produce liquid phase, therefore degreasing base quality is good, the degreasing defect such as do not occur any crackle, pore, be out of shape, cave in, has innerly also formed a large amount of connected pore channels.After catalysis degreasing completes, in base substrate, also remain on a small quantity to the insensitive HDPE of catalysis atmosphere and EVA polymer adhesive, these binding agents can not decompose by catalyzed gas, in the later stage, as skeleton, will play conformal effect, and these remaining adhesives can remove in the rapid pyrolysis of presintering stage.
(4) sintering process
Degreasing blank after catalysis degreasing is placed in to vacuum tube furnace order and carries out the processing that removes of remaining adhesive, sintering densification is processed, and solution heat treatment, obtains saving nickel high-nitrogen austenitic stainless steel goods.Fig. 3 is that removing of remaining adhesive processed and densification process curve figure, and concrete steps are as follows:
Removing of A, remaining adhesive
As shown in Figure 3, under low vacuum condition (vacuum >=10Pa), from room temperature, start to be warmed up to 350 ℃ of insulation 30min with 5 ℃/min speed, thoroughly to remove minute quantity polyformaldehyde residual in base substrate and other impurity, and starting to remove and prepare for the high binding agent constituent element of delayed heat decomposition temperature; With 2 ℃/min speed, being warming up to 420 ℃ of insulation 40min, is mainly in order to remove the EVA polymer in adhesive; With 2 ℃/min heating rate, be heated to 500 ℃ of insulation 40min, high density polyethylene (HDPE) is substantially all removed; With 2 ℃/min speed, be warmed up to 550 ℃ of insulation 60min, whole binding agents of guaranteeing to inject in base remove totally, and so far degreasing process all completes.
B, sintering densification are processed
Because the oxygen content of ball milling 60h powder is higher, be 1.16% after testing, adopt normal sintering technique oxide inclusions effectively cannot be reduced, will have influence on final sintering serviceability, so degreasing transfers high vacuum condition (vacuum>=1.0 * 10 to by low vacuum after finishing immediately
-2pa), as shown in Figure 3, with 8 ℃/min speed, be warmed up to 1150 ℃ of insulation 30min, object is to using the graphitic carbon that adds in ball milling material powder as interior reducing agent, make in a vacuum the metal oxide (as iron oxide, chromium oxide, manganese oxide etc.) in degreasing base, with carbon, reduction reaction occur as far as possible, oxygen atom is discharged with the form of carbon monoxide or carbon dioxide product, and the active metal atomic energy activated sintering discharging further improve stainless sintered density and ductility; Then the speed with 5 ℃/min is warmed up to 1270 ℃, in this process, deoxygenation is proceeded, and after arriving sintering temperature, closes vacuum, and the high pure nitrogen that is filled with circulation carries out sintering 90min, nitrogen flow is 1.0～1.2L/min, cooling with stove after sintering completes.
C, solution heat treatment
In order to eliminate the fragility Nitride Phase of separating out slowly due to cooling rate in sintered body, need carry out follow-up solution heat treatment, sintered article is reheated to 1100 ℃ of insulation 60min, then shrend is cooling, obtains saving nickel high-nitrogen austenitic stainless steel goods.
Effect embodiment
The joint nickel high-nitrogen austenitic stainless steel goods that obtain in embodiment are observed, and observed result as shown in Figures 4 and 5.
Fig. 4 is the photo in kind of joint nickel high-nitrogen austenitic stainless steel sintered article, and visible shape of product is intact, distortion, defects i.e.cracks evenly, do not appear in contraction.
Fig. 5 is for saving the SEM photo after the solution treatment of nickel high-nitrogen austenitic stainless steel, it under room temperature state, is single austenite crystal tissue, there is not ferrite, do not have fragility nitride to separate out yet, illustrate that intensified element nitrogen is that form with solid solution is present in austenite completely, provides assurance for stainless steel has good combination property.Because making the particle of powder and crystal grain, high-energy ball milling obtained remarkable refinement, atom diffusion when a large amount of crystal defects that ball milling produces have simultaneously promoted sintering, the sintering activating energy and the sintering that have further reduced body of powder are temperature required, the densification temperature of ball milling 48h powder has approximately reduced by 30～40 ℃ than the densification temperature of the atomized alloy powder of similar component in the present invention, cause the austenite crystal in final sintered stainless steel goods very tiny, approximately only have 10～15 μ m, this superfine institutional framework obviously contributes to improve stainless serviceability.
The joint nickel high-nitrogen austenitic stainless steel goods that obtain in embodiment are carried out to service check, result is as follows: after solution treatment, stainless steel products has obtained the excellent combination of sintered density, nitrogen content and performance, sintering relative density reaches 98.4%, nitrogen content is up to 0.88%, oxygen content 0.21%, carbon content 0.026%, yield strength σ
0.2=638MPa, tensile strength sigma
b=994MPa, percentage elongation δ
5=32.6%, contraction percentage of area ψ=50.3%, impact flexibility α kv=112J/cm
2, hardness HV10=308,60 ℃ of air blowing pitting potential Ep>=700mV in 22%NaCl solution, pitting potential Ep>=1200mV in the physiological saline of 37 ℃, simulating blood plasma and Hank ' s solution.
Joint nickel high-nitrogen austenitic stainless steel prepared by the present invention is not in the situation that losing plasticity and toughness, its intensity, hardness, decay resistance, especially the index such as pitting resistance is considerably beyond traditional 304,316L, 317L chromium-nickel austenitic stainless steel, meet or exceed the advanced level of the similar high indole austenitic stainless steel material of report in the world, aspect the high strength anti-corrosion for industrial circle saves low nickel high-quality, safe and reliable in nickel and stainless steel structural material and medical and health industry or nickelles stainless steel embedded material, had great development potentiality and prospect.With statistical method, the shape and size precision of the complicated shape ball-screw reverser part of preparation is tested, its dimensional accuracy is about ± and 0.15%～± 0.2%, higher than the industrial required precision to metal powder injection molded goods ± 0.3%, therefore can realize large-scale industrialization and produce.
Compare the shortcoming and defect with prior art, the present invention has following beneficial effect: the present invention organically combines high-energy stirring ball mill and metal powder injection molded two kinds of techniques and prepares that crystal grain is tiny, density and nitrogen content is high, excellent performance, dimensional accuracy are high, the joint nickel high-nitrogen austenitic stainless steel goods that can meet industrialization batch production requirements, meets resources conservation that new material exploitation proposes, healthy friendly, cost is lower, performance is better aim and requirement completely.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. save a preparation method for nickel high-nitrogen austenitic stainless steel goods, it is characterized in that comprising the following steps:
(1) raw material are used under nitrogen environment the steel ball of Φ 7～Φ 9mm with 400～500r/min rotating speed ball milling, 12～72h, obtained spherical powder, wherein, the ratio of grinding media to material of described raw material and steel ball is (10: 1)～(14: 1);
(2) high indole nickel and stainless steel spherical powder step (1) being obtained and adhesive be (54～60) by volume: (40～46) are mixing in mixing roll after mixing obtains injecting feeding, wherein, melting temperature is 175～185 ℃, and mixing time is 60～90min; Described injection feeding is carried out to injection moulding in injection machine, obtain the flawless shaping base of shape, wherein, injection temperature is 180～190 ℃, and injection pressure is 80～120MPa;
(3) shaping base step (2) being obtained is in catalysis degreasing stove and at nitrogen and HNO
3under gaseous environment, carry out degreasing, obtain degreasing blank, wherein, skimming temp is 120 ℃～130 ℃, and degreasing time is 4～6h;
(4) degreasing blank step (3) being obtained is placed in vacuum tube furnace order and carries out the processing that removes of remaining adhesive, and sintering densification is processed, and solution heat treatment, obtains saving nickel high-nitrogen austenitic stainless steel goods.
2. the preparation method of joint nickel high-nitrogen austenitic stainless steel goods as claimed in claim 1, it is characterized in that, in step (1), described raw material are iron powder, chromium powder, manganese powder, molybdenum powder and graphite powder (66～72) in mass ratio: (16～18): (10～12): (2.0～3.5): (0.1～0.3) obtains after mixing.
3. the preparation method of joint nickel high-nitrogen austenitic stainless steel goods as claimed in claim 2, is characterized in that, the granularity of described iron powder, chromium powder, manganese powder, molybdenum powder and graphite powder is 200 orders.
4. the preparation method of joint nickel high-nitrogen austenitic stainless steel goods as claimed in claim 3, is characterized in that, in step (1), described ratio of grinding media to material is 10: 1;
In step (1), the purity of described iron powder, chromium powder, manganese powder and molybdenum powder is all not less than 99.0%;
In step (1), described nitrogen flow is 1.0～1.5L/min.
5. the preparation method of joint nickel high-nitrogen austenitic stainless steel goods as claimed in claim 4, is characterized in that, in step (2), described adhesive comprises following by each component of mass parts:
6. the preparation method of joint nickel high-nitrogen austenitic stainless steel goods as claimed in claim 5, is characterized in that, in step (3), the speed that passes into of described nitrogen is 400～500mL/min, described HNO
3it is 0.05～0.10mL/min that gas passes into speed.
7. the preparation method of joint nickel high-nitrogen austenitic stainless steel goods as claimed in claim 6, is characterized in that, the processing that removes of described remaining adhesive comprises the following steps:
Under vacuum >=10Pa, when starting to be warmed up to 350 ℃ with 5 ℃/min speed, room temperature is incubated 30min, continuation is warming up to after 420 ℃ of when insulation 40min with 2 ℃/min speed, continuation is incubated after 40min while being heated to 500 ℃ with 2 ℃/min heating rate, continues to be warmed up to 550 ℃ of insulation 60min with 2 ℃/min speed.
8. the preparation method of joint nickel high-nitrogen austenitic stainless steel goods as claimed in claim 7, is characterized in that, described sintering densification is processed and comprised the following steps:
Described remaining adhesive remove step after, adjust vacuum>=1.0 * 10
-2pa, continues to be warmed up to after 1150 ℃ of insulation 30min with 8 ℃/min speed, when the speed that continues to take 5 ℃/min is warmed up to 1270 ℃, close vacuum and nitrogen flow under 1.0～1.2L/min environment after sintering 90min with the cooling sintered article that obtains of stove.
9. the preparation method of joint nickel high-nitrogen austenitic stainless steel goods as claimed in claim 8, is characterized in that, described solution heat treatment comprises the following steps: described sintered article is reheated to 1100 ℃ of insulation 60min, and then shrend is cooling.
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