CN103706793B - A kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods - Google Patents
A kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods Download PDFInfo
- Publication number
- CN103706793B CN103706793B CN201310692084.5A CN201310692084A CN103706793B CN 103706793 B CN103706793 B CN 103706793B CN 201310692084 A CN201310692084 A CN 201310692084A CN 103706793 B CN103706793 B CN 103706793B
- Authority
- CN
- China
- Prior art keywords
- powder
- nitrogen
- stainless steel
- austenitic stainless
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention provides a kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods, by by 200 mesh, the ferrum powder of purity >=99.0%, chromium powder, manganese powder, molybdenum powder as raw material and 200 mesh graphite powders according to mass parts ratio (66~72): (16~18): (10~12): (2.0~3.5): after (0.1~0.3) mixing, grind in a nitrogen environment, the most again by carrying out mixing injection moulding with adhesive after mixing, catalysis degreasing, remaining adhesive removing, obtain after sintering densification and solution heat treatment saving nickel high-nitrogen austenitic stainless steel goods.The joint nickel high-nitrogen austenitic stainless steel goods of the present invention have higher sintered density, nitrogen content and a dimensional accuracy, the feature such as excellent mechanical property, decay resistance, are suitable to extensive industrialized manufacture.
Description
Technical field
The invention belongs to rustless steel manufacturing technology field, particularly relate to a kind of system saving nickel high-nitrogen austenitic stainless steel goods
Preparation Method.
Background technology
The preparation method of nickel-saving type high nitrogen stainless steel mainly has high pressure smelting process and powder metallurgic method at present.High pressure melting bag
Include the techniques such as high temperature insostatic pressing (HIP) melting, pressurized Induction Melting, pressurization plasma melting, pressurization electroslag remelting, though high nitrogen can be obtained
Content and obdurability, but equipment needed thereby is complicated, it is huge to invest, technology controlling and process is more difficult, hinder they industrialization development and
Application.Compared with high pressure melting, powder metallurgy produces high nitrogen steel and has a lot of advantage, as equipment is simple, low cost is thin brilliant strong
Change, diffusate strengthening etc. enhance material property, and additionally nitrogen solid solubility in solid-state austenitic stainless steel is much larger than in liquid
In dissolubility, thus powder metallurgy solid State Nitriding technique has become one of focus of current high nitrogen steel preparation field.But it is traditional
Powder metallurgy mold pressing-sintering process can only suppress shape matching simple rustless steel parts, and its density, mechanics and anti-corrosion
Performance is the highest, thus is not appropriate for the preparation of complex-shaped high performance nickel saving high nitrogen stainless steel goods.
Metal injection moulding, as current state-of-the-art powder metallurgy Near net Shaping Technology, produces low-costly and in high volume
Have 3 D complex geometry, high-performance, high-precision product aspect have the advantage of uniqueness, it is also possible to be fully achieved automatically
Change and work continuously it is considered to be one of the most potential high nitrogen steel preparation of industrialization technology in future.Metal current is injected into
The general technology route of shape preparation joint nickel high nitrogen stainless steel is: first passes through inert gas atomizer technology and obtains spherical rustless steel
Material powder, is then mixed and made into powder of stainless steel and binding agent feeding and carries out injection moulding and obtain preform, through de-
It is sintered in blanket of nitrogen after fat and nitridation obtains high nitrogen stainless steel goods.But the shortcoming of above-mentioned technique is aerosolization system
Powder relatively costly, fine powder output capacity is low, and the granularity of powder is difficult to accurately control, due to by nitrogen in this externally sintered nitridation process
The dynamic (dynamical) impact of atoms permeating, the distribution of nitrogen is the most uniform, and is difficult to obtain the highest sintered density, thus impact is not
The tissue of rust steel and performance.
Ball grinding technique is the effective way preparing joint nickel high nitrogen stainless steel powder, by starting powder and containing nitrogen medium
There is solid-gas, solid-liquid or solid-solid reaction between (such as nitrogen, ammonia, nitride etc.), form the high nitrogen supersaturation of nonequilibrium state
Solid solution superfines even manocrystalline powders, owing to there is substantial amounts of distortion of lattice and crystal defect inside powder, sintering is lived
Property is higher, is readily available high sintered density and performance.In recent years, ball grinding technique is utilized to prepare multiple ultra-fine, super full
With the high nitrogen steel powder of nitrogen, but its grain shape mostly is irregular lamellar or polygon, and top layer oxygen content and hardness are high, powder
Mobility and tap density are the lowest, and formability is poor, it is impossible to meet the technique needs of subsequent metal injection moulding, can only use heat
The technique of the complex and expensive such as isostatic pressed, hot extrusion, powder forging rolling forms, it is difficult to realize industrialization large-scale production.
Summary of the invention
It is an object of the invention to provide a kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods, it is intended to solve existing
With the presence of nickel-saving type high nitrogen stainless steel preparation method equipment requirements height, nitrogen skewness, shape the problems such as poor.
The present invention is achieved in that a kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods, including following step
Rapid:
(1) by raw material in a nitrogen environment with the steel ball of Ф 7~Ф 9mm with 400~500r/min rotating speed ball millings 12~
72h, obtains spherical powder, and wherein, described raw material is (10: 1)~(14: 1) with the ratio of grinding media to material of steel ball;
(2) the joint nickel high nitrogen stainless steel spherical powder that step (1) is obtained and adhesive (54~60) by volume: (40
~46) mixing after in mixing roll mixing obtain inject feeding, wherein, melting temperature is 175~185 DEG C, and mixing time is 60
~90min;Described injection feeding is carried out injection moulding in injection machine, obtains shape flawless shaping base, wherein, injection
Temperature is 180~190 DEG C, and injection pressure is 80~120MPa;
(3) shaping base step (2) obtained is in catalysis degreasing stove and at nitrogen and HNO3Take off under gaseous environment
Fat, obtains degreasing blank, and wherein, skimming temp is 120 DEG C~130 DEG C, and degreasing time is 4~6h;
(4) degreasing blank that step (3) obtains is placed in vacuum tube furnace order carry out at the removing of remaining adhesive
Reason, sintering densification processes, and solution heat treatment, obtains saving nickel high-nitrogen austenitic stainless steel goods.
Preferably, in step (1), described raw material is iron powder, chromium powder, manganese powder, molybdenum powder and graphite powder in mass ratio (66
~72) (16~18): (10~12): (2.0~3.5): obtain after (0.1~0.3) mix homogeneously.
Preferably, the granularity of described iron powder, chromium powder, manganese powder, molybdenum powder and graphite powder is 200 mesh.
Preferably, in step (1), described ratio of grinding media to material is 10: 1;In step (1), described iron powder, chromium powder, manganese powder with
And the purity of 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 includes the most each component:
Preferably, in step (3), the speed that is passed through of described nitrogen is 400~500mL/min, described HNO3Gas leads to
Entering speed is 0.05~0.10mL/min.
Preferably, the removing of described remaining adhesive processes and comprises the following steps:
Under vacuum >=10Pa, after room temperature starts with 5 DEG C/min ramp to insulation 30min when 350 DEG C, continue
After 2 DEG C/min ramp to insulation 40min when 420 DEG C, continue to be incubated when being heated to 500 DEG C with 2 DEG C/min heating rate
After 40min, continue to be incubated 60min with 2 DEG C/min ramp to 550 DEG C.
Preferably, described sintering densification processes and comprises the following steps:
After the removing step of described remaining adhesive, adjust vacuum >=1.0 × 10-2Pa, continues with 8 DEG C/min speed
After rate is warmed up to 1150 DEG C of insulation 30min, continue to close vacuum when being warmed up to 1270 DEG C with the speed of 5 DEG C/min and at nitrogen stream
Amount is that after sintering 90min under 1.0~1.2L/min environment, furnace cooling obtains sintered article.
Preferably, described solution heat treatment comprises the following steps: described sintered article is reheated to 1100 DEG C of insulations
60min, then water quenching cooling.
The present invention overcomes the deficiencies in the prior art, it is provided that a kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods,
It is low that the joint nickel high nitrogen stainless steel powder prepared for conventional ball grinding technique is usually irregular lamellar, mobility and tap density,
Cannot meet subsequent metal this shortcoming of injection molding process requirement, the present invention, with pure element powder as primary raw material, explores
Optimal stirring ball-milling process route prepares good sphericity, nitrogen content is high, granule is tiny, can preferably meet subsequent injections
The high nitrogen stainless steel powder that shape requires, obtains followed by metal injection moulding and has higher sintered density and nitrogen content,
The joint nickel high-nitrogen austenitic stainless steel goods that excellent mechanical property, decay resistance and dimensional accuracy is high, it is achieved thereby that ball
Mill and the combination of two kinds of technologies of preparing of powder injection forming.
Additionally, mainly use solvent degreasing+thermal debinding two step degreasing process for conventional injection moulding high nitrogen stainless steel, deposit
In complex procedures, defat speed is slow, it is many to produce defect, power consumption is high, pollute the shortcomings such as environment, present invention also offers a kind of catalysis
The adhesive of degreasing type, implements advanced catalysis degreasing technique, is greatly shortened degreasing time, improves production efficiency, reduce
The production cost of injection forming product, and the skimming temp used is low, occurs without liquid phase during defat, it is to avoid product becomes
The weakness such as shape and dimension control difficulty, defat base quality is good, does not has open defect.
Finally, the oxygen content for conventional ball milling high nitrogen stainless steel powder is high, causes oxide in its injection sintered article
Many and be difficult to reduce, thus affect the problem of sintering character, the present invention uses and adds appropriate graphite in ball milling material powder
Carbon, as interior reducing agent, carries out presintering to injection moulding defat base in high vacuum conditions, utilizes the carbon heat of vacuum-sintering also
Former reaction carrys out deoxidation, efficiently reduces the oxide in sintered body, improves 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 to inject green compact material object photo and the SEM shape appearance figure of internal fracture in the embodiment of the present invention;
Fig. 3 is removing process and the densification process curve figure of remaining adhesive in the embodiment of the present invention;
Fig. 4 is the photo in kind saving nickel high-nitrogen austenitic stainless steel sintered article in the embodiment of the present invention;
Fig. 5 is the SEM photograph after saving nickel high-nitrogen austenitic stainless steel solution treatment in the embodiment of the present invention.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and
It is not used in the restriction present invention.
Embodiment
A kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods, comprises the following steps:
(1) stirring ball-milling preparation joint nickel high nitrogen stainless steel spherical powder
Select granularity be 200 mesh, (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 adds 200 mesh of (0.1~0.3) mass parts
Graphite powder, as lubricant and deoxidization reducer, will be placed in high-energy stirring formula ball milling together with abrading-ball after all powder mix homogeneously
In the ball grinding cylinder of machine, ball milling 12~72h under the High Purity Nitrogen atmosphere of circulation, ball cylinder volume is 10L, and abrading-ball selects Ф 7~Ф 9mm
Bearing steel ball, rotating speed is 400~500r/min, and ratio of grinding media to material is 10: 1~14: 1, and nitrogen flow is 1.0~1.5L/min.For
Reduce the adverse effect of other impurity, mechanical milling process do not uses process control agent.
It is 400r/min at rotating speed, ratio of grinding media to material 10: 1, under the conditions of ball radius Ф 7mm, the master of ball milling different time powder
Want characteristic as shown in table 1:
The characteristic of table 1 ball milling different time powder
From table 1 it follows that along with the prolongation of Ball-milling Time, the nitrogen content sustainable growth of body of powder, particle mean size is not
Disconnected reduction, specific surface area becomes big, and apparent density and the tap density of powder gradually step up, when ball milling reaches 60h, breaking of powder
Broken and cold welding has reached the dynamic equilibrium stage, and particle size becomes the most tiny (5~20 μm), and specific surface area is maximum, and nitrogen contains
Measure the highest (1.32%), tap density higher (about the 59.1% of solid density);The powder of ball milling 72h and the powder of ball milling 60h
End is compared, and powder size has been roughened, and tap density change is little, illustrates that now cold welding effect dominant powder is difficult to by carefully
Change, continue ball milling and the undue of body of powder only can be brought to reunite and the rising of impurity content, the final performance of alloy is caused bad
Impact.
As it is shown in figure 1, wherein, Fig. 1 is spherical powder prepared by stirring ball-milling to the scanning electron microscope pattern of ball milling 60h powder particle
End SEM shape appearance figure, a figure is the powder particle under low power, and b figure is the powder particle under high power.It appeared that powder from Fig. 1
Grain very fine uniform, shape very convergence is spherical, and high tap density is favorably improved the useful load of injection feeding, Large ratio surface
The long-pending sintering activity that can improve powder, good sphericity is then conducive to improving the mobility of powder, and this shows that ball milling significantly improves
The shape of powder and granularity, i.e. improve the operational characteristic of powder, and it is high that stirring ball-milling 60h has prepared nitrogen content, and granule is thin
Little, the high-nitrogen nickel-free rustless steel composite powder of good sphericity, has good mobility, high useful load and sintering activity, very
The injection of suitable metal powder injection forming and the needs of sintering process.
(2) preparation and the injection molding process of feeding are injected
In embodiments of the present invention, the adhesive of employing is mainly by polyformaldehyde (POM), high density polyethylene (HDPE) (HDPE), second
Alkene-vinyl acetate copolymer (EVA) and stearic acid (SA) composition, 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.Compared to common binding agent, the adhesive of the present invention has that removing speed is fast, stream
The dynamic feature that property is good, conformality is high, with low cost, is well suited for the feeding for making METAL INJECTION MOLDING OF STAINLESS STEELS goods, energy
Realize the quick zero defect defat of product, and guarantee its high dimensional accuracy.
By the high nitrogen spherical powder of adhesive and ball milling 60h according to volume ratio (40~46): (54~60) mix after close
Carry out on refining machine mixing make be evenly distributed, granular injection feeding that rheological property is excellent, melting temperature is 175~185 DEG C, time
Between be 60~90min.Feeding is carried out on injection machine injection moulding, injection temperature 180~190 DEG C, injection pressure be 80~
120MPa, the zero defect obtaining required form shapes base.
Fig. 2 be powder volume mark be feeding when 58% at 185 DEG C, the injection obtained under the injection parameters of 110MPa is raw
Base material object photo and the SEM shape appearance figure of internal fracture, wherein, a figure is pictorial diagram, and b figure is the fracture SEM shape appearance figure that a figure is in kind.
Injection base substrate mainly includes following three kinds: a kind of is injection moulding MPIF35 standard tensile sample, for testing the tensile force of material
Learn performance;Another kind is the disk of Ф 20mm × 5mm, for testing the decay resistance of material;The third is a kind of complex shape
The ball-screw reverser part blanks of shape, for testing the dimensional accuracy of sintered article.Figure it is seen that injection base table
Face is bright and clean smooth, does not occur filling the defects such as type deficiency, face crack, distortion, hole, from fracture photo it can be seen that in base substrate
Portion's adhesive is mixed homogeneously with powder, and does not produce the segregation phenomenon of powder.
(3) catalysis degreasing technique
Being positioned in catalysis degreasing stove by injection moulding green compact and carry out defat, degreasing process is as follows: skimming temp 120 DEG C~
130 DEG C, degreasing time 4~6h, protective gas N2Being passed through speed is 400~500mL/min, is catalyzed gas HNO3Being passed through speed is
0.05~0.10mL/min.Owing to the main constituent element polyformaldehyde in adhesive is very sensitive, at nitric acid vapor to acid atmosphere
Being cracked into formaldehyde gas rapidly under catalytic action and remove, shaping base is after 4~6h catalysis degreasings, and total removing amount of adhesive is
Reaching more than 85%, it is complete that the most main adhesive polyformaldehyde decomposes removing substantially, and catalysis degreasing process is complete.Catalysis degreasing
Degreasing effect preferable, not only degreasing time is considerably shorter than the thermal debinding time, and catalytic reaction temperature is less than acetal resin
Fusing point, does not produce liquid phase in whole skimming processes, therefore defat base quality is good, do not occur any crackle, pore, deformation,
The defat defect such as caving in, inside has formed substantial amounts of connected pore channel the most.After catalysis degreasing completes, it is the most right also to remain in base substrate
Being catalyzed the insensitive HDPE of atmosphere and EVA polymer adhesive, these binding agents can not be decomposed, in later stage conduct by catalysis gas
Skeleton will play conformal effect, and these remaining adhesives can be pyrolyzed rapidly removing at pre-sintered state.
(4) sintering process
Degreasing blank after catalysis degreasing is placed in vacuum tube furnace order and carries out the removing process of remaining adhesive, burn
Knot densification, and solution heat treatment, obtain saving nickel high-nitrogen austenitic stainless steel goods.Fig. 3 is the de-of remaining adhesive
Except processing and densification process curve figure, specifically comprise the following steps that
A, the removing of remaining adhesive
As it is shown on figure 3, under the conditions of coarse vacuum (vacuum >=10Pa), from room temperature start with 5 DEG C/min ramp to
350 DEG C of insulation 30min, with the very small amount polyformaldehyde remained in thoroughly removing base substrate and other impurity, and decompose temperature for delayed heat
The removing that starts spending high binding agent constituent element is prepared;With 2 DEG C/min ramp to 420 DEG C of insulation 40min, primarily to
Remove the EVA polymer in adhesive;It is heated to 500 DEG C of insulation 40min with 2 DEG C/min heating rate, makes high density polyethylene (HDPE)
The most all remove;It is incubated 60min, it is ensured that the whole binding agents removing in injection base is dry with 2 DEG C/min ramp to 550 DEG C
Only, so far degreasing process has been fully completed.
B, sintering densification process
Owing to the oxygen content of ball milling 60h powder is higher, it is detected as 1.16%, uses conventional sintering process will aoxidize
Thing is mingled with and effectively reduces, and will have influence on and finally sinter serviceability, and be transferred to height by coarse vacuum immediately after therefore defat terminates
Vacuum condition (vacuum >=1.0 × 10-2Pa), as it is shown on figure 3, be incubated 30min, mesh with 8 DEG C/min ramp to 1150 DEG C
Be in ball milling material powder add graphitic carbon as interior reducing agent, make the metal-oxide in defat base in a vacuum
There is reduction reaction in (such as ferrum oxide, chromium oxide, manganese oxide etc.) and carbon, makes oxygen atom with carbon monoxide or carbon dioxide as far as possible
The form of gaseous product is discharged, and the active metal atom energy activated sintering discharged, improve stainless sintered density further
And ductility;Then being warmed up to 1270 DEG C with the speed of 5 DEG C/min, deoxygenation proceeds in the process, when arriving sintering
Closing vacuum after temperature, the high pure nitrogen being filled with circulation is sintered 90min, and nitrogen flow is 1.0~1.2L/min, has sintered
Furnace cooling after one-tenth.
C, solution heat treatment
In order to eliminate fragility Nitride Phase that is slow due to cooling rate in sintered body and that separate out, follow-up solution heat treatment need to be carried out,
Sintered article is reheated to 1100 DEG C of insulations 60min, then water quenching coolings, obtains saving nickel high-nitrogen austenitic stainless steel system
Product.
Effect example
The joint nickel high-nitrogen austenitic stainless steel goods obtained in embodiment are observed, observed result such as Figure 4 and 5 institute
Show.
Fig. 4 is the photo in kind of joint nickel high-nitrogen austenitic stainless steel sintered article, it is seen that shape of product is intact, contraction is equal
Even, the defects such as deformation, crackle do not occur.
Fig. 5 is the SEM photograph after joint nickel high-nitrogen austenitic stainless steel solution treatment, is single austenite under room temperature state
, there is not ferrite in grain structure, does not has fragility nitride to separate out yet, and illustrates that intensified element nitrogen is entirely and deposits with the form of solid solution
It is in austenite for rustless steel, there is good combination property and provide guarantee.Due to high-energy ball milling make powder granule and
Crystal grain has obtained notable refinement, and a large amount of crystal defects that ball milling produces simultaneously promote atoms permeating during sintering, drop further
Sintering activating energy and the sintering of low body of powder are temperature required, and the densification temperature ratio of ball milling 48h powder is similar in the present invention
The densification temperature of the atomized alloy powder of composition about reduces 30~40 DEG C, causes the Austria in final sintered stainless steel goods
Family name's body crystal grain is the most tiny, only about 10~15 μm, and this superfine organizational structure obviously helps and improves stainless making
Use performance.
The joint nickel high-nitrogen austenitic stainless steel goods obtained in embodiment are carried out service check, and result is as follows: Jing Guogu
After molten process, stainless steel products obtains the excellent combination of sintered density, nitrogen content and performance, and sintering relative density reaches
98.4%, nitrogen content is up to 0.88%, oxygen content 0.21%, carbon content 0.026%, yield strength σ0.2=638MPa, tension is strong
Degree σb=994MPa, percentage elongation δ5=32.6%, contraction percentage of area ψ=50.3%, impact flexibility α kv=112J/cm2, hardness
HV10=308,60 DEG C of air blowing pitting potential Ep >=700mV in 22%NaCl solution, at normal saline, the simulating blood plasma of 37 DEG C
With pitting potential Ep >=1200mV in Hank ' s solution.
Joint nickel high-nitrogen austenitic stainless steel prepared by the present invention is not in the case of losing plasticity and toughness, its intensity, hardness, resistance to
The indexs such as corrosive nature, especially pitting resistance considerably beyond traditional 304,316L, 317L chromium-nickel austenitic stainless steel,
Meet or exceed the advanced level of the similar joint nickel high-nitrogen austenitic stainless steel material reported in the world, for industrial circle
In high strength anti-corrosion joint nickel and stainless steel structural material and medical and health industry in high-quality, safe and reliable low nickel or stainless without nickel
Steel embedded material aspect has great development potentiality and prospect.Anti-to the complicated shape ball-screw of preparation with statistical method
Shape and size precision to device part is tested, its dimensional accuracy about ± 0.15%~± 0.2%, right higher than industrial
The required precision of metal powder injection molded goods ± 0.3%, therefore, it is possible to realize industrialization large-scale production.
Compare the shortcoming and defect with prior art, the method have the advantages that the present invention is by high-energy stirring ball
Mill and metal powder injection molded two kinds of techniques organically combine and prepare that crystal grain is tiny, consistency and nitrogen content height, excellent performance,
Dimensional accuracy is high, can meet the joint nickel high-nitrogen austenitic stainless steel goods of industrialization batch production requirements, complies fully with new material
Resources conservation that exploitation is proposed, healthy friendly, cost is lower, performance more preferably objective and requirement.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (8)
1. the preparation method saving nickel high-nitrogen austenitic stainless steel goods, it is characterised in that comprise the following steps:
(1) by raw material in a nitrogen environment with the steel ball of Φ 7~Φ 9mm with 400~500r/min rotating speed ball millings 12~72h,
Obtaining spherical powder, wherein, described raw material is (10: 1)~(14: 1) with the ratio of grinding media to material of steel ball;
(2) the joint nickel high nitrogen stainless steel spherical powder that step (1) is obtained and adhesive (54~60) by volume: (40~46)
After mixing in mixing roll mixing obtain inject feeding, wherein, melting temperature is 175~185 DEG C, mixing time be 60~
90min;Described injection feeding is carried out injection moulding in injection machine, obtains shape flawless shaping base, wherein, injection temperature
Degree is 180~190 DEG C, and injection pressure is 80~120MPa;
(3) shaping base step (2) obtained is in catalysis degreasing stove and at nitrogen and HNO3Defat is carried out under gaseous environment,
To degreasing blank, wherein, skimming temp is 120 DEG C~130 DEG C, and degreasing time is 4~6h;
(4) degreasing blank that step (3) obtains is placed in vacuum tube furnace order and carries out the removing process of remaining adhesive, burn
Knot densification, and solution heat treatment, obtain saving nickel high-nitrogen austenitic stainless steel goods;The removing of described remaining adhesive
Process comprises the following steps:
Under vacuum >=10Pa, after room temperature starts with 5 DEG C/min ramp to insulation 30min when 350 DEG C, continue with 2
DEG C/min ramp to 420 DEG C time insulation 40min after, insulation when continuing to be heated to 500 DEG C with 2 DEG C/min heating rate
After 40min, continue to be incubated 60min with 2 DEG C/min ramp to 550 DEG C.
2. the preparation method saving nickel high-nitrogen austenitic stainless steel goods as claimed in claim 1, it is characterised in that in step
(1), in, described raw material is iron powder, chromium powder, manganese powder, molybdenum powder and graphite powder (66~72) in mass ratio: (16~18): (10~
12): (2.0~3.5): obtain after (0.1~0.3) mix homogeneously.
3. the preparation method saving nickel high-nitrogen austenitic stainless steel goods as claimed in claim 2, it is characterised in that described ferrum
The granularity of powder, chromium powder, manganese powder, molybdenum powder and graphite powder is 200 mesh.
4. the preparation method saving nickel high-nitrogen austenitic stainless steel goods as claimed in claim 3, it is characterised in that in step
(1), in, 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 saving nickel high-nitrogen austenitic stainless steel goods as claimed in claim 4, it is characterised in that in step
(2), in, described adhesive includes the most each component:
6. the preparation method saving nickel high-nitrogen austenitic stainless steel goods as claimed in claim 5, it is characterised in that in step
(3), in, the speed that is passed through of described nitrogen is 400~500mL/min, described HNO3It is 0.05~0.10mL/ that gas is passed through speed
min。
7. the preparation method saving nickel high-nitrogen austenitic stainless steel goods as claimed in claim 1, it is characterised in that described sintering
Densification comprises the following steps:
After the removing step of described remaining adhesive, adjust vacuum >=1.0 × 10-2Pa, continues with 8 DEG C/min speed liter
After temperature to 1150 DEG C insulation 30min, continue to close when being warmed up to 1270 DEG C with the speed of 5 DEG C/min vacuum and at nitrogen flow be
After sintering 90min under 1.0~1.2L/min environment, furnace cooling obtains sintered article.
8. the preparation method saving nickel high-nitrogen austenitic stainless steel goods as claimed in claim 7, it is characterised in that described solid solution
Heat treatment comprises the following steps: described sintered article is reheated to 1100 DEG C of insulations 60min, then water quenching coolings.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310692084.5A CN103706793B (en) | 2013-12-18 | 2013-12-18 | A kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310692084.5A CN103706793B (en) | 2013-12-18 | 2013-12-18 | A kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103706793A CN103706793A (en) | 2014-04-09 |
CN103706793B true CN103706793B (en) | 2016-08-17 |
Family
ID=50400342
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201310692084.5A Expired - Fee Related CN103706793B (en) | 2013-12-18 | 2013-12-18 | A kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103706793B (en) |
Families Citing this family (28)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6655542B2 (en) * | 2014-09-25 | 2020-02-26 | 東洋アルミニウム株式会社 | Concrete formwork, method for producing concrete compact, and method for producing concrete structure |
CN105127695A (en) * | 2015-10-16 | 2015-12-09 | 新华手术器械有限公司 | One-time forming quick processing method applicable to medical tweezers or clip |
CN105290392B (en) * | 2015-12-08 | 2017-09-29 | 重庆文理学院 | A kind of 304L stainless steel metals powder injection forming method |
CN105772728A (en) * | 2016-04-24 | 2016-07-20 | 连云港东睦新材料有限公司 | Method for producing novel air cylinder of air-conditioning compressor by power injection |
CN106735170B (en) * | 2016-12-20 | 2019-01-25 | 佛山铂利镁特金属科技有限公司 | A kind of injection moulding method of big part metalwork |
CN107297503A (en) * | 2017-06-21 | 2017-10-27 | 合肥市旺友门窗有限公司 | A kind of preparation method of high nitrogen colored stainless steel product |
CN107598171B (en) * | 2017-08-16 | 2019-04-12 | 北京科技大学 | A kind of sea water desalination conduit coupling high nitrogen biphase stainless steel near-net-shape method |
CN107775005B (en) * | 2017-11-29 | 2019-08-02 | 安徽恒利增材制造科技有限公司 | A kind of injection molding method of high-strength aluminum alloy turbine wheel |
CN108031851A (en) * | 2017-12-28 | 2018-05-15 | 西安交通大学 | A kind of preparation method of austenitic stainless steel alloy |
CN108817402A (en) * | 2018-06-26 | 2018-11-16 | 深圳市鑫迪科技有限公司 | Metallic powder injection moulding process |
CN108889952A (en) * | 2018-06-26 | 2018-11-27 | 深圳市鑫迪科技有限公司 | Using the method for metal powder injection molding preparation metal gear |
CN109014211B (en) * | 2018-08-09 | 2021-03-12 | 上海富驰高科技股份有限公司 | Low-cost MIM (metal-insulator-metal) manufacturing process for high-nitrogen non-magnetic high-strength stainless steel part |
CN109261864A (en) * | 2018-09-29 | 2019-01-25 | 中国航发哈尔滨轴承有限公司 | A kind of Cronidur30 high nitrogen stainless steel bearing ring blank forging manufacturing process |
CN109702205A (en) * | 2019-03-08 | 2019-05-03 | 成都双创时代科技有限公司 | A kind of austenitic stainless steel metal powder injection molding components heat treatment process |
CN110000389B (en) * | 2019-03-14 | 2020-07-31 | 全亿大科技(佛山)有限公司 | Method for preparing stainless steel |
CN110142413A (en) * | 2019-05-30 | 2019-08-20 | 华南理工大学 | It is a kind of for metal powder injection molded no wax pattern feeding and preparation method thereof |
CN110295308B (en) * | 2019-07-12 | 2020-10-16 | 歌尔股份有限公司 | Preparation method of stainless steel material |
CN110480014B (en) * | 2019-08-20 | 2022-02-18 | 扬州海昌新材股份有限公司 | Method for producing multifunctional outer circle chamfer cutter by taking powder as raw material |
CN110405214B (en) * | 2019-08-26 | 2021-11-05 | 怡力精密制造有限公司 | Preparation method of stainless steel material |
CN110699614B (en) * | 2019-11-04 | 2021-08-06 | 南华大学 | B-C-N-O supersaturated solid solution austenitic stainless steel powder and preparation and cladding methods |
CN111519006B (en) * | 2020-04-24 | 2021-04-20 | 深圳市泛海统联精密制造股份有限公司 | Vacuum solid solution method for high manganese nitrogen nickel-free stainless steel |
CN111570802B (en) * | 2020-05-27 | 2021-08-20 | 中南大学 | 3D printing manufacturing process of ultrathin metal-based diamond cutting blade |
CN111451507A (en) * | 2020-05-27 | 2020-07-28 | 江苏省海洋资源开发研究院(连云港) | Near-net forming method of high-nitrogen nickel-free austenitic stainless steel |
CN112605390B (en) * | 2020-10-19 | 2022-08-26 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of vacuum-grade low-nitrogen metal chromium for preparing high-temperature alloy by using chromium powder |
CN112195419A (en) * | 2020-11-23 | 2021-01-08 | 浙江宝武钢铁有限公司 | Preparation method of corrosion-resistant high-nitrogen stainless steel |
CN113862582B (en) * | 2021-08-25 | 2023-04-14 | 江苏精研科技股份有限公司 | Non-magnetic nickel-free polishing product and preparation method thereof |
CN113732287A (en) * | 2021-09-13 | 2021-12-03 | 东莞市环力智能科技有限公司 | Non-magnetic sintering process for 17-4 products |
CN114737117A (en) * | 2022-03-31 | 2022-07-12 | 广东潮艺金属实业有限公司 | High-hardness and high-rust-resistance stainless steel 316L and sintering process thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10195502A (en) * | 1997-01-09 | 1998-07-28 | Ritsumeikan | Stainless steel powder, stainless steel member and production of the stainless steel member |
CN101125368A (en) * | 2007-10-09 | 2008-02-20 | 北京科技大学 | Method for preparing globular high-nitrogen stainless steel powder using with high-energy ball mill |
CN101353561A (en) * | 2008-09-04 | 2009-01-28 | 中南大学 | Catalysis degreasing type adhesive for powder injection moulding and preparation of material feeding thereof |
-
2013
- 2013-12-18 CN CN201310692084.5A patent/CN103706793B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10195502A (en) * | 1997-01-09 | 1998-07-28 | Ritsumeikan | Stainless steel powder, stainless steel member and production of the stainless steel member |
CN101125368A (en) * | 2007-10-09 | 2008-02-20 | 北京科技大学 | Method for preparing globular high-nitrogen stainless steel powder using with high-energy ball mill |
CN101353561A (en) * | 2008-09-04 | 2009-01-28 | 中南大学 | Catalysis degreasing type adhesive for powder injection moulding and preparation of material feeding thereof |
Non-Patent Citations (2)
Title |
---|
固溶处理对注射成形0Cr17Mn11Mo3N钢组织性能的影响;李科等;《材料热处理学报》;20070228;第28卷(第1期);第58-61页 * |
粉末注射成形催化脱脂工艺研究;郑礼清等;《粉末冶金工业》;20090430;第19卷(第2期);第32-35页 * |
Also Published As
Publication number | Publication date |
---|---|
CN103706793A (en) | 2014-04-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103706793B (en) | A kind of preparation method saving nickel high-nitrogen austenitic stainless steel goods | |
CN101342591B (en) | Method of manufacturing powder metallurgy nitrogen/high nitrogen containing stainless steel parts | |
CN108103381B (en) | High-strength FeCoNiCrMn high-entropy alloy and preparation method thereof | |
CN104278200B (en) | High-hot-strength spray-formed hot work die steel and preparation method thereof | |
CN102650021B (en) | Bainite pre-hardening plastic mold steel and preparation method and heat treatment method thereof | |
CN103667766B (en) | A kind of nitro-alloy and preparation method thereof | |
CN104043672B (en) | Extra-supercritical unit high-quality P92 method for manufacturing large-diameter thick-wall seamless steel pipe | |
CN109848420A (en) | A kind of 440C stainless steel metal powder injection forming method and its product | |
CN101353768A (en) | Nitrogen-containing nickel-free stainless steel and metallurgy forming process for powder thereof | |
CN104388789B (en) | Nanostructure tungsten-zirconium carbide alloy and preparation method thereof | |
CN113502428B (en) | Method for preparing high-nitrogen nickel-free austenitic stainless steel and product thereof | |
CN105274440A (en) | Oxide dispersion strengthened (ODS) steel preparing method and martensitic steel | |
CN113136531A (en) | Powder metallurgy stainless steel and preparation method thereof | |
CN110819842A (en) | Preparation method of formed part based on reduced graphene oxide and copper composite material | |
CN110238401A (en) | A kind of method that powder rolling prepares high-compactness Fine Grain Ti Alloy | |
CN104550956A (en) | Component preparation method through beta-gamma titanium-aluminum alloy prealloy powder spark plasma sintering | |
CN109338219A (en) | A kind of wind power flange super-thick steel plate and its production method | |
CN102605245A (en) | Ni-free normalized type Q370R pressure vessel steel plate and manufacturing method thereof | |
CN104018063B (en) | The production method of low-alloy high-strength Q420C medium plates | |
CN115125431B (en) | Method for refining low-activation ferrite martensite steel structure | |
CN111979499A (en) | Production method of low-cost Q460C thick steel plate | |
CN114480943A (en) | Ultralow-carbon low-cobalt martensitic steel and preparation method thereof | |
CN106834870B (en) | Ni-Al2O3Composite material near-net-shape method | |
CN113913669A (en) | Preparation method of P-containing high-strength stainless steel product | |
CN111020279B (en) | High-strength high-conductivity copper-graphite composite material and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
DD01 | Delivery of document by public notice |
Addressee: Cui Dawei Document name: Notice of termination of patent |
|
DD01 | Delivery of document by public notice | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160817 Termination date: 20191218 |
|
CF01 | Termination of patent right due to non-payment of annual fee |