CN104946994B - Preparation method for nano-crystallization low-alloy heat-resistant high-strength steel mould - Google Patents
Preparation method for nano-crystallization low-alloy heat-resistant high-strength steel mould Download PDFInfo
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Abstract
The invention relates to a preparation method for a nano-crystallization low-alloy heat-resistant high-strength steel mould. The preparation method comprises the following steps: (1) preparing low-alloy steel from the following components in percentage by weight: 0.09-0.15% of C, 1.35-1.55% of Cr, 0.22-0.28% of Si, 0.33-0.38% of Mn, 0.17-0.24% of Mo, 0.05-0.15% of Ni, 0.05-0.08% of Nb, 0.15-0.35% of V, less than or equal to 0.010% of P, less than or equal to 0.010% of S and the balance of Fe and inevitable impurities; (2) processing the low-alloy steel obtained in the step (1) into a required dimension and a required shape, thereby obtaining a low-alloy steel mould; and (3) carrying out surface nanocrystallization treatment on the low-alloy steel mould prepared in the step (2). The nano-crystallization low-alloy heat-resistant high-strength steel mould prepared by the preparation method disclosed by the invention is improved in heat resistance and corrosion resistance; and meanwhile, the varieties of the alloys are reduced, the impurity components are simpler and easy to control, and a nitride effective penetrating layer is remarkably increased in thickness.
Description
Technical field
The present invention relates to a kind of preparation method of alloy mold, especially a kind of nanosizing low-alloy heat-resistant high-strength steel mould
Preparation method.
Background technology
(it is often referred to more than 0.3～0.5 times of material melting point of temperature) under hot conditions, there is non-oxidizability and sufficiently high
The steel of warm intensity and good heat resistance is referred to as heat resisting steel, and in heat resisting steel, a most representational class is low-alloy steel,
The 15crmo of such as China is a kind of typical low-alloy steel, and 15crmo is because of its good heat resistance, mechanical property, corrosion resistant
Corrosion energy and be widely used in boiler, petrochemical industry, coal conversion, the use condition such as steam turbine wheel cylinder body, thermoelectricity, nuclear power harsh,
The complicated pipeline of main equipment of corrosive medium, container, parts etc..
General 15crmo chemical composition (mass fraction) (%) is: c 0.12～0.18, mn 0.40～0.70, si
0.17～0.37, cr 0.80～1.10, mo 0.40～0.55, ni≤0.30, s≤0.035, p≤0.035.The power of 15crmo
Learn performance: tension intensity is 440～640mpa, yield point about 235mpa, percentage elongation 21% about.
Developing rapidly however as modern industry, 15crmo heat-resistance high-strength steel has been increasingly difficult to meet industrial equipment
In the higher requirement of the aspects such as obdurability, creep properties, weldability, in the production engineering such as optimized alloy composition, adjustment are smelted, rolling
Technological parameter be increasingly becoming people's focus of interest for improving 15crmo steel.Simultaneously as needs to be obtained is excellent
Wearability and fatigue durability etc. in addition it is also necessary to it is carried out with the heat treatment such as carburizing and quenching, and this so that product is produced certain
Deformation and affect the dimensional accuracy of product.
A kind of preparation of low-alloy heat-resistant high-strength steel component is disclosed, with percentage by weight in patent 201110392208.9
Meter, comprises following components: c 0.09～0.11, and si 0.06～0.2, mn 0.06～0.35, cr 1.3～1.5, mo 0.35～
0.45, p≤0.009, s≤0.006, ni 0.2～0.4, cu 0.01～0.08, v 0.3～0.4, nb 0.1～0.2, w 0.2
～0.5, ti 0.005～0.02, balance of fe and inevitable impurity.The room temperature tensile intensity of this component is 610mpa,
At 600 DEG C, under 200mpa stress test, its useful life is about the twice of 15crmo, and the case hardness after heat treatment is about
750hv, and the thin hardened layer more than 500hv for the hardness is 0.5mm, and deflection is little, has been above general 15crmo.But
Wherein tenor is higher, is not applied for some special Production requirements, and the metal species comprising are many, production cost is relatively
High, it is possible to create impurity component also more complicated.
Metal nano qpq technology is to increase the change of nanosizing operation on the basis of retaining original common Nitriding Technology
Compound depth, is allowed to be deepened to more than 1000 μm by original 10-25 μm.Metal nano qpq technology includes nm deep and exists
More than 1000 μm of multistage gradient superfine nano-crystalline organized layer, nitriding operation more than 100 μm for the compound layer depth, or carbon nitrogen
The oxidation operation of permeation and its subsequent salt bath or gas is it is not necessary to original polishing process.With this technique to metal at
Reason does not need to spray any protective materials, and process is simple, and with low cost, energy-conserving and environment-protective are nuisanceless, and working environment cleans, outward
The features such as see attractive in appearance.This technology has accomplished that raw material are nontoxic free from environmental pollution, and every environmental protection index measures through environmental administration and all reaches
To national standard, make wearability, corrosion resistance and the mechanical property hardness strength of metal surface have carrying by a larger margin simultaneously
High.
Existing common Nitriding Technology has significant limitation in application aspect, its reason be exactly compound layer depth too
Shallow it is impossible to bear heavy load it is impossible to bear high speed load it is impossible to bear larger abrasion.If compound layer depth is become number
The raising of magnitude, the wearability of infiltration layer also can be correspondingly improved.Metal nano qpq technology can be used for nitrogenizing than common
The bigger mould of the bigger load of technology, more speed, wear extent.The mould of common nitrogen treatment can not bear grinding, but metal
The mould of nanosizing qpq technical finesse can bear grinding, and therefore metal nano qpq technology more can be used for high accuracy precision
Mould.
Content of the invention
For the problems of the prior art problem, it is an object of the invention to provide a kind of nanosizing low-alloy heat-resistant high-strength steel
The preparation method of mould.
The technical solution adopted in the present invention is as follows:
A kind of preparation method of nanosizing low-alloy heat-resistant high-strength steel mould, it comprises the following steps:
(1) by weight percentage, the component of following proportioning is prepared low-alloy steel: c 0.09～0.15, cr 1.35～
1.55, si 0.22～0.28, mn 0.33～0.38, mo 0.17～0.24, ni 0.05～0.15, nb 0.05～0.08, v
0.15～0.35, ti 0.008～0.015, p≤0.010, s≤0.010, balance of fe and inevitable impurity；
(2) low-alloy steel obtaining step (1) is processed into the size and dimension of needs, prepares low-alloy punching block
Tool；
(3) low-alloy steel mould prepared by step (2) carries out Surface Nanocrystalline.
Further,
The described method preparing low-alloy steel of step (1) comprises the steps:
(11) smelt cast: sequentially carry out refining at the beginning of electric arc furnaces, ladle rh is processed and lf process, control molten steel to meet restriction
Argon is carried out at least 5 minutes with the pressure of more than 3atm, to be conducive to impurity during cast, wherein ladle refining after chemical composition
Float and remove；
(12) roll: include all heat-treated, rolling and cooling, wherein all heat-treated is the heating furnace at 1100～1150 DEG C
Middle soaking about 4～6 hours, the start rolling temperature of rolling is 950～1050 DEG C, finishing temperature is 840～880 DEG C, and mill speed is 3
～5m/s, cooling velocity be 5～10 DEG C/s, cooling after finishing temperature be 650～680 DEG C.
Surface Nanocrystalline described in step (3) comprises the steps:
(31) nanosizing: described low to be impacted with the frequency of 10-20khz using the tungsten alloy cutter for 280-480w for the power
The surface of Alloy-steel mold；Impact energy produces the compression of 450-650mpa；Make to be strengthened thus realizing by impact site
Nanosizing, forms nano-micrometre gradient-structure on surface；
(32) the low-alloy steel mould of nanosizing is put into crucible, be heated to 450 DEG C, add saline oxide 2～5kg beginning
Salt melts to saline oxide；Again base salt is added in crucible by several times, after heating base salt all melts, salt bath face rises to apart from crucible
Stop during top edge 120mm adding base salt, add adjustment salt 1～2kg, run 2.5h under the conditions of 200～350 DEG C；
(33) aoxidize: the crucible cleaning rustless is hung in oxidation furnace, instrument constant temperature, at 220 DEG C, puts the workpiece in crucible,
Thermocouple is against sidewall of crucible；Then saline oxide is added in crucible, be added to the 1/3 of crucible height, be then electrified to melt；For the first time
The salt adding is gradually added into saline oxide after all melting again, adds suitable number every time, and side is melted, and side adds, until liquid level
It is increased to till crucible top edge 200mm；After salt bath face reaches the height of requirement, 250 DEG C of insulations, make moisture a large amount of
Volatilization, till liquid level no longer has bubble generation calmness completely；Then salt temperature heats up 15～20 DEG C again, so circulates,
Until temperature is raised to 350 DEG C；
(34) immersion oil: low-alloy steel mould is put into immersion 1～2min in machinery oil, then oil droplet is done.
Preferably,
Adjustment salt described in step (32) is made up of following components in parts by weight: na2co320-30 part, k2co320-30 part,
Nacl 20-30 part, kcl 20-30 part, nh4Cl 10-20 part, ce2co32-4 part, beo 2-4 part.
Saline oxide described in step (32) and (33) is selected from na2co3、k2co3Or the mixture of the two.
Base salt described in step (32) is selected from the mixture of potassium cyanate and metal oxide.
It is further preferred that base salt described in base salt includes following components in parts by weight: potassium cyanate 80- described in step (32)
100 parts, ce2co31-3 part, zro20.5-1.5 part, ceo20.5-1.5 part.
In the present invention, the nano-micrometre gradient-structure that the nanosizing process of step (31) produces can significantly increase metal
The synthesis military service performance of material and military service behavior.Metal material, after making Nano surface processing, forms body between table is nanocrystalline
Fraction is that 100% interface provides preferable passage for Elements Diffusion, can significantly accelerate the dynamic process spreading, make
The nitrogen treatment of metal material surface be easier to make for, obvious processing effect；Nanosizing can also be using this area routine
Other modes are carried out, such as zl03111200.5 (gas-solid two-phase flow impact metal material surface nano apparatus and its application),
Receiving disclosed in the patents such as zl200510029205.3 (the metal-surface nano method of ultrasonic wave high energy surface machining)
Riceization method is all applied to the present invention.
The nanosizing low-alloy heat-resistant high-strength steel mould heat resistance of the present invention and corrosion resistance are obtained for raising, reduce simultaneously
The species of alloy, is that impurity component is simpler, easy to control, nitride effective codiffusional layer thickness also dramatically increases.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
Prepare the nanosizing low-alloy heat-resistant high-strength steel mould of embodiment 1 in accordance with the following steps:
(1) by weight percentage, the component of following proportioning is prepared low-alloy steel: c 0.09, cr 1.45, si
0.30, mn 0.33, mo 0.17, ni 0.15, nb 0.05, v 0.15, ti 0.0015, p 0.002, s 0.002, balance of
Fe and inevitable impurity；
(11) smelt cast: sequentially carry out refining at the beginning of electric arc furnaces, ladle rh is processed and lf process, control molten steel to meet restriction
Argon is carried out at least 5 minutes with the pressure of more than 3atm, to be conducive to impurity during cast, wherein ladle refining after chemical composition
Float and remove；
(12) roll: include all heat-treated, rolling and cooling, wherein all heat-treated is soaking in 1150 DEG C of heating furnace
About 5 hours, the start rolling temperature of rolling was 1000 DEG C, finishing temperature is 850 DEG C, and mill speed is 4m/s, cooling velocity is 5 DEG C/
Finishing temperature after s, cooling is 680 DEG C.
(2) low-alloy steel obtaining step (1) is processed into the block low-alloy steel mould of 40mm × 20mm × 3mm；
(3) low-alloy steel mould prepared by step (2) carries out Surface Nanocrystalline；
(31) nanosizing: using the tungsten alloy cutter for 480w for the power so that described low-alloy is impacted with the frequency of 10-20khz
The surface of steel mold；Impact energy produces the compression of 500-650mpa；Make to be strengthened thus realizing nanometer by impact site
Change, form nano-micrometre gradient-structure on surface；
(32) the low-alloy steel mould of nanosizing is put into crucible, be heated to 450 DEG C, add saline oxide 3kg to start salt dissolving
To saline oxide fusing；Again base salt is added in crucible by several times, after heating base salt all melts, salt bath face rises on crucible
Stop during portion edge 120mm adding base salt, add adjustment salt 2kg, run 2.5h under the conditions of 220 DEG C；
(33) aoxidize: the crucible cleaning rustless is hung in oxidation furnace, instrument constant temperature, at 220 DEG C, puts the workpiece in crucible,
Thermocouple is against sidewall of crucible；Then saline oxide is added in crucible, be added to the 1/3 of crucible height, be then electrified to melt；For the first time
The salt adding is gradually added into saline oxide after all melting again, adds suitable number every time, and side is melted, and side adds, until liquid level
It is increased to till crucible top edge 200mm；After salt bath face reaches the height of requirement, 250 DEG C of insulations, make moisture a large amount of
Volatilization, till liquid level no longer has bubble generation calmness completely；Then salt temperature heats up 20 DEG C again, so circulates, until
Temperature is raised to 350 DEG C；
(34) immersion oil: low-alloy steel mould is put into l-an32# total loss system oil (product execution gb443-89 mark
Standard, purchased from Jinan You Run Chemical Co., Ltd.) then oil droplet is done by middle immersion 2min.
Adjustment salt described in step (32) is made up of following components in parts by weight: na2co330 parts, k2co330 parts, nacl
30 parts, 25 parts of kcl, nh415 parts of cl, ce2co32 parts, 2 parts of beo.
Described in step (32) and (33), saline oxide is na2co350wt% and k2co3The blend of 50wt%.
Base salt described in base salt described in step (32) includes following components in parts by weight: 100 parts of potassium cyanate, ce2co33 parts,
zro21.5 part, ceo21.5 part.
The nitriding furnace of step (32) and step (33) and oxidation furnace apparatus are that Cheng Long industrial furnace Co., Ltd of Foshan City produces
Qpq liquid salt bath composite nitride stove oxidation furnace, model: snyn-20-6, rated temperature be 650 DEG C, workspace a size of φ
400mm × 550mm, it starts (hydraulic pressure or manual) by furnace shell, bell, heat-insulated furnace lining, heating element heater, heat-resisting steel crucible, bell
The part such as device forms.
Embodiment 2
According to embodiment 1 methods described, but base salt described in step (32) is following components in parts by weight: potassium cyanate 100
Part, ce2co33 parts, zro23 parts.Obtain the nanosizing low-alloy heat-resistant high-strength steel mould of embodiment 2.
Embodiment 3
According to embodiment 1 methods described, but base salt described in step (32) is following components in parts by weight: potassium cyanate 100
Part, ce2co33 parts, ceo23 parts.Obtain the nanosizing low-alloy heat-resistant high-strength steel mould of embodiment 3.
Embodiment 4
According to embodiment 1 methods described, but base salt described in step (32) is following components in parts by weight: potassium cyanate 100
Part, ceo23 parts, zro23 parts.Obtain the nanosizing low-alloy heat-resistant high-strength steel mould of embodiment 4.
Comparative example
According to embodiment 1 methods described, the Surface Nanocrystalline of step (3) in embodiment 1 is replaced with conventional quenching
Heat treatment；Conventional quenching heat treatment method is as follows:
Block low-alloy steel mould prepared by step (2) is put into after Carburization Treatment stove with vertical state, here perpendicular
Straight state refer to by mould three-dimensional the longest one-dimensional keep vertical as far as possible and be defined, be heated to 890 DEG C, and the speed with 90 droplets/minute
Degree instills methyl alcohol, passes through to control the flow of propane to maintain carbon potential in stove 0.85%, to be diffused Carburization Treatment 2 hours simultaneously,
Subsequently low-alloy steel mould is pre-chilled to 760 DEG C and reduces carbon potential in stove simultaneously and to 0.7% and be incubated 10 minutes, then by low-alloy
Steel mold take out from carburizer and oil temperature be 125 DEG C cooling oil in direct quenching, be tempered again after quenching, tempering temperature
Spend for 170 DEG C, tempering time is 1.5 hours, obtains the low-alloy steel mould of comparative example.
Test case
The low-alloy steel mould that embodiment 1-4 and comparative example are obtained carries out performance test, nitride effective codiffusional layer thickness
Measuring method and standard referring to " gb/t 11354-2005 steel-iron components depth of penetration measure and microstructure examination ", test
The results are shown in Table 1.
Table 1: the performance test table of embodiment 1-3 and comparative example
From table 1 result, the low-alloy steel mould that embodiment of the present invention 1-3 is obtained with comparative example 1 compares, under room temperature
Tensile strength is bigger, and yield point is higher, and case hardness is bigger.Especially embodiment 1, employs ce2co3、zro2、ceo2Three kinds
Oxide compounds and base salt is modified, better, due to being provided with thicker nitride effective codiffusional layer, using side of the present invention
The low-alloy steel mould of method preparation has good corrosion resistance.
The above, the only specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, and any
Those of ordinary skill in the art disclosed herein technical scope in, the change that can expect without creative work or
Replace, all should be included within the scope of the present invention.Therefore, protection scope of the present invention should be limited with claims
Fixed protection domain is defined.
Claims (6)
1. a kind of preparation method of nanosizing low-alloy heat-resistant high-strength steel mould, it comprises the following steps:
(1) by weight percentage, the component of following proportioning is prepared low-alloy steel: c 0.09～0.15, cr 1.35～
1.55, si 0.22～0.28, mn 0.33～0.38, mo 0.17～0.24, ni 0.05～0.15, nb 0.05～0.08, v
0.15～0.35, ti 0.008～0.015, p≤0.010, s≤0.010, balance of fe and inevitable impurity；
(2) low-alloy steel obtaining step (1) is processed into the size and dimension of needs, prepares low-alloy steel mould；
(3) low-alloy steel mould prepared by step (2) carries out Surface Nanocrystalline；
Surface Nanocrystalline described in step (3) comprises the steps:
(31) nanosizing: described low-alloy steel is impacted with the frequency of 10-20khz using the tungsten alloy cutter for 280-480w for the power
The surface of mould；Impact energy produces the compression of 450-650mpa；Make to be strengthened thus realizing nanosizing by impact site,
Form nano-micrometre gradient-structure on surface；
(32) the low-alloy steel mould of nanosizing is put into crucible, be heated to 450 DEG C, add saline oxide 2～5kg to start salt dissolving extremely
Saline oxide melts；Again base salt is added in crucible by several times, after heating base salt all melts, salt bath face rises to apart from crucible top
Stop during edge 120mm adding base salt, add adjustment salt 1～2kg, run 2.5h under the conditions of 200～350 DEG C；
(33) aoxidize: the crucible cleaning rustless is hung in oxidation furnace, instrument constant temperature, at 220 DEG C, puts the workpiece in crucible, thermoelectricity
Occasionally against sidewall of crucible；Then saline oxide is added in crucible, be added to the 1/3 of crucible height, be then electrified to melt；Add for the first time
Salt all melt after be gradually added into saline oxide again, add suitable number every time, side is melted, and side adds, until liquid level raises
To apart from crucible top edge 200mm；After salt bath face reaches the height of requirement, 250 DEG C of insulations, so that moisture is waved in a large number
Send out, till liquid level no longer has bubble generation calmness completely；Then salt temperature heats up 15～20 DEG C again, so circulates, directly
It is raised to 350 DEG C to temperature；
(34) immersion oil: low-alloy steel mould is put into immersion 1～2min in machinery oil, then oil droplet is done.
2. the preparation method of nanosizing low-alloy heat-resistant high-strength steel mould as claimed in claim 1: it is characterized in that: step
(1) the described method preparing low-alloy steel comprises the steps:
(11) smelt cast: sequentially carry out refining at the beginning of electric arc furnaces, ladle rh is processed and lf process, control molten steel to meet claim 1
Argon is carried out at least 5 minutes with the pressure of more than 3atm, to be conducive to during cast, wherein ladle refining after the chemical composition limiting
The floating of impurity removes；
(12) roll: include all heat-treated, rolling and cooling, wherein all heat-treated is equal in 1100～1150 DEG C of heating furnace
Heat about 4～6 hours, the start rolling temperature of rolling is 950～1050 DEG C, finishing temperature is 840～880 DEG C, mill speed is 3～
5m/s, cooling velocity be 5～10 DEG C/s, cooling after finishing temperature be 650～680 DEG C.
3. nanosizing low-alloy heat-resistant high-strength steel mould as claimed in claim 1 preparation method it is characterised in that: step
(32) base salt described in is selected from the mixture of potassium cyanate and metal oxide.
4. nanosizing low-alloy heat-resistant high-strength steel mould as claimed in claim 3 preparation method it is characterised in that: step
(32) base salt described in includes following components in parts by weight: potassium cyanate 80-100 part, ce2co31-3 part, zro20.5-1.5 part,
ceo20.5-1.5 part.
5. nanosizing low-alloy heat-resistant high-strength steel mould as claimed in claim 1 preparation method it is characterised in that: step
(32) adjustment salt described in is made up of following components in parts by weight: na2co320-30 part, k2co320-30 part, nacl 20-30
Part, kcl 20-30 part, nh4Cl 10-20 part, ce2co32-4 part, beo 2-4 part.
6. nanosizing low-alloy heat-resistant high-strength steel mould as claimed in claim 1 preparation method it is characterised in that: step
(32) and saline oxide described in (33) be selected from na2co3、k2co3Or the mixture of the two.
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| CN105803342B (en) * | 2016-04-20 | 2017-09-12 | 上海瀚氏模具成型有限公司 | A kind of preparation method of making Nano surface low-alloy steel mould |
| CN105714203B (en) * | 2016-04-20 | 2017-12-08 | 上海瀚氏模具成型有限公司 | A kind of preparation method of making Nano surface high-strength temperature-resistant steel mold |
| CN105803341B (en) * | 2016-04-20 | 2017-09-12 | 上海瀚氏模具成型有限公司 | A kind of preparation method of the anti-rotten steel mold of nanosizing low-alloy abrasion-proof |
| CN107975468A (en) * | 2017-11-23 | 2018-05-01 | 宁波升鸿机械设备有限公司 | A kind of vacuum pump |
| CN108396255A (en) * | 2018-03-01 | 2018-08-14 | 合肥康之恒机械科技有限公司 | A kind of power shovel with temperature variation resistant high-strength alloy steel making |
| CN109702442B (en) * | 2019-03-11 | 2022-04-22 | 精利模塑科技（无锡）有限公司 | Manufacturing method of precise and rapid forming automobile electronic die |
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| CN1699617A (en) * | 2005-06-29 | 2005-11-23 | 上海大学 | Technological process for surface low temperature boriding of low carbon steel |
| CN100491581C (en) * | 2006-12-08 | 2009-05-27 | 湖北工业大学 | Surface low-temperature boriding process for hot-work die steel |
| CN100595292C (en) * | 2007-06-15 | 2010-03-24 | 中国科学院金属研究所 | High speed processing method for realizing superfine crystal grain structure on metallic material surface |
| CN102304691A (en) * | 2011-09-09 | 2012-01-04 | 舒彩云 | New QPQ (quench-polish-quench) low-temperature salt bath nitridation composite treatment process |
| CN102433513B (en) * | 2011-11-29 | 2013-05-08 | 宁波兴柯汽车新材料科技有限公司 | Preparation and heat treatment method of low-alloy heat-resistant high-strength steel memebers |
| CN102505098B (en) * | 2011-11-29 | 2013-06-26 | 宁波市博祥新材料科技有限公司 | Low-alloy heat-resistant high-strength steel and member thereof |
| CN103305671B (en) * | 2013-05-17 | 2015-04-29 | 西安交通大学 | Method for performing gradient nano-crystallization on surface of metal |
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