CN104946994A - 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 preparation method of nanometer low-alloy heat-resistant high-strength steel mould.
Background technology
(temperature of more than 0.3 ~ 0.5 times of material melting point is often referred to) under hot conditions, the steel with oxidation-resistance and sufficiently high temperature intensity and good resistance toheat is called high temperature steel, and the representational class of most is low alloy steel in high temperature steel, namely the 15CrMo of such as China is a kind of typical low alloy steel, 15CrMo is because of its good resistance toheat, mechanical property, corrosion resistance nature and be widely used in boiler, petrochemical complex, coal transforms, steam turbine wheel cylinder body, thermoelectricity, the working conditionss such as nuclear power are harsh, the pipeline of the main equipment of corrosive medium complexity, container, component etc.
General 15CrMo chemical composition (massfraction) (%) 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 mechanical property of 15CRMO: tension intensity is 440 ~ 640MPA, and yield-point is about 235MPa, elongation about 21%.
But along with the develop rapidly of modern industry, 15CrMo heat-resistance high-strength steel has more and more been difficult to meet industrial equipments requirement higher in obdurability, creep properties, weldability etc., and the processing parameter in optimized alloy composition, production engineering such as adjustment smelting, rolling etc. becomes people day by day for the focus improved 15CrMo steel and pay close attention to.Meanwhile, due to the wear resistance and resistance to fatigue etc. of the excellence of needs will be obtained, also need to carry out it thermal treatments such as carburizing and quenching, and this often makes product produce certain deformation and affect the dimensional precision of product.
Disclose a kind of preparation of low-alloy heat-resistant high-strength steel component in patent 201110392208.9, by weight percentage, comprise following component: C 0.09 ~ 0.11, 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, surplus is 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 surface hardness after thermal treatment is about 750HV, and hardness is 0.5mm more than the thin hardened layer of 500HV, deflection is little, has all exceeded general 15CrMo.But wherein metal content is higher, can not be applicable to the Production requirement that some are special, and the metal species comprised is many, production cost is higher, and issuable impurity component is also more complicated.
Metal nano QPQ technology is on the basis retaining original common Nitriding Technology, increases the compound degree of depth of nanometer operation, makes it to deepen to more than 1000 μm by original 10-25 μm.Metal nano QPQ technology comprises the multistage gradient superfine nano-crystalline organized layer of nm deep more than 1000 μm, the nitriding operation of the compound layer degree of depth more than 100 μm, or the oxidation operation of carbonitriding and salt bath subsequently or gas, do not need original polishing process.To process metal by this technique and do not need to spray any protective material, and technique is simple, with low cost, energy-conserving and environment-protective are nuisanceless, and Working environment cleans, the features such as appearance looks elegant.This technology has accomplished that starting material are nontoxic free from environmental pollution, and every environmental protection index measures through environmental administration and is all up to state standards, and makes the wear resistance of metallic surface, erosion resistance and mechanical property hardness strength have raising by a larger margin simultaneously.
Existing common Nitriding Technology has significant limitation in application aspect, and its reason is exactly that the compound layer degree of depth is too shallow, can not bear heavy loading, can not bear high speed load, can not bear larger wearing and tearing.If the compound layer degree of depth is become the raising of the order of magnitude, the wear resistance of infiltration layer also can be improved accordingly.Metal nano QPQ technology may be used for than the larger load of common Nitriding Technology, more speed, mould that abrasion loss is larger.The mould of common nitriding treatment can not bear grinding, but the mould of metal nano QPQ technical finesse can bear grinding, and therefore metal nano QPQ technology more may be used for high precision precision die.
Summary of the invention
For the problems of the prior art problem, the object of this invention is to provide a kind of preparation method of nanometer low-alloy heat-resistant high-strength steel mould.
The technical solution adopted in the present invention is as follows:
A preparation method for nanometer 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, surplus is Fe and inevitable impurity;
(2) low alloy steel that step (1) obtains is processed into the size and dimension of needs, prepares low alloy steel mould;
(3) Surface Nanocrystalline is carried out to low alloy steel mould prepared by step (2).
Further,
The described method preparing low alloy steel of step (1) comprises the steps:
(11) cast is smelted: carry out electric arc furnace in turn and just refine, ladle RH process and LF process, control to pour into a mould after molten steel meets the chemical composition of restriction, wherein carry out Argon at least 5 minutes with the pressure of more than 3atm during ladle refining, remove with the floating being conducive to impurity;
(12) rolling: comprise equal thermal treatment, rolling and cooling, wherein all thermal treatment is soaking about 4 ~ 6 hours in the process furnace of 1100 ~ 1150 DEG C, the start rolling temperature of rolling is 950 ~ 1050 DEG C, finishing temperature is 840 ~ 880 DEG C, roll speed is 3 ~ 5m/s, and speed of cooling is 5 ~ 10 DEG C/s, cooled finishing temperature is 650 ~ 680 DEG C.
Surface Nanocrystalline described in step (3) comprises the steps:
(31) nanometer: the tungstenalloy cutter utilizing power to be 280-480W is to impact the surface of described low alloy steel mould with the frequency of 10-20KHZ; Impact energy produces the stress of 450-650MPA; Make strengthened by impact site thus realize nanometer, form nano-micrometre gradient-structure on surface;
(32) the low alloy steel mould of nanometer is put into crucible, be heated to 450 DEG C, add saline oxide 2 ~ 5kg beginning salt and melt to saline oxide; Again the gradation of base salt is added in crucible, add hot radical salt and all melt when rear salt bath face rises to distance crucible top edge 120mm and stop adding base salt, add adjustment salt 1 ~ 2kg, under 200 ~ 350 DEG C of conditions, run 2.5h;
(33) be oxidized: hang in oxidized still by clean rustless crucible, workpiece, at 220 DEG C, is put into crucible by instrument constant temperature, and thermopair is near sidewall of crucible; Then add in crucible by saline oxide, be added to 1/3 of crucible height, be then energized fusing; Add saline oxide gradually again after the salt that first time adds all melts, add suitable number at every turn, limit is melted, while add, until liquid level is elevated to distance crucible top edge 200mm; After salt bath face meets the requirements of height, 250 DEG C of insulations, make moisture volatilize in a large number, until liquid level no longer includes bubble produce complete calmness; 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 machinery oil and soak 1 ~ 2min, then oil droplet is done.
Preferably,
Adjust salt described in step (32) to be made up of the component of following weight parts: Na
2cO
320-30 part, K
2cO
320-30 part, NaCl 20-30 part, KCl 20-30 part, NH
4cl 10-20 part, Ce
2cO
32-4 part, BeO 2-4 part.
Described in step (32) and (33), saline oxide is selected from Na
2cO
3, K
2cO
3or the mixture of the two.
Described in step (32), base salt is selected from the mixture of potassium cyanate and metal oxide.
Preferred further, described in step (32), described in base salt, base salt comprises the component of following weight parts: potassium cyanate 80-100 part, Ce
2cO
31-3 part, ZrO
20.5-1.5 part, CeO
20.5-1.5 part.
In the present invention, the nano-micrometre gradient-structure of the nanometer process generation of step (31) can improve comprehensive military service performance and the military service behavior of metallic substance significantly.Metallic substance is after making Nano surface processing, show nanocrystalline between formed volume fraction be 100% interface be that Elements Diffusion provides desirable passage, can add the dynamic process of fast diffusion significantly, the nitriding treatment of the metal material surface made more easily carries out, obvious processing effect; Nanometer also can adopt other modes of this area routine to carry out, and disclosed in the patents such as such as ZL03111200.5 (gas-solid two-phase flow impacts metal material surface nano apparatus and application thereof), ZL200510029205.3 (the metal-surface nano method of ultrasonic wave high energy surface mechanical workout), method for making Nano is all applicable to the present invention.
Nanometer low-alloy heat-resistant high-strength steel mould thermotolerance of the present invention and solidity to corrosion are obtained for raising, decrease the kind of alloy simultaneously, and be that impurity component is simpler, easy to control, nitride effective codiffusional layer thickness also significantly increases.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Prepare the nanometer 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, surplus is Fe and inevitable impurity;
(11) cast is smelted: carry out electric arc furnace in turn and just refine, ladle RH process and LF process, control to pour into a mould after molten steel meets the chemical composition of restriction, wherein carry out Argon at least 5 minutes with the pressure of more than 3atm during ladle refining, remove with the floating being conducive to impurity;
(12) rolling: comprise equal thermal treatment, rolling and cooling, wherein all thermal treatment is soaking about 5 hours in the process furnace of 1150 DEG C, and the start rolling temperature of rolling is 1000 DEG C, finishing temperature is 850 DEG C, roll speed is 4m/s, and speed of cooling is 5 DEG C/s, cooled finishing temperature is 680 DEG C.
(2) low alloy steel that step (1) obtains is processed into the block low alloy steel mould of 40mm × 20mm × 3mm;
(3) Surface Nanocrystalline is carried out to low alloy steel mould prepared by step (2);
(31) nanometer: the tungstenalloy cutter utilizing power to be 480W is to impact the surface of described low alloy steel mould with the frequency of 10-20KHZ; Impact energy produces the stress of 500-650MPA; Make strengthened by impact site thus realize nanometer, form nano-micrometre gradient-structure on surface;
(32) the low alloy steel mould of nanometer is put into crucible, be heated to 450 DEG C, add saline oxide 3kg beginning salt and melt to saline oxide; Again the gradation of base salt is added in crucible, add hot radical salt and all melt when rear salt bath face rises to distance crucible top edge 120mm and stop adding base salt, add adjustment salt 2kg, under 220 DEG C of conditions, run 2.5h;
(33) be oxidized: hang in oxidized still by clean rustless crucible, workpiece, at 220 DEG C, is put into crucible by instrument constant temperature, and thermopair is near sidewall of crucible; Then add in crucible by saline oxide, be added to 1/3 of crucible height, be then energized fusing; Add saline oxide gradually again after the salt that first time adds all melts, add suitable number at every turn, limit is melted, while add, until liquid level is elevated to distance crucible top edge 200mm; After salt bath face meets the requirements of height, 250 DEG C of insulations, make moisture volatilize in a large number, until liquid level no longer includes bubble produce complete calmness; 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 in L-AN32# total loss system oil (product performs GB443-89 standard, purchased from Jinan You Run Chemical Co., Ltd.) and soak 2min, then oil droplet is done.
Adjust salt described in step (32) to be made up of the component of following weight parts: Na
2cO
330 parts, K
2cO
330 parts, NaCl 30 parts, KCl 25 parts, NH
4cl 15 parts, Ce
2cO
32 parts, BeO 2 parts.
Described in step (32) and (33), saline oxide is Na
2cO
350wt% and K
2cO
3the blend of 50wt%.
Described in step (32), described in base salt, base salt comprises the component of following weight parts: potassium cyanate 100 parts, Ce
2cO
33 parts, ZrO
21.5 parts, CeO
21.5 part.
The nitriding furnace of step (32) and step (33) and oxidized still equipment are the QPQ liquid salt bath composite nitride stove oxidized still that Cheng Long industrial furnace company limited of Foshan City produces, model is: SNYN-20-6, temperature rating is 650 DEG C, workspace is of a size of Φ 400mm × 550mm, it is by furnace shell, bell, heat insulation furnace lining, and heating unit, high temperature steel crucible, bell start (hydraulic pressure or manual), and the parts such as device form.
Embodiment 2
According to method described in embodiment 1, but described in step (32), base salt is the component of following weight parts: potassium cyanate 100 parts, Ce
2cO
33 parts, ZrO
23 parts.Obtain the nanometer low-alloy heat-resistant high-strength steel mould of embodiment 2.
Embodiment 3
According to method described in embodiment 1, but described in step (32), base salt is the component of following weight parts: potassium cyanate 100 parts, Ce
2cO
33 parts, CeO
23 parts.Obtain the nanometer low-alloy heat-resistant high-strength steel mould of embodiment 3.
Embodiment 4
According to method described in embodiment 1, but described in step (32), base salt is the component of following weight parts: potassium cyanate 100 parts, CeO
23 parts, ZrO
23 parts.Obtain the nanometer low-alloy heat-resistant high-strength steel mould of embodiment 4.
Comparative example
According to method described in embodiment 1, the Surface Nanocrystalline of step (3) in embodiment 1 is replaced with conventional quenching thermal treatment; Conventional quenching heat treating method is as follows:
After block low alloy steel mould step (2) prepared puts into carburizing treatment stove with vertical state, here vertical state refers to and keeps vertical being as the criterion with mould the longest three-dimensional one dimension as far as possible, be heated to 890 DEG C, and with the speed of 90 droplets/minute instillation methyl alcohol, flow simultaneously by controlling propane to maintain in stove carbon potential 0.85%, carry out diffusion carburizing treatment 2 hours, subsequently low alloy steel mould is pre-chilled to 760 DEG C reduce carbon potential to 0.7% in stove simultaneously and be incubated 10 minutes, then low alloy steel mould is taken out from cementing furnace and be direct quenching in the cooling oil of 125 DEG C in oil temperature, tempering is carried out again after quenching, tempering temperature is 170 DEG C, tempering time is 1.5 hours, obtain the low alloy steel mould of comparative example.
Test case
Carry out performance test to the low alloy steel mould that embodiment 1-4 and comparative example obtain, the measuring method of nitride effective codiffusional layer thickness and standard are see " GB/T 11354-2005 steel-iron components depth of penetration measures and microstructure examination ", and test result is in table 1.
The performance test table of table 1: embodiment 1-3 and comparative example
From table 1 result, the low alloy steel mould that embodiment of the present invention 1-3 obtains with comparative example 1 is compared, and room temperature Tensile strength is larger, and yield-point is higher, and surface hardness is larger.Especially embodiment 1, employs Ce
2cO
3, ZrO
2, CeO
2three kinds of oxide compounds are composite carries out modification to base salt, and effect is better, and owing to being provided with thicker nitride effective codiffusional layer, the low alloy steel mould using the inventive method to prepare has good solidity to corrosion.
The above; be only the specific embodiment of the present invention; but protection scope of the present invention is not limited thereto; any those of ordinary skill in the art are in the technical scope disclosed by the present invention; the change can expected without creative work or replacement, all should be encompassed within protection scope of the present invention.Therefore, the protection domain that protection scope of the present invention should limit with claims is as the criterion.
Claims (7)
1. a preparation method for nanometer 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, surplus is Fe and inevitable impurity;
(2) low alloy steel that step (1) obtains is processed into the size and dimension of needs, prepares low alloy steel mould;
(3) Surface Nanocrystalline is carried out to low alloy steel mould prepared by step (2).
2. the preparation method of nanometer low-alloy heat-resistant high-strength steel mould as claimed in claim 1: it is characterized in that: the described method preparing low alloy steel of step (1) comprises the steps:
(11) cast is smelted: carry out electric arc furnace in turn and just refine, ladle RH process and LF process, control to pour into a mould after molten steel meets the chemical composition of claim 1 restriction, the pressure wherein with more than 3atm during ladle refining carries out Argon at least 5 minutes, removes with the floating being conducive to impurity;
(12) rolling: comprise equal thermal treatment, rolling and cooling, wherein all thermal treatment is soaking about 4 ~ 6 hours in the process furnace of 1100 ~ 1150 DEG C, the start rolling temperature of rolling is 950 ~ 1050 DEG C, finishing temperature is 840 ~ 880 DEG C, roll speed is 3 ~ 5m/s, and speed of cooling is 5 ~ 10 DEG C/s, cooled finishing temperature is 650 ~ 680 DEG C.
3. the preparation method of nanometer low-alloy heat-resistant high-strength steel mould as claimed in claim 1, is characterized in that: the Surface Nanocrystalline described in step (3) comprises the steps:
(31) nanometer: the tungstenalloy cutter utilizing power to be 280-480W is to impact the surface of described low alloy steel mould with the frequency of 10-20KHZ; Impact energy produces the stress of 450-650MPA; Make strengthened by impact site thus realize nanometer, form nano-micrometre gradient-structure on surface;
(32) the low alloy steel mould of nanometer is put into crucible, be heated to 450 DEG C, add saline oxide 2 ~ 5kg beginning salt and melt to saline oxide; Again the gradation of base salt is added in crucible, add hot radical salt and all melt when rear salt bath face rises to distance crucible top edge 120mm and stop adding base salt, add adjustment salt 1 ~ 2kg, under 200 ~ 350 DEG C of conditions, run 2.5h;
(33) be oxidized: hang in oxidized still by clean rustless crucible, workpiece, at 220 DEG C, is put into crucible by instrument constant temperature, and thermopair is near sidewall of crucible; Then add in crucible by saline oxide, be added to 1/3 of crucible height, be then energized fusing; Add saline oxide gradually again after the salt that first time adds all melts, add suitable number at every turn, limit is melted, while add, until liquid level is elevated to distance crucible top edge 200mm; After salt bath face meets the requirements of height, 250 DEG C of insulations, make moisture volatilize in a large number, until liquid level no longer includes bubble produce complete calmness; 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 machinery oil and soak 1 ~ 2min, then oil droplet is done.
4. the preparation method of nanometer low-alloy heat-resistant high-strength steel mould as claimed in claim 3, is characterized in that: described in step (32), base salt is selected from the mixture of potassium cyanate and metal oxide.
5. the preparation method of nanometer low-alloy heat-resistant high-strength steel mould as claimed in claim 4, is characterized in that: described in step (32), described in base salt, base salt comprises the component of following weight parts: potassium cyanate 80-100 part, Ce
2cO
31-3 part, ZrO
20.5-1.5 part, CeO
20.5-1.5 part.
6. the preparation method of nanometer low-alloy heat-resistant high-strength steel mould as claimed in claim 3, is characterized in that: adjust salt described in step (32) and be made up of the component of following weight parts: Na
2cO
320-30 part, K
2cO
320-30 part, NaCl 20-30 part, KCl 20-30 part, NH
4cl 10-20 part, Ce
2cO
32-4 part, BeO 2-4 part.
7. the preparation method of nanometer low-alloy heat-resistant high-strength steel mould as claimed in claim 3, is characterized in that: described in step (32) and (33), saline oxide is selected from Na
2cO
3, K
2cO
3or the mixture of the two.
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| CN105803341A (en) * | 2016-04-20 | 2016-07-27 | 上海瀚氏模具成型有限公司 | Preparation method of nanocrystallized low alloy wear-resistant and corrosion-resistant steel mold |
| CN105803342A (en) * | 2016-04-20 | 2016-07-27 | 上海瀚氏模具成型有限公司 | Preparation method of surface-nanocrystallized low alloy steel mold |
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| 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 |
| CN109702442A (en) * | 2019-03-11 | 2019-05-03 | 精利模塑科技（无锡）有限公司 | A kind of production method of precision rapid shaping auto electronics mold |
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| CN105803341A (en) * | 2016-04-20 | 2016-07-27 | 上海瀚氏模具成型有限公司 | Preparation method of nanocrystallized low alloy wear-resistant and corrosion-resistant steel mold |
| CN105803342A (en) * | 2016-04-20 | 2016-07-27 | 上海瀚氏模具成型有限公司 | Preparation method of surface-nanocrystallized low alloy steel mold |
| 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 |
| CN109702442A (en) * | 2019-03-11 | 2019-05-03 | 精利模塑科技（无锡）有限公司 | A kind of production method of precision rapid shaping auto electronics mold |
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| CN104946994B (en) | 2017-01-25 |
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