CN104846327A - Environment-friendly nanocrystallizing compound deep modifying method for metal materials - Google Patents
Environment-friendly nanocrystallizing compound deep modifying method for metal materials Download PDFInfo
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- CN104846327A CN104846327A CN201510209352.2A CN201510209352A CN104846327A CN 104846327 A CN104846327 A CN 104846327A CN 201510209352 A CN201510209352 A CN 201510209352A CN 104846327 A CN104846327 A CN 104846327A
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Abstract
The invention relates to an environment-friendly nanocrystallizing compound deep modifying method for metal materials, in particular to a brand new composite surface strengthening and modifying technology for the metal materials. The environment-friendly nanocrystallizing compound deep modifying method includes the steps of (1) nanocrystallizing; (2) detergent degreasing; (3) nitriding; (4) oxidizing; (5) desalting by cold water; (6) drying. The environment-friendly nanocrystallizing compound deep modifying method has a deep modifying effect, can form a high-quality nanocrystallized infiltrated layer with a certain depth and certain hardness on the surface of a workpiece and is capable of improving performance of the workpiece.
Description
Technical field
The present invention relates to nanometer composite environmental-friendly deep layer method of modifying, particularly relate to a kind of metallic substance nanometer composite environmental-friendly deep layer method of modifying.
Background technology
Nanometer composite environmental-friendly deep layer modification technology is on the basis retaining original common Nitriding Technology, the compound degree of depth of plus nano chemical industry sequence, makes it to deepen to more than 40 μm by original 10-25 μm.Nanometer composite environmental-friendly deep layer modification technology comprises the salt bath of the compound layer degree of depth more than 40 μm or the nitriding of gas, or the oxidation operation of carbonitriding and salt bath subsequently or gas, and middle also have 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 increased exponentially, the wear resistance of infiltration layer also can be improved accordingly.Nanometer composite environmental-friendly deep layer modification technology may be used for than the larger load of common Nitriding Technology, more speed, part that abrasion loss is larger.The part of common nitriding treatment can not bear grinding, but the part of nanometer composite environmental-friendly deep layer modification technology process can bear grinding, and therefore nanometer composite environmental-friendly deep layer modification technology more may be used for high precision precision component.
Though existing common nitrogenize solidity to corrosion is fine, but if the intensification at double of the compound layer degree of depth, solidity to corrosion also can be improved accordingly, because corrosion proof raising is completely according to resistance to compound layer in Nitriding Technology.
Deepen the compound layer degree of depth and mainly nitriding temperature is brought up to more than 650 DEG C by 550 DEG C ~ 590 DEG C now.But it is a brand-new problem in Metallkunde field that nitriding temperature brings up to more than 650 DEG C, the temperature in usual iron and steel nitriding region is 550 DEG C ~ 650 DEG C, the temperature in carbonitriding region is more than 730 DEG C, and for a long time, 600 DEG C ~ 730 DEG C is the technological gap district of steel material surface process.Nanometer composite environmental-friendly deep layer modification technology has filled up this technological gap district domestic first.
Much all require high solidity to corrosion with relevant product abroad at present, common Nitriding Technology has been difficult to meet the demands.Such as the solidity to corrosion of a lot of concern-foreigner-product neutral salt spray test requires to reach more than 300h now, and this is that common Nitriding Technology is beyond one's reach, and adopts nanometer composite environmental-friendly deep layer modification technology can reach this index completely.
Nanometer composite environmental-friendly deep layer modification technology has application prospect widely, first be originally had a lot of product to want to adopt Nitriding Technology, but can not adopt because its infiltration layer is too thin, present nanometer composite environmental-friendly deep layer modification technology can broadened application scale in this respect; Next is the product of the common Nitriding Technology of existing employing, if adopt nanometer composite environmental-friendly deep layer modification technology can increase substantially the wear resistance of product, solidity to corrosion and fatigue strength, extend the work-ing life of product, therefore You compare great market in improving the quality of products.The compound layer of more than 35 μm can bear some accurate grinding, such nanometer composite environmental-friendly deep layer modification technology can expand have widely in the application aspect of a lot of high-precision product, very important purposes.In a word, the potential market of nanometer composite environmental-friendly deep layer modification technology is very huge.
Summary of the invention
The object of this invention is to provide and a kind ofly the object of this invention is to provide brand-new nanometer composite environmental-friendly deep layer method of modifying, it has deep layer modified effect, the high quality nanometer deep layer with enough degree of depth and certain degree of hardness is formed at workpiece surface, and can greatly improve its performance, meet the technical requirements of nitride metal, improve the surface property of nitrogenize workpiece further, thus reduce energy consumption, raise the efficiency and benefit, the hardness of metallic surface can be improved, intensity, impact property, wear resistance and erosion resistance, each side in work-ing life extending product all has significant effect, is widely applied to engineering machinery, agricultural machine, food machinery, plastics machinery, petroleum machinery, automobile, motorcycle, textile manufacturing machine, light industry machinery, instrument, boats and ships, lathe, gear, instrument, mould, five metals, light industry, pipelines and petrochemical pipelines, photographic camera, sewing machine, washing machine, shoes making machine, hydraulic part, sheet metal component, radar, firearms, etc. in industry, production efficiency can be increased substantially, improve the quality of products, simplification of flowsheet, shorten the production cycle, reduce production cost, increase social benefit.
In order to solve the problem existing for background technology, by the following technical solutions, nanometer composite environmental-friendly deep layer method of modifying, comprises the steps: (1) nanometer in the present invention; (2) clean-out system degreasing; (3) nitrogenize; (4) be oxidized; (5) cold wash is desalted; (6) dry.
Concrete,
(1) nanometer;
(2) clean-out system degreasing: workpiece is placed in the container containing metal cleaner, with cotton yarn by the greasy dirt of workpiece surface and account thing scrub, finally removes clean by the cotton yarn being bonded at workpiece surface;
(3) nitrogenize: workpiece is put into crucible, is heated to 450 ~ 750 DEG C, adds saline oxide 2 ~ 5kg beginning salt and melts 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 170mm and stop adding base salt, add adjustment salt 2 ~ 5kg, under 300 ~ 420 DEG C of conditions, run 3 ~ 4.5h;
(4) be oxidized: hang in oxidized still by clean rustless crucible, workpiece, at 230 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 250mm; 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 ~ 30 DEG C again ..., so circulate, until temperature is raised to 370 DEG C;
(5) cold wash is desalted: workpiece from oxidized still out after precooling in atmosphere, until the saline solution of workpiece surface all starts condensation, then workpiece sent in cold water clean;
(6) dry.
Step (1) described nanometer can adopt this area ordinary method to carry out, be a kind of that changed by electric energy, high frequency (frequency is 30-50KHz), high-energy-density, export constant, the intensity of activation of metallic substance plasticity and the recombination energy of striking energy can be increased.Nanometer processing comprises the following aspects: first, under the effect of elasticity pre-tension, the tool heads contact workpiece surface of nanometer cutting tool assembly; Secondly, workpiece metal material plasticity under the highdensity nanometer of macro-energy can act on improves; 3rd, tool heads impacts piece surface with the frequency of 3-5 per second ten thousand times; 4th, tool heads is processed part with certain machining locus (as: lathe turning track).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.
Preferably,
Step (3) nitrogenize is specially: first hang in nitriding furnace by the crucible through cleaning, rust cleaning, then workpiece is put into crucible, temperature control galvanic couple is inserted in crucible near sidewall of crucible, temperature control instrument fixes on 450 ~ 750 DEG C, then adds saline oxide 2 ~ 5kg beginning salt and melts to saline oxide; Again base salt is added in crucible, be added to 1/2 of the crucible degree of depth; Then bell is covered, start ventilation system, treat that the salt of crucible bottom starts to melt and after sinking, continue to add appropriate base salt, base salt bath face is made to remain at stable height, to the last all be fused into liquid, when salt bath face rises to distance crucible top edge 170mm, stop adding base salt; When cyanate radical massfraction lower than 31% time, add adjustment salt 2 ~ 5kg, to improve cyanate radical massfraction to 35%; Under 300 ~ 420 DEG C of conditions, run 3 ~ 4.5h, then come into operation.
Described in step (3), base salt is selected from Zassol, potassium cyanate or the mixture of the two, and described base salt can further include Na
2cO
3, K
2cO
3, NaCl, K
2sO
3, K
2one or more in S, urea, rare earth oxide; Preferred further, described base salt comprises the component of following weight parts: Zassol 80-100 part, Ce
2cO
32-4 part, ZrO
20.5-1.5 part, CeO
20.5-1.5 part.
Adjust salt described in step (3) 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.
The effect of step (3): 1) form the compound layer of the densification of enough degree of depth and the diffusion layer of respective depth at workpiece surface.Increase substantially metallic surface wear resistance, solidity to corrosion and fatigue performance; 2) base salt is for filling up the nitriding furnace crucible of initial period sky of going into operation, and supplements after normal production as salt bath consumption, is used for raising salt bath face; 3) adjusting salt is when in salt bath, cyanate radical declines, and adds in nitriding furnace the content being used for raising cyanate radical.
Step (3) and (4) described saline oxide are selected from Na
2cO
3, K
2cO
3or the mixture of the two.
The effect of step (4): 1) workpiece is thoroughly decomposed from the cyanogen root the nitridation salt that nitriding furnace brings out, eliminates public hazards; 2) form the oxide film of black at workpiece surface, increase the antirust ability of workpiece, and beautify the effect of workpiece outward appearance in addition; 3) compound layer can be made to be oxidized, increase the oxygen level in compound layer, make its passivation, increase substantially solidity to corrosion.
The effect of step (5): the temperature of workpiece is declined gradually and saline oxide workpiece surface in cold water dissolves.
Workpiece put into the hot water tank of 75 DEG C ~ 90 DEG C in drying described in step (6), insulation 10 ~ 15min, then cools in atmosphere, and workpiece is dry rapidly.Effect: ensure that workpiece is dry, and accelerate workpiece rate of drying, shortens the production cycle.Sticky floating saccharoid on the dry rear surface of workpiece is avoided to affect workpiece visual appearance.
Can also comprise step (7) immersion oil after step (6), the immersion oil described in step (7) is after workpiece drying, puts into machinery oil and soaks 3 ~ 5min, then done by oil droplet.Effect: after workpiece immersion oil, appearance luster is uniformity more.Workpiece is after immersion oil, and the surface of workpiece is covered to close by oil reservoir and becomes finer and close and have certain antirust ability.
Embodiment
Below in conjunction with embodiments of the invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.
Embodiment 1
(1) nanometer: first, under the effect of elasticity pre-tension, the tool heads contact workpiece surface of nanometer cutting tool assembly; Secondly, workpiece metal material plasticity under the highdensity nanometer of macro-energy can act on improves; 3rd, tool heads impacts piece surface with the frequency of 3-5 per second ten thousand times; 4th, tool heads is processed part with certain machining locus (as: lathe turning track);
(2) clean-out system degreasing: workpiece is placed in the container containing metal cleaner, with cotton yarn by the greasy dirt of workpiece surface and account thing scrub, finally removes clean by the cotton yarn being bonded at workpiece surface;
(3) nitrogenize: first hang in nitriding furnace by the crucible through cleaning, rust cleaning, then workpiece is put into crucible, inserted in crucible near sidewall of crucible by temperature control galvanic couple, temperature control instrument fixes on 650 DEG C, then adds saline oxide 2kg and starts intensificationization salt; Again base salt is added in crucible, be added to 1/2 of the crucible degree of depth; Then cover bell, start ventilation system, treat that the salt of crucible bottom starts to melt and after sinking, continue to add appropriate base salt, make base salt bath face remain at stable height, be to the last all fused into liquid, when salt bath face rises to distance crucible top edge 170mm, stop salt adding; When cyanate radical massfraction lower than 31% time, add adjustment salt 4.5kg, to improve cyanate radical content to 35%; After base salt all melts, under 400 DEG C of conditions, run 4.5h, then come into operation;
(4) be oxidized: hang in oxidized still by clean rustless crucible, workpiece, at 230 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 250mm; 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 ~ 30 DEG C again ..., so circulate, until temperature is raised to 370 DEG C;
(5) cold wash is desalted: workpiece from oxidized still out after precooling in atmosphere, until the saline solution of workpiece surface all starts condensation, then workpiece sent in cold water clean;
(6) dry; Workpiece is put into the hot water tank of 75 DEG C ~ 90 DEG C, insulation 10 ~ 15min, then cool in atmosphere, workpiece is dry rapidly;
(7) immersion oil: after workpiece drying, puts in L-AN32# total loss system oil (product performs GB443-89 standard, purchased from Jinan You Run Chemical Co., Ltd.) and soaks 3 ~ 5min, then done by oil droplet.
Wherein,
The workpiece used is of a size of the bar-shaped iron and steel parts of Φ 20mm × 100mm, and roughness is less than 0.6 μm.
The nitriding furnace of step (3) and step (4) 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.
Step (2) described metal cleaner is the FCC-JS03 Industrial Metal clean-out system that Jinghui Chemical Inst., Hefei produces.
Described in step (3), base salt comprises following component: Zassol 80kg, Ce
2cO
32kg, ZrO
21kg, CeO
21kg.
Adjust salt described in step (3) to be made up of following weight parts: Na
2cO
325 parts, K
2cO
325 parts, NaCl 20 parts, KCl 20 parts, NH
4cl 10 parts, Ce
2cO
32 parts, BeO 2 parts.
Described in step (3) and (4), saline oxide is Na
2cO
350wt% and K
2cO
3the blend of 50wt%.
Embodiment 2
According to the method described in embodiment 1, but described in step (3), base salt comprises following component: Zassol 80kg, Ce
2cO
32kg, ZrO
22kg.
Embodiment 3
According to the method described in embodiment 1, but described in step (3), base salt comprises following component: Zassol 80kg, Ce
2cO
32kg, CeO
22kg.
Embodiment 4
According to the method described in embodiment 1, but described in step (3), base salt comprises following component: Zassol 80kg, ZrO
22kg, CeO
22kg.
Test case
The workpiece performance implementing 1-4 acquisition is tested.
Workpiece surface after treatment has certain thickness nitride effective codiffusional layer, and nitride effective codiffusional layer is made up of with the compound layer being positioned at subsurface the zone of oxidation being positioned at most surface, and nitride effective codiffusional layer thickness sees the following form.Measuring method and standard are see " GB/T 11354-2005 steel-iron components depth of penetration measures and microstructure examination ".
| Nitride effective codiffusional layer thickness (μm) | |
| Embodiment 1 | 47 |
| Embodiment 2 | 43 |
| Embodiment 3 | 40 |
| Embodiment 4 | 41 |
As can be seen here, embodiment 1-4 has thicker nitride effective codiffusional layer, especially implements 1 and employs Ce
2cO
3, ZrO
2, CeO
2three kinds of rare earth oxides are composite carries out modification to base salt, and effect is better, owing to being provided with thicker nitride effective codiffusional layer, uses the workpiece after the inventive method process to have good solidity to corrosion.
Claims (9)
1. metallic substance nanometer composite environmental-friendly deep layer method of modifying, is characterized in that, comprises the steps: (1) nanometer; (2) clean-out system degreasing; (3) nitrogenize; (4) be oxidized; (5) cold wash is desalted; (6) dry.
2. metallic substance nanometer composite environmental-friendly deep layer method of modifying according to claim 1, it is characterized in that: step (3) nitrogenize is specially: workpiece is put into crucible, be heated to 450 ~ 750 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 170mm and stop adding base salt, add adjustment salt 2 ~ 5kg, under 300 ~ 420 DEG C of conditions, run 3 ~ 4.5h.
3. metallic substance nanometer composite environmental-friendly deep layer method of modifying according to claim 1, it is characterized in that: step (3) nitrogenize is specially: first the crucible through cleaning, rust cleaning is hung in nitriding furnace, then workpiece is put into crucible, temperature control galvanic couple is inserted in crucible near sidewall of crucible, temperature control instrument fixes on 450 ~ 750 DEG C, then adds saline oxide 2 ~ 5kg beginning salt and melts to saline oxide; Again base salt is added in crucible, be added to 1/2 of the crucible degree of depth; Then bell is covered, start ventilation system, treat that the salt of crucible bottom starts to melt and after sinking, continue to add appropriate base salt, base salt bath face is made to remain at stable height, to the last all be fused into liquid, when salt bath face rises to distance crucible top edge 170mm, stop adding base salt; When cyanate radical massfraction lower than 31% time, add adjustment salt 2 ~ 5kg, to improve cyanate radical massfraction to 35%; Under 300 ~ 420 DEG C of conditions, run 3 ~ 4.5h, then come into operation.
4. metallic substance nanometer composite environmental-friendly deep layer method of modifying according to claim 1, it is characterized in that: step (4) oxidation is specially: hang in oxidized still by clean rustless crucible, workpiece, at 230 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 250mm; 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 ~ 30 DEG C again, so circulates, until temperature is raised to 370 DEG C.
5. metallic substance nanometer composite environmental-friendly deep layer method of modifying according to claim 1, it is characterized in that: workpiece put into the hot water tank of 75 DEG C ~ 90 DEG C in the drying of step (6), insulation 10 ~ 15min, then cool in atmosphere, workpiece is dry rapidly.
6. metallic substance nanometer composite environmental-friendly deep layer method of modifying according to claim 1, it is characterized in that: after step (6), also comprise step (7) immersion oil, be workpiece is put into machinery oil to soak 3 ~ 5min, then oil droplet done.
7. the metallic substance nanometer composite environmental-friendly deep layer method of modifying according to Claims 2 or 3, is characterized in that: described in step (3), base salt is selected from Zassol, potassium cyanate or the mixture of the two.
8. metallic substance nanometer composite environmental-friendly deep layer method of modifying according to claim 7, is characterized in that: described base salt also comprises Na further
2cO
3, K
2cO
3, NaCl, K
2sO
3, K
2one or more in S, urea, rare earth oxide.
9. metallic substance nanometer composite environmental-friendly deep layer method of modifying according to claim 8, is characterized in that: described base salt comprises the component of following weight parts: Zassol 80-100 part, Ce
2cO
32-4 part, ZrO
20.5-1.5 part, CeO
20.5-1.5 part.
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Cited By (1)
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| CN111763907A (en) * | 2020-08-12 | 2020-10-13 | 北京天仁道和新材料有限公司 | Salt bath nitriding agent for metal workpiece surface treatment and metal workpiece surface treatment method |
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Application publication date: 20150819 |