CN102925851B - Two-section gas nitridation method for surfaces of aluminum and aluminum alloy - Google Patents
Two-section gas nitridation method for surfaces of aluminum and aluminum alloy Download PDFInfo
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- CN102925851B CN102925851B CN201210423467.8A CN201210423467A CN102925851B CN 102925851 B CN102925851 B CN 102925851B CN 201210423467 A CN201210423467 A CN 201210423467A CN 102925851 B CN102925851 B CN 102925851B
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Abstract
The invention relates to a two-section gas nitridation method for the surfaces of aluminum and aluminum alloy. The method comprises a surface oxidation film removing step and a surface nitridation treatment step. The step 1 comprises the following steps of: pre-treating; primarily galvanizing zinc; washing by water; removing zinc; secondarily galvanizing zinc; and drying after water washing. The step 2 comprises the following steps of: exhausting in a furnace, wherein the ammonia resolution ratio is less than 10%; primarily heating to 570-590 DEG C, wherein the ammonia resolution ratio is 15-25%; carrying out one-section nitridation, wherein the furnace temperature is 580-640DEG C, and the ammonia resolution ratio is kept at 15-25%; secondarily heating to 620-640 DEG C, wherein the ammonia resolution ratio is 40-55%; carrying out two-section nitridation, wherein the temperature is 620-640DEG C, and the ammonia resolution ratio is 40-55%; and denitriding, wherein the furnace temperature is 580-640DEG C, and the ammonia resolution ratio is controlled at 70-80%. The two-section gas nitridation method has the advantages that compact oxidation films on the surfaces of aluminum and the aluminum alloy can be effectively eliminated, the nitrogen atom can be preferably infiltrated, the nitridation treatment can be carried out by a common gas nitridation furnace, and the two-section gas nitridation method is low in production cost, simple and easy to operate, wide in adaptability, and good in infiltration layer quality.
Description
Technical field
The present invention relates to a kind of thermal treatment process of aluminium alloy, particularly relate to a kind of two sections, surface gas nitriding method of Al and Alalloy.
Background technology
Al and Alalloy is very extensive in the application of engineering structure and manufacture particularly automobile industry, because it is high that they have specific tenacity, proportion is little, under the prerequisite not reducing safety and stability, can alleviate the weight of engineering structure and machine, Al and Alalloy also has good machinability simultaneously.But along with the development of industrial technology, the hardness that Al and Alalloy is lower, lower wear resistance and solidity to corrosion make the requirement of the harsh service conditions such as its high between not competent component relative movement, high-quality stream and high corrosion.
Al and Alalloy surface strengthening means conventional at present have: anodic oxidation (hard anodizing, differential arc oxidation), laser and electron beam alloyage, ion sputtering, the methods such as plating hard chromium on surface and some Combined Processing.But the oxide film that anodic oxidation (hard anodizing) is formed easily produces thermal crack, reduces anticorrosion ability, between Al and Alalloy zone of oxidation, difference of hardness is comparatively large simultaneously, has ready conditions, there will be zone of oxidation obscission in heavily stressed load operation.And other enhancement methods are all costly, inadaptable batch production.
In recent years by carrying out nitriding treatment to Al and Alalloy, forming high hardness aluminium nitride layer on aluminium surface and improving the interest that the hardness of Aluminum-aluminum alloy and wear resistance have more and more caused people.
But because the chemical property of aluminium is very active, fine aluminium and aluminum alloy surface be the good natural oxide film of existence and stability all.Environmentally middle moisture content, the thickness of oxide film is the thickest reaches about 0.1 μm, seriously hinder nitrogen-atoms to the diffusion in aluminum substrate, this is also the difficult point that Al and Alalloy realizes surface carburization, so it is generally acknowledged that traditional nitridation process is difficult to realize nitriding on Al and Alalloy surface.
Main research at present and the Al and Alalloy nitridation process adopted are glow discharge plasma nitriding.
Conventional direct current glow discharge plasma nitriding process generally adopts bipolar DC system, workpiece is negative electrode, vacuum vessel is anode, volts DS is added between cathode and anode, gas glow discharge is made to produce plasma body, to cathode-workpiece accelerated motion under positive ion biased effect outside, collide with workpiece surface and infiltrate surface, completing the process of nitriding.
But this method usually needs to carry out pre-sputtering before nitriding to eliminate oxide film.Simultaneous temperature is higher, and what have even reaches 650 DEG C, cause aluminium alloy local melting and due to the resistance of AlN very high, when common direct current glow discharge nitriding, with thickening of AlN layer, it is sustain discharge process, must processing parameter be changed, thus add nitriding difficulty etc.
In order to obtain better nitriding result, a lot of research worker improves technique and device, successively propose and strengthen plasma ion nitriding, laser induced plasma nitriding, ECR(electron cyclotron resonance) microwave plasma nitriding, radio frequency (high frequency) plasma nitridation etc., but the common ground of the nitriding process of above-mentioned aluminium and aluminium alloy thereof is: equipment requirements and production cost is high, the difficult control of complicated operation, the nitride layer obtaining desired homogeneous is difficult to for large size and baroque workpiece.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art, provide a kind of nitride layer uniform, controllable, cost is low, and Al and Alalloy nitriding method simple for process.The two sections of gas nitriding method concrete steps in described Al and Alalloy surface are as follows:
1) surface film oxide is removed
A. pre-treatment clean Al and Alalloy workpiece;
B. first time soaks zinc, under room temperature environment, soak zinc, time 50 ~ 70s by carrying out first time in the described workpiece immersion zinc dipping solution of cleaning;
C. wash, with the described workpiece of water cleaning after first time leaching zinc;
D. move back zinc, the described workpiece after washing is at room temperature immersed nitric acid HNO
3zinc is moved back in the aqueous solution;
E. second time soaks zinc, under room temperature environment, soak zinc, time 25 ~ 35s by carrying out second time in the described workpiece immersion zinc dipping solution through moving back zinc;
F. washing dries up, and cleans the described workpiece after second time leaching zinc and dry up or dry with water;
2) surfaces nitrided
A. be vented: the described workpiece through above-mentioned removal surface film oxide is placed in after in nitriding furnace, starts to pass into ammonia to get rid of furnace air, until ammonia dissociation rate is less than 10%;
B. first time heats up: make furnace temperature rise to 570 ~ 590 DEG C, in temperature-rise period, reduce ammonia flow gradually, until ammonia dissociation rate reaches 30 ~ 45%;
C. first paragraph nitriding: keep furnace temperature 570 ~ 590 DEG C, 5 ~ 20 hours, this process keeps ammonia dissociation rate 15 ~ 25%;
D. second time heats up, and after single-stage nitriding completes, makes furnace temperature rise to 620 ~ 640 DEG C, reduces ammonia flow simultaneously, make the ammonia dissociation rate at this temperature reach 40 ~ 55%;
E. second segment nitriding: keep furnace temperature 620 ~ 640 DEG C, 5 ~ 30 hours, this process keeps ammonia dissociation rate 40 ~ 55%;
F. move back nitrogen, keep furnace temperature 620 ~ 640 DEG C, reduce ammonia flow, cause ammonia dissociation rate to 70 ~ 80%, this state keeps 1 ~ 2 hour.
Described zinc dipping solution is the proportion relation gained solution by 1 liter of water following masses compound:
Zinc oxide ZnO 10 ~ 30 g,
Sodium hydroxide NaOH 50 ~ 70g,
Seignette salt KNaC
4h
4o
650 ~ 90g.
Zinc process of moving back nitric acid HNO used in described removal surface film oxide step
3the aqueous solution is water and the nitric acid HNO of 1: 0.8 ~ 1: 1.1 volumetric ratios
3mixing solutions, the described workpiece time of immersing in this solution is 6 ~ 12s.
Pre-treatment in described removal surface film oxide step cleaning workpiece surface comprise carry out successively electrochemical deoiling, hot water wash, cold wash, acid etch and washing step by step.
In described surfaces nitrided steps of exhausting, be placed in after in nitriding furnace at described workpiece, stove heated up, starts to pass into ammonia when furnace temperature rises to 300 DEG C.
Above-mentioned technical solution of the present invention produces following beneficial effect:
1) after the process of leaching zinc, can effectively eliminate Al and Alalloy surface compact oxide film and stop it to be formed once again, being conducive to the infiltration of nitrogen-atoms;
2) gas carbruizing furance adopting ordinary gas nitridation stove maybe can carry out Nitrizing Treatment just can realize Al and Alalloy nitriding, and nitriding equipment requirements is not high, and production cost is low, and operation is simple;
3) wide adaptability, can process the workpiece of different shape and size;
4) quality layer is good, and workpiece all surface can obtain the uniform aluminum nitride compound layer of thickness.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Following embodiment is all carried out at RQ3-35-9 gas carbruizing furance.
Embodiment 1
Workpiece material is 1050 fine aluminiums, and its chemical composition is aluminium Al 99.50%, Si0.25%, Cu0.05%, Mg0.05%, separately has minute quantity Zn, Mn etc.First the process of removal surface film oxide is carried out to this fine aluminium workpiece, is specifically completed by following step:
1) pre-treatment, carries out electrochemical deoiling, hot water wash, cold wash, acid etch and washing successively to fine aluminium workpiece surface, and wherein electrochemical deoiling, acid etch process according to existing general industry surface of pure aluminum treatment process, repeat no more.
2) first time soaks zinc, first prepares zinc dipping solution, prepares by the proportion relation of 1 liter of water following masses compound:
Zinc oxide ZnO 10 g,
Sodium hydroxide NaOH 50g,
Seignette salt KNaC
4h
4o
650g,
Under room temperature environment, the above-mentioned workpiece through cleaning immerses and carries out first time in the zinc dipping solution prepared and soak zinc, immersion time 50s by (5 ~ 35 DEG C, following identical).
3) wash, with the described workpiece of water cleaning after first time leaching zinc.
4) move back zinc, first prepare dezincifying solution, by water and nitric acid HNO
3volumetric ratio 1:1 prepare, immersed in dezincifying solution by above-mentioned workpiece after washing, carry out moving back zinc, temperature is room temperature, and the immersion time is 6s.
5) second time soaks zinc, under room temperature environment, soak zinc, time 25s by carrying out second time in the workpiece immersion zinc dipping solution through moving back zinc; Second time zinc dipping solution is identical with first time zinc dipping solution, and the present embodiment shares same groove solution.
6) washing dries up, and cleans the workpiece after second time leaching zinc and dry up with water.
Make the zone of oxidation of workpiece surface densification be removed after above-mentioned steps completes, obtain the very thin zinc tectum of one deck on aluminum metal surface, produce to prevent the oxide film of aluminium.Then nitriding treatment is carried out to workpiece surface, is specifically completed by following step:
1) be vented: first open bell, bell is built by being placed in after in described nitriding furnace through the workpiece of above-mentioned removal surface film oxide, stove is heated up, start to pass into ammonia when furnace temperature rises to 300 DEG C, be used for getting rid of oxygen in stove by the oxygen in ammonia and furnace air, furnace air is got rid of situation and is obtained by monitoring ammonia dissociation rate, and the fewer ammonia dissociation rate of furnace air is less, otherwise ammonia dissociation rate is larger.The ammonia dissociation rate of the present embodiment controls below 10%, controls to realize by controlling ammonia flow to ammonia dissociation rate.
2) first time heats up: make furnace temperature rise to 570 DEG C, reduce ammonia flow gradually, control ammonia dissociation rate 15% in temperature-rise period.
3) first paragraph nitriding: keep furnace temperature 570 DEG C, 5 hours, this process keeps ammonia dissociation rate 15%.
4) second time heats up: after single-stage nitriding completes, make furnace temperature rise to 620 DEG C, reduce ammonia flow simultaneously, make the ammonia dissociation rate at this temperature reach 40%;
5) second segment nitriding: keep furnace temperature 620 DEG C, 5 hours, this process keeps ammonia dissociation rate 40%;
6) move back nitrogen, keep furnace temperature 620 DEG C, reduce ammonia flow, cause ammonia dissociation rate to 70%, this state keeps 1 hour.
Above-mentioned steps makes the surfaces nitrided process of workpiece complete, turn off furnace power, make workpiece furnace cooling, furnace pressure should be kept in the process to be malleation, when furnace reduces to 150 DEG C, open fire door and take out workpiece, recording depth of penetration is 8 μm, and workpiece surface microhardness is 64.5HV0.1.
Embodiment 2
Workpiece material is 5050 aluminium alloys, and its chemical composition and content (wt%) are: Si0.4, Fe0.7, Cu0.2, Mn1.1, Mg1.4, Zn0.25, other 0.15, surplus is aluminium.First the process of removal surface film oxide is carried out to this Al alloy parts, is specifically completed by following step:
1) pre-treatment, carries out electrochemical deoiling, hot water wash, cold wash, acid etch and washing successively to Al alloy parts surface, and wherein electrochemical deoiling, acid etch process according to existing general industry surface of pure aluminum treatment process, repeat no more.
2) first time soaks zinc, first prepares zinc dipping solution, prepares by the proportion relation of 1 liter of water following masses compound:
Zinc oxide ZnO 20 g,
Sodium hydroxide NaOH 60g,
Seignette salt KNaC
4h
4o
670g,
Under room temperature environment, the above-mentioned workpiece through cleaning is immersed and carry out first time in the zinc dipping solution prepared and soak zinc, immersion time 60s.
3) wash, with the described workpiece of water cleaning after first time leaching zinc.
4) move back zinc, first prepare dezincifying solution, by water and nitric acid HNO
3volumetric ratio 1:1.1 prepare, immersed in dezincifying solution by above-mentioned workpiece after washing, carry out moving back zinc, temperature is room temperature, and the immersion time is 10s.
5) second time soaks zinc, under room temperature environment, soak zinc, time 30s by carrying out second time in the workpiece immersion zinc dipping solution through moving back zinc; Second time zinc dipping solution is identical with first time zinc dipping solution, and the present embodiment shares same groove solution.
6) washing dries up, and cleans the workpiece after second time leaching zinc and dry with water.
Make the zone of oxidation of workpiece surface densification be removed after above-mentioned steps completes, obtain the very thin zinc tectum of one deck on aluminum metal surface, produce to prevent the oxide film of aluminium.Then surface is carried out to workpiece and carries out nitriding treatment, specifically completed by following step:
1) be vented: first open bell, bell is built by being placed in after in described nitriding furnace through the workpiece of above-mentioned removal surface film oxide, stove is heated up, start to pass into ammonia when furnace temperature rises to 300 DEG C, be used for getting rid of oxygen in stove by the oxygen in ammonia and furnace air, furnace air is got rid of situation and is obtained by monitoring ammonia dissociation rate, and the fewer ammonia dissociation rate of furnace air is less, otherwise ammonia dissociation rate is larger.The ammonia dissociation rate of the present embodiment controls below 10%, controls to realize by controlling ammonia flow to ammonia dissociation rate.
2) first time heats up: make furnace temperature rise to 575 DEG C, reduce ammonia flow gradually, control ammonia dissociation rate 20% in temperature-rise period.
3) first paragraph nitriding: keep furnace temperature 575 DEG C, 10 hours, this process keeps ammonia dissociation rate 20%.
4) second time heats up: after single-stage nitriding completes, make furnace temperature rise to 630 DEG C, reduce ammonia flow simultaneously, make the ammonia dissociation rate at this temperature reach 50%;
5) second segment nitriding: keep furnace temperature 630 DEG C, 15 hours, this process keeps ammonia dissociation rate 50%;
6) move back nitrogen, keep furnace temperature 630 DEG C, reduce ammonia flow, cause ammonia dissociation rate to 75%, this state keeps 1.5 hours.
Above-mentioned steps makes the surfaces nitrided process of workpiece complete, and turns off furnace power, workpiece furnace cooling, furnace pressure should be kept in the process to be malleation, when furnace reduces to 170 DEG C, to open fire door and take out workpiece, recording depth of penetration is 25 μm, and workpiece surface microhardness is 238HV0.1.
Embodiment 3
Workpiece material is 2A12 aluminium alloy, and its chemical composition and content (wt%) are: Cu4.3, Mg1.6, Mn0.6, Si0.4, surplus are aluminium.First the process of removal surface film oxide is carried out to this Al alloy parts, is specifically completed by following step:
1) pre-treatment, carries out electrochemical deoiling, hot water wash, cold wash, acid etch and washing successively to Al alloy parts surface, and wherein electrochemical deoiling, acid etch process according to existing general industry surface of pure aluminum treatment process, repeat no more.
2) first time soaks zinc, first prepares zinc dipping solution, prepares by the proportion relation of 1 liter of water following masses compound:
Zinc oxide ZnO 30 g,
Sodium hydroxide NaOH 70g,
Seignette salt KNaC
4h
4o
690g,
Under room temperature environment, the above-mentioned workpiece through cleaning is immersed and carry out first time in the zinc dipping solution prepared and soak zinc, immersion time 70s.
3) wash, with the described workpiece of water cleaning after first time leaching zinc.
4) move back zinc, first prepare dezincifying solution, by water and nitric acid HNO
3volumetric ratio 1:0.8 prepare, immersed in dezincifying solution by above-mentioned workpiece after washing, carry out moving back zinc, temperature is room temperature, and the immersion time is 12s.
5) second time soaks zinc, under room temperature environment, soak zinc, time 35s by carrying out second time in the workpiece immersion zinc dipping solution through moving back zinc; Second time zinc dipping solution is identical with first time zinc dipping solution, and the present embodiment shares same groove solution.
6) washing dries up, and cleans the workpiece after second time leaching zinc and dry up with water.
Make the zone of oxidation of workpiece surface densification be removed after above-mentioned steps completes, obtain the very thin zinc tectum of one deck on aluminum metal surface, produce to prevent the oxide film of aluminium.Then surface is carried out to workpiece and carries out nitriding treatment, specifically completed by following step:
1) be vented: first open bell, bell is built by being placed in after in described nitriding furnace through the workpiece of above-mentioned removal surface film oxide, stove is heated up, start to pass into ammonia when furnace temperature rises to 300 DEG C, be used for getting rid of oxygen in stove by the oxygen in ammonia and furnace air, furnace air is got rid of situation and is obtained by monitoring ammonia dissociation rate, and the fewer ammonia dissociation rate of furnace air is less, otherwise ammonia dissociation rate is larger.The ammonia dissociation rate of the present embodiment controls below 10%, controls to realize by controlling ammonia flow to ammonia dissociation rate.
2) first time heats up: make furnace temperature rise to 590 DEG C, reduce ammonia flow gradually, control ammonia dissociation rate 25% in temperature-rise period.
3) first paragraph nitriding: keep furnace temperature 590 DEG C, 20 hours, this process keeps ammonia dissociation rate 25%.
4) second time heats up: after single-stage nitriding completes, make furnace temperature rise to 640 DEG C, reduce ammonia flow simultaneously, make the ammonia dissociation rate at this temperature reach 50%;
5) second segment nitriding: keep furnace temperature 640 DEG C, 30 hours, this process keeps ammonia dissociation rate 55%;
4) move back nitrogen, keep furnace temperature 640 DEG C, reduce ammonia flow, cause ammonia dissociation rate to 80%, this state keeps 2 hours.
Above-mentioned steps makes the surfaces nitrided process of workpiece complete, turn off furnace power, make workpiece furnace cooling, furnace pressure should be kept in the process to be malleation, when furnace reduces to 150 DEG C, open fire door and take out workpiece, recording depth of penetration is 35 μm, and workpiece surface microhardness is 337HV0.1.
The present invention is never confined to above-described embodiment, may be combined with out more embodiment again according to technical scheme of the present invention in conjunction with state of the art means, these all fall into the present invention want the scope of resist technology scheme.In addition the present invention's cementing furnace used is also not limited to the RQ3-35-9 gas carbruizing furance described in above-described embodiment, and other types of gases nitriding furnace or gas carbruizing furance can be implemented by the described step of above-described embodiment and processing condition equally.
Claims (5)
1. the two sections of gas nitriding methods in Al and Alalloy surface, comprise the steps:
1) surface film oxide is removed
A. pre-treatment clean Al and Alalloy workpiece;
B. first time soaks zinc, under room temperature environment, soak zinc, time 50 ~ 70s by carrying out first time in the described workpiece immersion zinc dipping solution of cleaning;
C. wash, with the described workpiece of water cleaning after first time leaching zinc;
D. move back zinc, the described workpiece after washing is at room temperature immersed nitric acid HNO
3zinc is moved back in the aqueous solution;
E. second time soaks zinc, under room temperature environment, soak zinc, time 25 ~ 35s by carrying out second time in the described workpiece immersion zinc dipping solution through moving back zinc;
F. washing dries up, and cleans the described workpiece after second time leaching zinc and dry up or dry with water;
2) surfaces nitrided
A. be vented: the described workpiece through above-mentioned removal surface film oxide is placed in after in nitriding furnace, starts to pass into ammonia to get rid of furnace air, until ammonia dissociation rate is less than 10%;
B. first time heats up: make furnace temperature rise to 570 ~ 590 DEG C, in temperature-rise period, reduce ammonia flow gradually, until ammonia dissociation rate reaches 30 ~ 45%;
C. first paragraph nitriding: keep furnace temperature 570 ~ 590 DEG C, 5 ~ 20 hours, this process keeps ammonia dissociation rate 15 ~ 25%;
D. second time heats up, and after single-stage nitriding completes, makes furnace temperature rise to 620 ~ 640 DEG C, reduces ammonia flow simultaneously, make the ammonia dissociation rate at this temperature reach 40 ~ 55%;
E. second segment nitriding: keep furnace temperature 620 ~ 640 DEG C, 5 ~ 30 hours, this process keeps ammonia dissociation rate 40 ~ 55%;
F. move back nitrogen, keep furnace temperature 620 ~ 640 DEG C, reduce ammonia flow, cause ammonia dissociation rate to 70 ~ 80%, this state keeps 1 ~ 2 hour.
2. the two sections of gas nitriding methods in Al and Alalloy surface according to claim 1, is characterized in that described zinc dipping solution is the proportion relation gained solution by 1 liter of water following masses compound:
Zinc oxide ZnO 10 ~ 30 g,
Sodium hydroxide NaOH 50 ~ 70g,
Seignette salt KNaC
4h
4o
650 ~ 90g.
3. the two sections of gas nitriding methods in Al and Alalloy surface according to claim 1, is characterized in that zinc process of the moving back nitric acid HNO used in described removal surface film oxide step
3the aqueous solution is water and the nitric acid HNO of 1: 0.8 ~ 1: 1.1 volumetric ratios
3mixing solutions, the described workpiece time of immersing in this solution is 6 ~ 12s.
4. the two sections of gas nitriding methods in Al and Alalloy according to claim 1 surface, the preprocessing process that it is characterized in that in described removal surface film oxide step comprise carry out successively electrochemical deoiling, hot water wash, cold wash, acid etch and washing step by step.
5. the two sections of gas nitriding methods in Al and Alalloy surface according to claim 1, is characterized in that, in described surfaces nitrided steps of exhausting, being placed in after in nitriding furnace at described workpiece, are heated up by stove, start to pass into ammonia when furnace temperature rises to 300 DEG C.
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CN105887000A (en) * | 2016-06-08 | 2016-08-24 | 连云港江南精工机械有限公司 | Nitriding heat treatment method of die-casting machine accessory |
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CN110423977B (en) * | 2019-09-05 | 2021-06-18 | 合肥工业大学 | Gas nitriding method for aluminum material by taking chemical iron-immersion plating as pretreatment |
CN114875353B (en) * | 2022-04-27 | 2024-03-19 | 宁波同创强磁材料有限公司 | Preparation method of high-corrosion-resistance sintered NdFeB magnet |
CN115505865B (en) * | 2022-09-26 | 2024-01-23 | 沈阳飞机工业(集团)有限公司 | Hook-type part local nitriding heat treatment clamp and method thereof |
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