CN101058875A - Diffusion prevention method for inorganic fused salt on magnesium alloy surface - Google Patents
Diffusion prevention method for inorganic fused salt on magnesium alloy surface Download PDFInfo
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Abstract
The invention discloses a dispersing protective method of inorganic fused salt on the magnesium alloy surface in the antiseptic technical domain of metal surface, which comprises the following steps: cleaning the surface of magnesium alloy; placing the alloy into inorganic fusing salt; selecting AlCl3-NaCl or AlCl3-NaCl-KCl as the inorganic fusing salt system; proceeding induction heating for the inorganic fusing salt system; forming metal compound on the surface of magnesium alloy; connecting magneium-aluminium metal compound and magnesium alloy base without generating surface cracking or stripping easily.
Description
Technical field
What the present invention relates to is the method in aseptic technic field, a kind of metallic surface, particularly a kind of diffusion prevention method for inorganic fused salt on magnesium alloy surface.
Background technology
Though magnesium alloy has the performance of many excellences, active because of its chemical property, be vulnerable to corrode, its subcarbonate film that natural passivation forms in air is thin and loose, and erosion resistance is very poor, has limited the further application of magnesium and alloy thereof.Therefore magnesium alloy must adopt reliable surfacecti proteon measure as structured material.At present, the method for magnesium alloy surface protective mainly contains chemical conversion coating, anode oxidation membrane, surface metal plating layer (electroless plating, plating etc.), diffusion coating, laser surface modification, vapor deposition layer, organism coating etc.Chemical conversion is handled and is mainly contained chromate treating, stannate processing and bonderizing etc., it faces the pressure of environmental protection on the one hand, anti-corrosion and the crocking resistance of gained rete is all not enough so that it uses separately under mal-condition on the other hand, generally is used as the pre-treatment of organic coating.Anode oxidation membrane is very crisp, and is non-conductive, and therefore, being not suitable for load maybe needs the application scenario of conducting electricity.The metal plating of magnesium alloy has some to use, but because of the activity of magnesium makes Mg alloy surface plating or electroless plating all compare difficulty, and have problems such as environmental pollution, corrosion resistance nature are not high.Laser surface modification, vapour deposition cost are higher, and solidity to corrosion improves few.Organic coating matter is soft and easily peel off, and barrier propterty is general.From many aspects, aluminium all is the ideal coated material, and the electrical and thermal conductivity performance and the mechanical property of aluminium are fine, and aluminium is because of the oxidation film layer of its surface oxidation generation one deck densification, so its barrier propterty is very excellent.And aluminum coating can carry out various aftertreatment to satisfy such as corrosion-resistant, decoration, performance demands such as wear-resistant.The aluminum coating technology of comparative maturity has hot dipping aluminising, spraying, physical vapor deposition, plating.Preceding several method needs to carry out under the comparatively high temps, can the structure property of magnesium alloy be exerted an influence, and the Electroplating Aluminum method is implemented relatively difficulty at Mg alloy surface, because the very active MgO of magnesium alloy can form rapidly at alloy surface, hinders metal refining and basic unit to form the metal-metal key.Though the technical study of fused salt aluminum diffusing is started late, very fast relatively in some developed country's development, China's research report in this respect is considerably less.The fused salt of fused salt aluminum diffusing comprises two classes: inorganic fused salt and organic molten salt.The fused salt aluminum diffusing begins one's study from inorganic fused salt.And existing fused salt aluminum diffusing all adopts is electroplating technology, and the common inorganic fused salt system of having studied has AlCl
3-NaCl and AlCl
3-NaCl-KCl system.The base material of fused salt aluminum diffusing mainly contains copper, nickel and iron and steel etc. at present, yet there are no report in Mg alloy surface fused salt aluminum diffusing, because the fused salt aluminum diffusing can be carried out in the melt temperature scope of molten salt system, so as long as the melt temperature of molten salt system is not high, the performance of magnesium alloy burning or material is changed, thereby be fully feasible in Mg alloy surface fused salt aluminum diffusing.
Through retrieval invention to the prior art document, Ma Youping has delivered " solid-state expansion zincizing is handled pure magnesium surface tissue and Effect on Performance " (" non-ferrous metal " by name, 2005,57 (2): introduce 29-31): solid-state diffusion has formed the Mg-Zn layer at pure magnesium surface, and the formation of this alloy layer has also improved the hardness and the solidity to corrosion of pure magnesium surface.But this method preparation temperature height easily causes the distortion and the changes in microstructure of low-melting magnesium and magnesium alloy component, and diffusion layer is thin, and plating defect causes the protection function forfeiture.Based on this, also just arisen at the historic moment in Mg alloy surface fused salt aluminum diffusing method.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of diffusion prevention method for inorganic fused salt on magnesium alloy surface is provided, thereby improve the etch-proof ability of Mg alloy surface.By in Mg alloy surface fused salt aluminum diffusing, utilize the deposition of aluminium at Mg alloy surface, form magnalium intermetallic compound with magnesium alloy with efficient corrosion resisting performance, formed the etch-proof protection barrier of one deck at Mg alloy surface.By this method, the cost that Mg alloy surface is handled is reduced, barrier propterty obtains big raising, and finally promotes magnesium alloy being extensive use of in multi-field.
The present invention realizes by following scheme, the present invention with the Mg alloy surface clean after, put into the inorganic fused salt system, the inorganic fused salt system is selected AlCl for use
3-NaCl or AlCl
3-NaCl-KCl inorganic fused salt carries out induction heating to the inorganic fused salt system, forms intermetallic compound at Mg alloy surface.
Described inorganic fused salt system is AlCl
3During-NaCl, AlCl
3With NaCl molar fraction ratio be 2: 3～4: 1, the fused salt diffusion temperature is 230 ℃～320 ℃, soaking time is 5 hours～8 hours;
Described inorganic fused salt system is AlCl
3During-NaCl-KCl, AlCl
3Molar fraction accounts for 60%～75%, and the NaCl molar fraction accounts for 20%-30%, and KCl accounts for molar fraction 10%～15%, and the fused salt diffusion temperature is 230 ℃～280 ℃, and soaking time is 6 hours～8 hours.
Described inorganic fused salt system is AlCl
3During-NaCl, carry out according to the following step:
1) Mg alloy surface is carried out mechanical scrubbing (sandblast, sand papering), remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl
3Prepare AlCl in proportion with anhydrous NaCl
3The inorganic fused salt mixt of-NaCl is in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with sample with same mixing salt rapidly then, cover crucible cover;
4) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, heating, and soaking time is 5 hours～8 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
In the step 4), described heating, its temperature is 270 ℃～320 ℃.
In the step 4), described heating, preferred 270 ℃～300 ℃ of its temperature.
Described inorganic fused salt system is AlCl
3During-NaCl-KCl, carry out according to the following step:
1) Mg alloy surface is carried out mechanical scrubbing (sandblast, sand papering), remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl
3, anhydrous NaCl and anhydrous K Cl prepare AlCl in proportion
3The inorganic fused salt mixt of-NaCl-KCl is in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with the magnesium alloy block with same mixing salt rapidly then, cover crucible;
4) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, and Heating temperature generally is controlled at 230 ℃～280 ℃, and soaking time is 6 hours～8 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
The present invention utilizes the deposition of aluminium at Mg alloy surface by in Mg alloy surface fused salt aluminum diffusing, forms the magnalium intermetallic compound with efficient corrosion resisting performance with magnesium alloy, has formed the etch-proof protection barrier of one deck at Mg alloy surface.By this method, the cost that Mg alloy surface is handled is reduced, barrier propterty obtains big raising, promotes magnesium alloy being extensive use of in multi-field.This method is owing to select AlCl for use
3-NaCl or AlCl
3-NaCl-KCl is as the inorganic fused salt system, and unharmful substance is discharged in concrete operations, environmentally safe, and can under lower temperature, carry out, not only can reduce energy consumption, reduce production costs, and can not influence the mechanical property of body material, significant to Application of Magnesium.
Embodiment
Below embodiments of the invention are elaborated: present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
Material is extruding attitude AZ91D magnesium alloy, and the concrete operations step is:
1) Mg alloy surface is carried out mechanical scrubbing (as sandblast, sand papering), remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl
3With anhydrous NaCl example preparation in 2: 3 in molar ratio 500g AlCl
3The inorganic fused salt mixt of-NaCl is in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with sample with same mixing salt rapidly then, cover crucible cover;
4) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, and Heating temperature generally is controlled at 230 ℃, and soaking time is 5 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
Through soak test and polarization curve solidity to corrosion test shows: compare with undressed magnesium alloy, the corrosion stability of magnesium alloy after present embodiment is handled with this scheme improves nearly two orders of magnitude.
Embodiment 2:
Material is extruding attitude AZ91D magnesium alloy, and the concrete operations step is:
1) Mg alloy surface is carried out mechanical scrubbing (as sandblast, sand papering), remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl3 and the anhydrous NaCl inorganic fused salt mixt of example preparation in 4: 1 500g AlCl3-NaCl in molar ratio, in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with sample with same mixing salt rapidly then, cover crucible cover;
4) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, and Heating temperature generally is controlled at 320 ℃, and soaking time is 8 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
Through soak test and polarization curve solidity to corrosion test shows: compare with undressed magnesium alloy, the corrosion stability of magnesium alloy after present embodiment is handled with this scheme improves nearly two orders of magnitude.
Embodiment 3:
Material is pure magnesium, and the concrete operations step is:
1) Mg alloy surface is carried out mechanical scrubbing (as sandblast, sand papering), remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl
3With anhydrous NaCl example preparation in 1: 1 in molar ratio 500g AlCl
3The inorganic fused salt mixt of-NaCl is in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with sample with same mixing salt rapidly then, cover crucible cover;
4) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, and Heating temperature generally is controlled at 300 ℃, and soaking time is 6 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
Through soak test and polarization curve solidity to corrosion test shows: compare with undressed magnesium alloy, the corrosion stability of magnesium alloy after present embodiment is handled with this scheme improves nearly two orders of magnitude.
Embodiment 4:
Material is extruding attitude AZ91D magnesium alloy, and the concrete operations step is:
1) Mg alloy surface is carried out mechanical scrubbing (as sandblast, sand papering), remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl
3, anhydrous NaCl and anhydrous K Cl ratio preparation in 6: 3: 1 in molar ratio 500gAlCl
3The inorganic fused salt mixt of-NaCl-KCl is in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with sample with same mixing salt rapidly then, cover crucible cover;
4) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, and Heating temperature generally is controlled at 250 ℃, and soaking time is 7 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
Through soak test and polarization curve solidity to corrosion test shows: compare with undressed magnesium alloy, the corrosion stability of magnesium alloy after present embodiment is handled with this scheme improves nearly two orders of magnitude.
Embodiment 5:
Material is extruding attitude ZM5 magnesium alloy, and the concrete operations step is:
Mg alloy surface is carried out mechanical scrubbing (as sandblast, sand papering), remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
Choose anhydrous AlCl3, anhydrous NaCl and anhydrous K Cl ratio preparation in 15: 4: 3 in molar ratio 500gAlCl
3The inorganic fused salt mixt of-NaCl-KCl is in the exsiccant ceramic crucible of packing into;
1) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with sample with same mixing salt rapidly then, cover crucible cover;
2) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, and Heating temperature generally is controlled at 230 ℃, and soaking time is 8 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
3) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
Through soak test and polarization curve solidity to corrosion test shows: compare with undressed magnesium alloy, the corrosion stability of magnesium alloy after present embodiment is handled with this scheme improves nearly two orders of magnitude.
Embodiment 6:
Material is pure magnesium, and the concrete operations step is:
1) Mg alloy surface is carried out mechanical scrubbing (as sandblast, sand papering), remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl
3, anhydrous NaCl and anhydrous K Cl ratio preparation in 18: 4: 3 in molar ratio 500gAlCl
3The inorganic fused salt mixt of-NaCl-KCl is in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with sample with same mixing salt rapidly then, cover crucible cover;
4) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, and Heating temperature generally is controlled at 250 ℃, and soaking time is 7 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
Through soak test and polarization curve solidity to corrosion test shows: compare with undressed magnesium alloy, the corrosion stability of magnesium alloy after present embodiment is handled with this scheme improves nearly two orders of magnitude.
Claims (7)
1. a diffusion prevention method for inorganic fused salt on magnesium alloy surface is characterized in that, after the Mg alloy surface clean, puts into the inorganic fused salt system, and the inorganic fused salt system is selected AlCl for use
3-NaCl or AlCl
3-NaCl-KCl inorganic fused salt carries out induction heating to the inorganic fused salt system, forms intermetallic compound at Mg alloy surface.
2. diffusion prevention method for inorganic fused salt on magnesium alloy surface as claimed in claim 1 is characterized in that, described inorganic fused salt system is AlCl
3During-NaCl, AlCl
3With NaCl molar fraction ratio be 2: 3～4: 1, the fused salt diffusion temperature is 230 ℃～320 ℃, soaking time is 5 hours～8 hours.
3. diffusion prevention method for inorganic fused salt on magnesium alloy surface as claimed in claim 1 is characterized in that, described inorganic fused salt system is AlCl
3During-NaCl-KCl, AlCl
3Molar fraction accounts for 60%～75%, and the NaCl molar fraction accounts for 20%-30%, and KCl accounts for molar fraction 10%～15%, and the fused salt diffusion temperature is 230 ℃～280 ℃, and soaking time is 6 hours～8 hours.
4. diffusion prevention method for inorganic fused salt on magnesium alloy surface as claimed in claim 1 or 2 is characterized in that, described inorganic fused salt system is AlCl
3During-NaCl, carry out according to the following step:
1) Mg alloy surface is carried out mechanical scrubbing, remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl
3Prepare AlCl in proportion with anhydrous NaCl
3The inorganic fused salt mixt of-NaCl is in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with sample with same mixing salt rapidly then, cover crucible cover;
4) ceramic crucible that magnesium alloy is housed is placed into the diffusion of stove internal heating fused salt, heating, and soaking time is 5 hours～8 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
5. diffusion prevention method for inorganic fused salt on magnesium alloy surface as claimed in claim 4 is characterized in that, in the step 4), and described heating, its temperature is 270 ℃～320 ℃.
6. diffusion prevention method for inorganic fused salt on magnesium alloy surface as claimed in claim 5 is characterized in that, in the step 4), and described heating, its temperature is 270 ℃～300 ℃.
7. as claim 1 or 3 described diffusion prevention method for inorganic fused salt on magnesium alloy surface, it is characterized in that described inorganic fused salt system is AlCl
3During-NaCl-KCl, carry out according to the following step:
1) Mg alloy surface is carried out mechanical scrubbing, remove surface contaminant, use the acetone oil removing again, the alcohol flushing is then at air drying;
2) choose anhydrous AlCl
3, anhydrous NaCl and anhydrous K Cl prepare AlCl in proportion
3The inorganic fused salt mixt of-NaCl-KCl is in the exsiccant ceramic crucible of packing into;
3) pretreated magnesium alloy is put into the ceramic crucible that fills inorganic fused salt mixt, and guarantee that magnesium alloy must not contact sidewall of crucible, bury with the magnesium alloy block with same mixing salt rapidly then, cover crucible;
4) ceramic crucible that magnesium alloy will be housed is placed into the diffusion of stove internal heating fused salt, and Heating temperature generally is controlled at 230 ℃～280 ℃, and soaking time is 6 hours～8 hours; When stove internal heating fused salt spreads, for preventing the intrusion of water vapour and oxygen, make the oxidation of inorganic fused salt system suction and magnesium alloy, take to feed the mode of argon shield, before the stove heating, just feed in the stove, finish until insulation;
5) ceramic crucible that will reach soaking time takes out in stove, is cooled to room temperature in air, and magnesium alloy is taken out from fused salt, has promptly obtained forming on the surface magnesium alloy of magnalium intermetallic compound.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352502A (en) * | 2011-09-28 | 2012-02-15 | 武汉理工大学 | Thermal diffusing permeation method of inorganic rare earth molten salt on surface of magnesium alloy |
| CN102500526A (en) * | 2011-11-02 | 2012-06-20 | 沈阳飞机工业（集团）有限公司 | Novel pretreatment process for spraying aluminum for composite material molded part |
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| US4882199A (en) * | 1986-08-15 | 1989-11-21 | Massachusetts Institute Of Technology | Method of forming a metal coating on a substrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352502A (en) * | 2011-09-28 | 2012-02-15 | 武汉理工大学 | Thermal diffusing permeation method of inorganic rare earth molten salt on surface of magnesium alloy |
| CN102500526A (en) * | 2011-11-02 | 2012-06-20 | 沈阳飞机工业（集团）有限公司 | Novel pretreatment process for spraying aluminum for composite material molded part |
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