CN102268678A - Method for preparing magnesium-lithium alloy coating from precursor polymers - Google Patents
Method for preparing magnesium-lithium alloy coating from precursor polymers Download PDFInfo
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- CN102268678A CN102268678A CN2010101919439A CN201010191943A CN102268678A CN 102268678 A CN102268678 A CN 102268678A CN 2010101919439 A CN2010101919439 A CN 2010101919439A CN 201010191943 A CN201010191943 A CN 201010191943A CN 102268678 A CN102268678 A CN 102268678A
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Abstract
The invention provides a method for preparing a magnesium-lithium alloy surface coating. Ceramic precursor polymers such as polysilazane, polycarbosilane and polysiloxane and the like are used as base materials in the match with fillers such as B4C powder, SiC powder, SiO2 powder and Al2O3 powder and the like as well as a small amount of auxiliary agent; the method comprises the following steps of: step 1, adding a certain amount of the fillers and the auxiliary agent to the precursor solution and mixing into uniform slurry in a ball mill; step 2, coating the slurry on the treated surface of magnesium-lithium alloy in a brush-coating or spray-coating manner; step 3, putting the brush-coated sample in a nitrogen or vacuum furnace and curing the sample for 0.5-2h at a temperature of 150 DEG C to 200 DEG C; and step 4, carrying out the brush-coating (or spray-coating) and curing treatments on the withdrawn sample to obtain a reinforced coating. According to the invention, the precursor molecules are subjected to the cross-linking reaction to form a three-dimensional net-like high-polymer; the coating with a compact structure is formed on the surface of the magnesium-lithium alloy by adding the fillers; and the coating has good corrosion resistance, abrasion resistance and heat resistance and the like. The method disclosed by the invention is an ideal method for preparing the magnesium-lithium alloy coating at low cost and high efficiency, and the scope of applying magnesium-lithium alloy to the fields such as aerospace, automobiles and electronics and the like is expanded.
Description
Technical field
The present invention relates to the preparation method of magnesium lithium alloy surface protection coating.
Background technology
Magnesium lithium alloy is to be that base adds the alloy that metallic lithium is formed with magnesium.Generally contain lithium more than 15%, density is 1.14～1.57g/cm
3, being the lightest current structured material, specific tenacity is higher than conventional magnesium alloy, and intensity is 220～340MPa, Young's modulus 40GPa.The damping capacity height, cushioning ability is strong, has good hot and cold processing characteristics.Be used for the part manufacturing of aerospace craft part and other high speed rotating device.Because the solidity to corrosion of magnesium lithium alloy is poorer than ordinary magnesium alloy, thereby the solidity to corrosion difference is the key of restriction magnesium lithium alloy widespread use.
Coating technology is one of effective ways that improve metal and alloy corrosion resistance always.But because magnesium lithium alloy very easily corrosion in traditional high temperature or liquid phase surface environment, therefore traditional coat preparing technology is difficult to obtain good coating result.Therefore for improving the solidity to corrosion of magnesium lithium alloy, enlarge its range of application and field, research and development magnesium lithium alloy anti-corrosion coating technology becomes an important topic of people's concern in recent years.
It is base-material that the present invention adopts ceramic precursor polymkeric substance Polycarbosilane, polysilazane, polysiloxane, is equipped with B
4C powder, SiC powder, SiO
2Powder, Al
2O
3Fillers such as powder, and add a little auxiliary, adopt brushing-curing process to prepare the magnesium lithium alloy coating.The ceramic precursor polymkeric substance is that people pass through a kind of novel high polymer material of chemical process synthetic in recent years, contain silicon on the main chain, crosslinking reaction takes place in its in lower temperature range (150 ℃～200 ℃), form three-dimensional netted polymkeric substance, finally form the anti-corrosion coating of dense structure with the filler that adds.At present, ceramic precursor being used for the research that the magnesium lithium coating prepares the aspect does not appear in the newspapers.It is simple to operate, with low cost that the present invention has, and characteristics such as corrosion resistance coating, wear resistance, fine heat-resisting performance are that a kind of low cost, high benefit prepare magnesium lithium alloy protective coating perfect method.The application of magnesium lithium alloy in fields such as aerospace, automobile, electronics widened in this invention.
Summary of the invention
The effective preparation method who the purpose of this invention is to provide a kind of magnesium lithium alloy coating.
The preparation technology of coating is:
(a) surface preparation of magnesium lithium alloy: operation is: polish-clean-dry up, promptly utilize abrasive paper for metallograph that magnesium lithium alloy surface black film is removed, cold wind dries up after cleaning again.
(b) preparation of coating: with certain density precursor (Polycarbosilane, polysilazane, polysiloxane) solution and a certain proportion of filler (B
4C powder, SiC powder, SiO
2Powder, Al
2O
3Powder) mixed 5 hours in ball mill, make it to become uniform slurry.
(c) brushing: slurry is brushed or sprayed to surface treated magnesium lithium alloy surface equably.
(d) solidification process: sample is put into nitrogen furnace or vacuum oven be heated to 150 ℃～200 ℃, be incubated 0.5～2 hour, then with 2 ℃～5 ℃/minute speed cooling cooling with 2～5 ℃/minute temperature rise rate.
(e) enhancement process: the sample that will make is put into atmosphere or vacuum oven then through brushing once more or spray treatment, by original temperature curve heat treated.
Coating preparation is finished after above-mentioned steps.
The preparation method of described magnesium lithium alloy coating is characterized in that: described preceramic polymer is polysilazane, Polycarbosilane or polysiloxane, and its molecular weight is between the 1500-7000.
The preparation method of described magnesium lithium alloy coating is characterized in that: described filler is B
4C powder, SiC powder, SiO
2Powder, Al
2O
3The powder mix of two or more of powder, its granularity are between 0.5～10 μ m.
The preparation method of described magnesium lithium alloy coating is characterized in that: the slurry of being prepared is by preceramic polymer and the filler of certain content, the uniform sizing material that auxiliary agent forms after 5 hours through the high speed ball milling.
The preparation method of described magnesium lithium alloy coating is characterized in that: the sample after will brushing is put into nitrogen or vacuum oven, is heated to 150 ℃～200 ℃ with 2～5 ℃/minute temperature rise rates, solidifies 0.5～2 hour, then cooling.
The preparation method of described magnesium lithium alloy coating is characterized in that: this method can be used for preparing anti-corrosion, the wear-resistant coating of materials such as magnesium alloy, magnesium lithium alloy.
Advantage of the present invention is:
(1) to propose to adopt ceramic precursor first be raw material to this project, and the crosslinking reaction by the precursor molecule forms in the magnesium lithium alloy surface has three-dimensional netted high-performance coating, rich scientific and perspective.
(2) to adopt precursor be raw material in the present invention, by precursor contained-OH ,-NH
2Deng group and the magnesium lithium alloy surface-the OH group formation chemical bonding of having an effect, thereby coating and base material are closely combined.Make the inner build reticulated structure that forms of coating by curing reaction, finally form the high-performance coating of compact structure.Therefore coating has good isolation corrosive medium and effect such as wear-resisting.
(3) filler that adds among the present invention and precursor solidify to form the superpolymer interaction of build, have finally formed the anti-corrosion coating of dense structure.Thereby this coating has good bonding force, solidity to corrosion, thermotolerance and to the barrier propterty of matrix.
(4) the present invention adopts brushing or spraying coating process to prepare coating, be that type material is combined with good technology, therefore to have equipment simple for this method, easy to operate, the composition of product and controllable structure, characteristics such as easy to implement are one of a kind of preparation magnesium lithium alloy coating processes that has development prospect.
Description of drawings
Accompanying drawing 1 is the magnesium lithium alloy coatingsurface pattern stereoscan photograph that adopts the precursor preparation.As can be seen from Figure, coatingsurface is more smooth evenly, defectives such as flawless.Accompanying drawing 2 is the cross-section photograph that prepared the magnesium lithium alloy coating by precursor, and as can be seen from Figure, coating combines closely with interface between the matrix, does not have defectives such as tangible space and crackle, and the interface is in conjunction with good.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1: the preparation method of magnesium lithium alloy coating
(a) surface preparation of magnesium lithium alloy: it is body material that magnesium lithium alloy is adopted in experiment, and its surface preparation operation is mainly: polish-clean-dry up, promptly utilize abrasive paper for metallograph that magnesium lithium alloy surface black film is removed, cold wind dries up after cleaning again.
(b) preparation of coating: with certain density polysilazane and 10～20%B
4C powder filler, 10～20% SiC powder mixed 3 hours in ball mill, obtained uniform slurry.
(c) spraying: slurry is added in the spray gun, spray to surface treated magnesium lithium alloy surface equably.
(d) solidification process: sample is put into nitrogen furnace be heated to 200 ℃, be incubated 1 hour, then with 5 ℃ of/minute clock rate cooling coolings with 5 ℃ of/minute clock rate.
(e) enhancement process: the sample that will make is brushing polysilazane solution once more, puts into nitrogen furnace solidification treatment once more then.Coating preparation is finished after above-mentioned steps.
This coat-thickness is 10～20 μ m, and hardness reaches 220Hv, and the salt fog time was above 60 hours in 5%NaCl.
Embodiment 2: the preparation method of magnesium lithium alloy coating
(a) surface preparation of magnesium lithium alloy: it is body material that magnesium lithium alloy is adopted in experiment, and its surface preparation operation is mainly: polish-clean-dry up, promptly utilize abrasive paper for metallograph that magnesium lithium alloy surface black film is removed, cold wind dries up after cleaning again.
(b) preparation of coating: with certain density Polycarbosilane and 15%B
4C powder filler, 10% SiC powder, 8%SiO
2Powder mixed 5 hours in ball mill, obtained uniform slurry.
(c) brushing: slurry is brushed to surface treated magnesium lithium alloy surface equably.
(d) solidification process: sample is put into vacuum oven be heated to 180 ℃ with 5 ℃/minute, insulation 2h is then with 5 ℃ of/minute cooling coolings.
(e) enhancement process: the sample that will make is the brushing precursor solution once more, puts into vacuum oven solidification treatment once more then.
Coating preparation is finished after above-mentioned steps.
This coat-thickness is 10～20 μ m, and hardness reaches 200Hv, and the salt fog time was above 60 hours in 5%NaCl.
Embodiment 3: the preparation method of magnesium lithium alloy coating
(a) surface preparation of magnesium lithium alloy: it is body material that magnesium lithium alloy is adopted in experiment, and its surface preparation operation is mainly: polish-clean-dry up.
(b) preparation of coating: with certain density polysiloxane and a certain proportion of filler 10～20%Al
2O
3Powder, 10～20% SiO
2Powder obtained uniform slurry in 4 hours in the ball mill mixing.
(c) brushing: slurry is brushed to surface treated magnesium lithium alloy surface equably.
(d) solidification process: sample is put into vacuum oven be heated to 200 ℃, be incubated 1 hour, then with 3 ℃ of/minute cooling coolings with 3 ℃/minute.
(e) enhancement process: the sample that will make is the brushing precursor solution once more, puts into vacuum oven solidification treatment once more then.
Coating preparation is finished after above-mentioned steps.
This coat-thickness is 10～20 μ m, and hardness reaches 180Hv, and the salt fog time was above 60 hours in 5%NaCl.
Embodiment 4: the preparation method of magnesium alloy coating
(a) surface preparation of magnesium alloy: experiment AZ91D diecast magnesium alloy is a body material, and its surface preparation operation is mainly: (distilled water) is washed → washed to oil removing → washing → weak acid.
(b) preparation of coating: with certain density polysilazane and 10～20%B
4C powder filler, 10～20% SiC powder mixed 5 hours in ball mill, obtained uniform slurry.
(c) spraying: slurry is added in the spray gun, spray to surface treated magnesium lithium alloy surface equably.
(d) solidification process: sample is put into nitrogen furnace be heated to 200 ℃, be incubated 1 hour, then with 5 ℃ of/minute clock rate cooling coolings with 5 ℃ of/minute clock rate.
(e) enhancement process: the sample that will make is brushing polysilazane solution once more, puts into nitrogen furnace then, by original temperature curve solidification treatment.
Coating preparation is finished after above-mentioned steps.
This coat-thickness is 10～20 μ m, and hardness reaches 220Hv, and the salt fog time was above 60 hours in 5%NaCl.
Claims (8)
1. method for preparing the magnesium lithium alloy coating, realized by following steps:
(1) surface preparation of magnesium alloy: operation is: polish-clean-dry up, promptly utilize abrasive paper for metallograph that magnesium lithium alloy surface black film is removed, cold wind dries up after cleaning again.
(2) preparation of coating: with the filler (B of certain density precursor (Polycarbosilane, polysilazane, polysiloxane) solution with certain content
4C powder, SiC powder, SiO
2Powder, Al
2O
3Powder) mixed 3～5 hours in ball mill, make it to become uniform slurry.
(3) brush or spray: with the mode of brushing or spray slurry is coated with and is contained in treated magnesium lithium alloy surface;
(4) solidification process: sample is put into nitrogen furnace or vacuum oven be heated to 150 ℃～200 ℃, be incubated 0.5～2 hour, then with 2 ℃～5 ℃/minute speed cooling cooling with 2～5 ℃/minute temperature rise rate.
(5) enhancement process: the sample that will make is put into nitrogen or vacuum oven, once more solidification treatment then through brushing once more or spray treatment.
Coating preparation is finished after above-mentioned steps.
2. the preparation method of magnesium lithium alloy coating according to claim 1 is characterized in that: described preceramic polymer is a kind of in polysilazane, Polycarbosilane or the polysiloxane, and its molecular weight is between the 1500-7000.
3. the preparation method of magnesium lithium alloy coating according to claim 1 is characterized in that: described filler is B
4C powder, SiC powder, SiO
2Powder, Al
2O
3The powder mix of one or more in the powder, its granularity are between 0.5～5 μ m.
4. the preparation method of magnesium lithium alloy coating according to claim 1 is characterized in that: preceramic polymer is made into uniform slurry with the filler and the auxiliary agent of certain content through ball milling after 3～5 hours.
5. the preparation method of magnesium lithium alloy coating according to claim 1 is characterized in that: with the mode of brushing or spray slurry is coated with and is contained in treated magnesium lithium alloy surface.
6. the preparation method of magnesium lithium alloy coating according to claim 1 is characterized in that: the sample after will brushing is put into nitrogen or vacuum oven, is warmed up to 150 ℃～200 ℃ with 2 ℃～5 ℃/minute speed, solidifies 0.5～2 hour, then naturally cooling.
7. the preparation method of magnesium lithium alloy coating according to claim 1 is characterized in that: the sample that will make is put into nitrogen or vacuum oven, once more solidification treatment then through brushing once more or spray treatment.
8. the preparation method of magnesium lithium alloy coating according to claim 1 is characterized in that: this method can be used for preparing anti-corrosion, the wear-resistant coating of materials such as magnesium alloy, magnesium lithium alloy.
Priority Applications (1)
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| CN2010101919439A CN102268678A (en) | 2010-06-04 | 2010-06-04 | Method for preparing magnesium-lithium alloy coating from precursor polymers |
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| CN2010101919439A CN102268678A (en) | 2010-06-04 | 2010-06-04 | Method for preparing magnesium-lithium alloy coating from precursor polymers |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543868A (en) * | 2016-11-08 | 2017-03-29 | 铜陵中锐电子科技有限公司 | Modified resistant polyester nitrile rubber composite powder coatings of a kind of Jing hyperbranched polycarbosilanes and preparation method thereof |
| CN107686559A (en) * | 2017-09-29 | 2018-02-13 | 西安近代化学研究所 | A kind of engine composite adiabatic layer |
| CN108793958A (en) * | 2018-07-12 | 2018-11-13 | 刘少标 | A method of improving steel substrate surface wearable ceramic coat layer thermal shock resistance |
| CN109261460A (en) * | 2018-09-10 | 2019-01-25 | 镇江朝阳机电科技有限公司 | A kind of composite anti-corrosion cable testing bridge and coating process |
| CN109400932A (en) * | 2018-09-28 | 2019-03-01 | 苏州泰仑电子材料有限公司 | Heat-resisting release film of highly flexible ultraviolet curing and preparation method thereof |
| CN110760916A (en) * | 2019-11-18 | 2020-02-07 | 和县科嘉阀门铸造有限公司 | Method for improving corrosion resistance of magnesium alloy valve |
| CN110925779A (en) * | 2019-12-11 | 2020-03-27 | 大连东泰产业废弃物处理有限公司 | Method for utilizing perhydropolysilazane-containing waste organic solvent in incinerator |
| CN111218207A (en) * | 2019-12-30 | 2020-06-02 | 江苏新宇生物科技有限公司 | Preparation and use method of polycarbosilane and aluminum oxide magnesium oxide compound solution |
| KR20200084270A (en) * | 2019-01-02 | 2020-07-10 | 금오공과대학교 산학협력단 | Coating method for inorganic polysilazane on the surface of magnesium alloy and magnesium alloy formed thereby |
| CN116355530A (en) * | 2023-03-24 | 2023-06-30 | 上海大学 | Magnesium alloy surface coating material, coating and preparation method thereof |
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2010
- 2010-06-04 CN CN2010101919439A patent/CN102268678A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106543868A (en) * | 2016-11-08 | 2017-03-29 | 铜陵中锐电子科技有限公司 | Modified resistant polyester nitrile rubber composite powder coatings of a kind of Jing hyperbranched polycarbosilanes and preparation method thereof |
| CN107686559A (en) * | 2017-09-29 | 2018-02-13 | 西安近代化学研究所 | A kind of engine composite adiabatic layer |
| CN108793958A (en) * | 2018-07-12 | 2018-11-13 | 刘少标 | A method of improving steel substrate surface wearable ceramic coat layer thermal shock resistance |
| CN109261460A (en) * | 2018-09-10 | 2019-01-25 | 镇江朝阳机电科技有限公司 | A kind of composite anti-corrosion cable testing bridge and coating process |
| CN109400932A (en) * | 2018-09-28 | 2019-03-01 | 苏州泰仑电子材料有限公司 | Heat-resisting release film of highly flexible ultraviolet curing and preparation method thereof |
| KR20200084270A (en) * | 2019-01-02 | 2020-07-10 | 금오공과대학교 산학협력단 | Coating method for inorganic polysilazane on the surface of magnesium alloy and magnesium alloy formed thereby |
| KR102170244B1 (en) | 2019-01-02 | 2020-10-28 | 금오공과대학교 산학협력단 | Coating method for inorganic polysilazane on the surface of magnesium alloy and magnesium alloy formed thereby |
| CN110760916A (en) * | 2019-11-18 | 2020-02-07 | 和县科嘉阀门铸造有限公司 | Method for improving corrosion resistance of magnesium alloy valve |
| CN110760916B (en) * | 2019-11-18 | 2022-04-05 | 和县科嘉阀门铸造有限公司 | Method for improving corrosion resistance of magnesium alloy valve |
| CN110925779A (en) * | 2019-12-11 | 2020-03-27 | 大连东泰产业废弃物处理有限公司 | Method for utilizing perhydropolysilazane-containing waste organic solvent in incinerator |
| CN111218207A (en) * | 2019-12-30 | 2020-06-02 | 江苏新宇生物科技有限公司 | Preparation and use method of polycarbosilane and aluminum oxide magnesium oxide compound solution |
| CN116355530A (en) * | 2023-03-24 | 2023-06-30 | 上海大学 | Magnesium alloy surface coating material, coating and preparation method thereof |
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Application publication date: 20111207 |