CN101210319B - Chemical aluminum plating solution and chemical aluminum plating method - Google Patents
Chemical aluminum plating solution and chemical aluminum plating method Download PDFInfo
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- CN101210319B CN101210319B CN200710164611XA CN200710164611A CN101210319B CN 101210319 B CN101210319 B CN 101210319B CN 200710164611X A CN200710164611X A CN 200710164611XA CN 200710164611 A CN200710164611 A CN 200710164611A CN 101210319 B CN101210319 B CN 101210319B
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Abstract
The invention discloses a chemical aluminum plating solution and a chemical aluminum plating method. The chemical aluminum plating solution is composed of an aluminum-containing room-temperature molten salt and a reducer, wherein 0.05 to 2.5 mol reducer is contained in every liter of the aluminum-containing room-temperature molten salt. The method comprises the following steps of: soaking a workpiece to be plated in SnCl2 solution for sensitizing treatment, cleaning with water, and soaking in a PdCL2 solution for activation; or soaking a mixture solution containing SnCl2 and PdCl2 for activation; and chemically plating aluminum using the chemical aluminum plating solution in a dry inert atmosphere. According to the invention, aluminum can be separated out on the workpiece to be plated to achieve chemical aluminum plating by soaking the workpiece in the solution without electrifying. The invention can plate light-weight aluminum with excellent electrical conductivity and thermal conductivity not only on a metal base but also on an insulating workpiece to be plate. Moreover, the aluminum can be uniformly plated even for the workpiece with complex shape or for powder without considering the uniformity of current distribution since no electroplating is adopted. Accordingly, the invention has great practical value.
Description
Technical field
The present invention relates to a kind of technology of aluminizing, especially relate to a kind of electroless plating aluminum solutions and chemical aluminum plating method.
Technical background
Aluminium is because big with the avidity of oxygen, and its redox potential is lower than hydrogen, therefore is difficult to electroplate in the aqueous solution.Use non-aqueous solution so generally aluminize, particularly organic solvent is as electroplate liquid, but organic solvent electroplate exist catch fire, danger such as blast.The melting salt that for this reason the works out no danger of combustion solution of aluminizing is aluminized, for example aluminum chloride-chlorination 1-methyl-3-ethyl imidazol(e) (AlCl
3-EMIC) room temperature fused salt, aluminum chloride-chlorination normal-butyl pyridine (AlCl
3-BPC) room temperature fused salt, and aluminum chloride-quaternary amine ([(R
1)
3N
+R
2] X
-, R
1Represent alkyl, the R of carbon containing 1～12
2The alkyl, the X that are carbon containing 1～12 are halogen atom) room temperature fused salt that forms.For example, patent documentation 1 (spy opens flat 6-101088 communique) discloses with imidazolium halides and aluminum halide and has mixed the low melting point electroplate liquid that forms, and negative electrode is separated out the electro-plating method of A1.Patent documentation 2 (spy opens flat 1-272788 communique) discloses the low melting point electroplate liquid of quaternary amine and the formation of aluminum halide mixed melting, the method for electroplating A1 at negative electrode.But Electroplating Aluminum can only be carried out at the body surface that metal etc. has electroconductibility, and carries out also difficulty relatively of even plating at complex-shaped body surface.
On the other hand, as non-patent literature 1 (Richard N.Rhoda, et al., Transactions of theInstitute of Metal Finishing, 82-85,36 (1959)) shown in, chemical nickel plating (Ni) has just been arranged, copper (Cu) since very early, cobalt (Co), silver (Ag), platinum (Pt), methods such as gold (Au) and alloy thereof.
Summary of the invention
The purpose of this invention is to provide a kind of electroless plating aluminum solutions and chemical aluminum plating method, power consumption is significantly descended, not only to metallic matrixes such as the copper of electroconductibility, brass, nickel, iron, also can be to isolator matrixes such as glass, plastics, potteries, and powder of these objects, CNT (carbon nano-tube) etc. carry out chemistry and aluminize, and object of complicated shape, powdered object etc. also can plating.
The technical solution adopted for the present invention to solve the technical problems is:
One, a kind of electroless plating aluminum solutions:
Be made up of aluminiferous room temperature fused salt and reductive agent, containing reductive agent in every liter of aluminiferous room temperature fused salt is 0.05～2.5mol.
Described aluminiferous room temperature fused salt is that halogenation and aluminum halide mixed melting are made; Both ratios are: 100 moles of halogenations, 60～300 moles of aluminum halides.
Described halogenation is quaternary amine, imidazole salts or pyridinium salt.
Described reductive agent is one or two or more kinds the mixture in lithium hydride, diisobutyl aluminium hydride, aluminium lithium hydride, sodium alanate, the lithium borohydride.
Can also contain the organic solvent that does not react with claim 3 or 4 in the described electroless plating aluminum solutions, organic solvent content in chemistry is aluminized liquid is 0～90% volume percent.
Described organic solvent is benzene, toluene, o-Xylol, m-xylene, p-Xylol.
Two, a kind of chemical aluminum plating method of electroless plating aluminum solutions:
Unplated piece is with containing SnCl
2After the solution impregnation sensitization was handled, washing entered and contains PdCl
2Solution impregnation is carried out activation treatment; Perhaps containing SnCl
2And PdCl
2Mixing solutions in flood, carry out activation treatment; In dry inert atmosphere, carry out chemistry with the electroless plating aluminum solutions and aluminize again.
The beneficial effect that the present invention has is:
Adopt electroless plating aluminum solutions of the present invention, can no power, only will flood in unplated piece and the solution, aluminium is separated out on unplated piece, the realization chemistry is aluminized.Adopt chemical aluminum plating method of the present invention, not only can also can on the unplated piece of isolator, obtain electroconductibility, thermal conductivity is good, light-weight aluminium at metallic matrix.And, owing to be not to electroplate, therefore can consider the homogeneity of distribution of current, though complex-shaped unplated piece, or powder, plating equably.Therefore the present invention has great practical value.
Embodiment
Electroless plating aluminum solutions of the present invention is made up of aluminiferous room temperature fused salt and reductive agent.Aluminiferous room temperature fused salt mixes acquisition by halide salt and aluminum contained compound, and (25 ℃) are liquid under the room temperature.The present invention is used contains the aluminium room temperature fused salt, is halogenation and aluminum chloride mixed melting thing, and aluminium also can add in the solution by anode dissolution.
Described halogenation, tetraethylammonium bromide is arranged, the trimethylammonium ethyl ammonium chloride, trimethylammonium butyl ammonium chloride, tripropyl butyl ammonium chloride, quaternary amines such as triethyl dodecyl bromination ammonium, trimethylammonium puratized agricultural spray system, two (trifluoromethane sulfonic acid acyl) inferior amine salt of tetra-allkylammonium, ammoniums such as trimethylammonium alkyl ammonium salt system, the chlorinated butyl pyridine, chlorination normal-butyl pyridine pyridinium salts such as (BPC), chlorination 1-methyl-3-ethyl imidazol(e) imidazole salts such as (EMIC), microcosmic salts such as ethyl tributyl bromo-phosphonium, Tetrafluoroboric acid 1-methyl-3-ethyl imidazol(e) (EMIBF4), the 1-ethyl-3-Methylimidazole two (trifluoromethanesulp-onyl-onyl imide) (EMITFSI), fluorine hydrogenation 1-ethyl-3-Methylimidazole (EMIF2, the fragrant same clan such as 3HF).Wherein, quaternary amine, imidazole salts, pyridinium salt are better.General expression is [(R
1)
3N
+R
2] X
-(R
1Represent alkyl, the R of carbon containing 1～12
2The alkyl, the X that are carbon containing 1～12 represent halogen element) quaternary amine, chlorination 1-methyl-3-propyl imidazole (EMIC), chlorination normal-butyl pyridine (BPC) to form the compositing range of liquid phase when room temperature big, the electric conductivity height, therefore better.These materials are by the combination of mineral ion and organic ion, and perhaps the combination of organic ion obtains.In addition, chloride salt and bromide salt Comparatively speaking, though fusing point is slightly high, price is cheaper, so chloride salt is more suitable.
Aluminum halide is AlX
3(X represents halogen atom) is specially aluminum fluoride (AlF
3), aluminum chloride (AlCl
3), aluminum bromide (AlBr
3) and aluminum iodide (AlI
3) etc., wherein with AlCl
3And AlBr
3More suitable, again with anhydrous AlCl
3Better, the fusing point of solution is lower, and price is also cheaper.
For aluminium is evenly separated out on the unplated piece surface, need the Al that considers that fusing point, electric conductivity, viscosity, aluminium are separated out
2Cl
7-ionic concn etc., therefore, to 100 moles of halogenations, aluminum halide is advisable for 60～300 moles, and 80～250 moles are better, and optimum is 200 moles.
Reductive agent is for containing basic metal and alkaline earth metal compounds such as Li, Na, Al.The used reductive agent of the present invention is lithium hydride (LiH), diisobutyl aluminium hydride (DIBAH), aluminium lithium hydride (LiAlH
4), sodium alanate (NaAlH
4), lithium borohydride (LiBH
4) in one or both and above mixture.Wherein DIBAH and LiH, LiAlH
4The reducing power that tool is identical and be liquid.
In the electroless plating aluminum solutions of the present invention, can add and contain aluminium room temperature fused salt and the nonreactive organic solvent of reductive agent.For example, benzene series, toluene system, diformazan benzene series etc., wherein better with benzene, toluene, o-Xylol, m-xylene, p-Xylol.
Reductive agent can add as follows: directly add the back in the room temperature fused salt and mix; Add in the organic solvents such as the benzene series that does not react with reductive agent, toluene system and disperse the back to add room temperature fused salt; Aluminum halide and halogenation add after with 1: 1～0.8: 1 scope mixed dissolution of mol ratio.Can get wherein a kind ofly, or two or more method combination all can.The addition of reductive agent is: add 0.05～2.5mol in every liter of chemical plating fluid for well, 0.1～1.5mol is better.Addition is very few, and then show-through situation can appear in all plating difficulties of matrix.
Chemical aluminum plating method of the present invention is that unplated piece is being contained PdCl
2Solution in after the dipping activation treatment, in dry inert atmosphere, carry out electroless plating with the aforementioned chemistry liquid of aluminizing.Unplated piece is not as long as decompose in containing the aluminium room temperature fused salt, whatsoever material, shape can.As long as not only metal, and glass, plastics, pottery etc. through the overactivation pre-treatment, impregnated in the plating bath, can be covered the aluminium of matrix fully.The no power because chemistry is aluminized, therefore which kind of state can not have problems.In addition, if before the activation treatment substrate is carried out roughening treatment, help obtaining the good aluminium coat of tack.
The following method of activation treatment is carried out: among the weakly acidic water solution 100ml that hydrochloric acid and deionized water form, add dissolving PdCl
20.0025～0.067g will flood in this solution 1～10 minute through the unplated piece that sensitization is handled.In addition, also with activating treatment process with other; It is also passable perhaps to make unplated piece absorption have the activation treatment of reactive ion.Contain PdCl
2Solution, be not limited to be dissolved with PdCl
2Solution, also can be to contain PdCl
2And SnCl
2Solution.
Rare gas element can be helium, neon, argon, krypton, xenon, radon, nitrogen etc., wherein with argon and nitrogen for well.
Chemical aluminum plating method of the present invention before the activation treatment, is preferably containing SnCl with unplated piece
2Flood in the solution.For example, unplated piece is being contained SnCl
2After the dipping sensitization was handled in the solution, washing was containing PdCl then
2Flood activation treatment in the solution, in dry inert atmosphere, carry out electroless plating afterwards with the electroless plating aluminum solutions.Thus, the condition of surface of plating is more even, and the speed of separating out of aluminium also can increase.
The sensitization treatment process is: among the acidic aqueous solution 100ml that hydrochloric acid and deionized water form, add 0.48～9.6g SnCl
2Dissolving forms sensitizing solution, unplated piece dipping 1-10 minute.Also can use sensitization treatment process in addition.In addition, unplated piece was preferably through grinding, skimming treatment before sensitization was handled.
The temperature of electroless plating aluminum solutions is controlled at 15 ℃～90 ℃, and temperature is high more, and to separate out the speed of aluminium fast, causes self-decomposition easily but surpass 70 ℃ of solution, and therefore, temperature preferably is controlled at 15 ℃～45 ℃.In addition, can change the amount of separating out of aluminium by the dipping time of unplated piece; For example 35 ℃ following 2 hours with the interior aluminium coat that can obtain to cover fully matrix.
Embodiment
(1) chemistry is aluminized with the preparation of solution
Plating bath 1: in the dry argon gas vacuum glove box, anhydrous AlCl
3(99.9%) and EMIC with molal weight than weighing in 2: 1, do not rise near maintaining the temperature at 50 ℃, progressively add AlCl while stirring on a small quantity
3Make its complete fusion, with the 99.99% aluminum steel dipping of q.s, the displacement of (about 25 ℃) 1 week is made with extra care under the room temperature, obtains chemistry and aluminizes with solution 1 (AlCl again
3-EMIC).
Plating bath 2: EMIC is substituted with BPC, and other steps identical with plating bath 1 are made the chemistry usefulness solution 2 (AlCl that aluminize
3-BPC).
Plating bath 3: EMIC is substituted with the trimethylammonium ethyl ammonium chloride, and other and plating bath 1 same steps as are made chemistry and are aluminized with solution 3.
Plating bath 4: EMIC is substituted with the tripropyl ethyl ammonium chloride, and other and plating bath 1 same steps as are made chemistry and are aluminized with solution 4.
Plating bath 5: with anhydrous AlCl
3(99.9%) the molal weight ratio with EMIC changed 3: 2 into by 2: 1, and other and plating bath 1 same steps as are made chemistry and aluminized with solution 5 (AlCl
3-EMIC).
Plating bath 6: with anhydrous AlCl
3(99.9%) the molal weight ratio with EMIC changed 52: 48 into by 2: 1, and other and plating bath 1 same steps as are made chemistry and aluminized with solution 6 (AlCl
3-EMIC).
Plating bath 7: with anhydrous AlCl
3(99.9%) with the molal weight of EMIC than changing 1: 2 into by 2: 1, other steps identical with plating bath 1 are made the chemistry usefulness solution 7 (AlCl that aluminize
3-EMIC).
(2) the preparation embodiment of electroless plating aluminum solutions
Embodiment 1: get 62.5ml plating bath 1 in general beaker, beaker has been put into temperature controlled well heater, and bath temperature remains on about 35 ℃, afterwards reductive agent LiH is added in the plating bath 1 while stirring, reductive agent is disperseed in plating bath, obtain the chemistry liquid 1 of aluminizing.The add-on of reductive agent is 1mol in every liter of plating bath 1 (0.5g).
Embodiment 2: replace plating baths 1 with plating bath 2, other is with embodiment 1, obtains the chemistry of the present invention liquid 2 of aluminizing.
Embodiment 3: replace plating baths 1 with plating bath 3, other is with embodiment 1, obtains the chemistry of the present invention liquid 3 of aluminizing.
Embodiment 4: replace plating baths 1 with plating bath 4, other is with embodiment 1, obtains the chemistry of the present invention liquid 4 of aluminizing.
Embodiment 5: replace plating baths 1 with plating bath 5, other is with embodiment 1, obtains the chemistry of the present invention liquid 5 of aluminizing.
Embodiment 6: replace plating baths 1 with plating bath 6, other is with embodiment 1, obtains the chemistry of the present invention liquid 6 of aluminizing.
Embodiment 7: use LiAlH
4Replace LiH, other is with embodiment 1, obtains the chemistry of the present invention liquid 7 of aluminizing.
Embodiment 8: replace LiH with DIBAH, and add-on is 0.2mol in every liter of plating bath 1 (1.78g), other is with embodiment 1, obtains the chemistry of the present invention liquid 8 of aluminizing.
Embodiment 9: replace plating baths 1 with plating bath 7, other is with embodiment 1, obtains the chemistry of the present invention liquid 9 of aluminizing.
Embodiment 10: add volume content respectively and be 10%, 50% or 90% toluene in the solution of embodiment 1 preparation, obtain chemical aluminium liquid 10 of the present invention.
Comparative example 1: do not add LiH in the plating bath 1, other are with embodiment 1, obtain relatively with the chemistry liquid R1 that aluminizes.
(3) experimental example of aluminizing
Test example 1:
Copper coin to be plated, sheet brass, tungsten plate, iron plate, grind through 320# sand paper (paper Co., Ltd. system is ground by Japan), if the powder of these objects is then directly used methyl alcohol ultrasonic cleaning 5 minutes, use the degreasing in 5 minutes of acetone ultrasonic cleaning afterwards again, carry out pre-treatment.
Use secondary deionized water 99ml in addition, add concentrated hydrochloric acid 1ml, and dissolving 2.4g SnCl
2(every liter of 0.127mol) is prepared into sensitizing solution.Secondary deionized water 99ml adds concentrated hydrochloric acid 1ml, and dissolving 0.030g PdCl
2(every liter of 1.691mmol) is prepared into activation solution.Through the unplated piece of pre-treatment, the sensitization of 5 minutes dippings is handled in sensitizing solution, washes 5 minutes dipping activation treatment in the postactivated liquid, washes cold air drying afterwards.
Each unplated piece after the activation treatment is flooded in chemistry is aluminized liquid 1～10, R1, and near room temperature (25 ℃) was taken out unplated piece after placing in 3 hours from chemistry is aluminized liquid 1～10, R1.As a result, chemistry is aluminized, and integral body has covered precipitate on the unplated piece of dipping in the liquid 1～8.The precipitate that obtains in wherein chemical aluminize liquid 1 and 8 is more even, and speed of separating out is very fast.The chemistry coating that obtains in the liquid 10 of aluminizing is more smooth, smooth.To plate that the back thing cleans in dehydration benzene and ultrasonic cleaning after, cold air drying.Carry out results of elemental analyses, detect aluminium with SEM (scanning electronic microscope)/EDX.X ray (CuK, 2kW), GD-OES (glow discharge optical emission spectrometry surface analysis JY-5000RF) detects and to show, confirmed that precipitate is an aluminium.In addition, this test shows that chemistry is aluminized and can at room temperature be carried out.On the other hand, chemistry is aluminized, and the unplated piece of dipping has the part precipitate in the liquid 9, and chemistry is aluminized on the unplated piece of liquid R1 dipping, does not have precipitate.
Test example 2:
The chemistry liquid 1 of aluminizing, unplated piece is the powder of sheet glass, ABS plastic plate, alumina plate or these objects, and CNT (carbon nano-tube) etc., dipping time 1 hour, activation treatment liquid are 0.3gg/L PdCl
2-12g/L SnCl
2The mixing solutions of-10ml/L HCl-160g/L NaCl, the treatment time is 30 minutes, other are with test example 1.As a result, integral body has covered precipitate on the unplated piece, shows that with detections such as X ray, SEM/EDX, GD-OES precipitate is an aluminium.
Test example 3:
With the chemistry liquid 8 instead of chemical liquid 1 of aluminizing of aluminizing, other is with test example 2.As a result, integral body has covered precipitate on the unplated piece, shows that with detections such as X ray, SEM/EDX, GD-OES precipitate is an aluminium.
Test example 4:
Use AlBr
3Replace AlCl
3, EMIB (bromination 1-methyl-3-ethyl imidazol(e)) replaces EMIC to aluminize as chemistry use solution, prepares the chemistry liquid of aluminizing with embodiment 1 then, carries out plating, and the result has obtained the aluminium precipitate.
Claims (5)
1. electroless plating aluminum solutions, it is characterized in that: be made up of aluminiferous room temperature fused salt and reductive agent, containing reductive agent in every liter of aluminiferous room temperature fused salt is 0.05～2.5mol;
Described aluminiferous room temperature fused salt is that halogenation and aluminum halide mixed melting are made; Both ratios are: 100 moles of halogenations, 60～300 moles of aluminum halides;
Described reductive agent is one or two or more kinds the mixture in lithium hydride, diisobutyl aluminium hydride, aluminium lithium hydride, sodium alanate, the lithium borohydride.
2. a kind of electroless plating aluminum solutions according to claim 1 is characterized in that described halogenation is quaternary amine, imidazole salts or pyridinium salt.
3. a kind of electroless plating aluminum solutions according to claim 1, it is characterized in that also containing in the described electroless plating aluminum solutions organic solvent that does not react with described halogenation and described reductive agent, organic solvent content in chemistry is aluminized liquid is 0～90% volume percent.
4. a kind of electroless plating aluminum solutions according to claim 3 is characterized in that described organic solvent is benzene, toluene, o-Xylol, m-xylene or p-Xylol.
5. be used for the chemical aluminum plating method of the described a kind of electroless plating aluminum solutions of claim 1, it is characterized in that: unplated piece is with containing SnCl
2After the solution impregnation sensitization was handled, washing entered and contains PdCl
2Solution impregnation is carried out activation treatment; Perhaps containing SnCl
2And PdCl
2Mixing solutions in flood, carry out activation treatment; In dry inert atmosphere, carry out chemistry with the electroless plating aluminum solutions and aluminize again.
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|---|---|---|---|
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|---|---|---|---|
| CN200710164611XA CN101210319B (en) | 2007-12-21 | 2007-12-21 | Chemical aluminum plating solution and chemical aluminum plating method |
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| CN101210319B true CN101210319B (en) | 2010-06-02 |
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| CN102347530A (en) * | 2010-08-05 | 2012-02-08 | 北京聚利科技有限公司 | Design of antenna array used for electronic toll collection for freeway |
| JP5914954B2 (en) | 2011-01-05 | 2016-05-11 | ディップソール株式会社 | Electroaluminum or aluminum alloy molten salt plating bath with good throwing power, and electroplating method and pretreatment method using the same |
| CN103469055B (en) * | 2013-08-01 | 2015-07-01 | 西安建筑科技大学 | Lead-adding process in smelt of lead-containing free-cutting stainless steel used for nibs |
| WO2020089690A2 (en) | 2018-10-30 | 2020-05-07 | The American University In Cairo | Method for aluminum electroless deposition |
| CN111663129A (en) * | 2019-03-06 | 2020-09-15 | 唐文海 | Chemical aluminium alloy plating process (aluminium chloride type) |
| 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 |
| CN113533405B (en) * | 2021-07-27 | 2022-08-09 | 唐山钢铁集团有限责任公司 | Method for observing Al5FeSi phase in aluminum-silicon coating original plate alloy layer |
| CN116140863B (en) * | 2023-02-25 | 2023-10-10 | 东莞市千岛金属锡品有限公司 | High-heat-resistance lead-free tin bar and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5135825A (en) * | 1989-06-22 | 1992-08-04 | Mitsubishi Petrochemical Co., Ltd. | Method for producing ambient temperature molten salt consisting of certain pyridinium and imidazolium halides and an aluminum trihalide |
-
2007
- 2007-12-21 CN CN200710164611XA patent/CN101210319B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5135825A (en) * | 1989-06-22 | 1992-08-04 | Mitsubishi Petrochemical Co., Ltd. | Method for producing ambient temperature molten salt consisting of certain pyridinium and imidazolium halides and an aluminum trihalide |
Non-Patent Citations (4)
| Title |
|---|
| JP特开2003-92135A 2003.03.28 |
| JP特开平5-271986A 1993.10.19 |
| 范春华，等。.室温氯化铝-有机熔盐电沉积铝的研究进展.材料保护40 10.2007,40(10),50-53. |
| 范春华等.室温氯化铝-有机熔盐电沉积铝的研究进展.材料保护40 10.2007,40(10),50-53. * |
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