CN109056007A - A kind of method that the electro-deposition of Organic Solvent at Room Temperature system prepares aluminum titanium alloy coating - Google Patents
A kind of method that the electro-deposition of Organic Solvent at Room Temperature system prepares aluminum titanium alloy coating Download PDFInfo
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- CN109056007A CN109056007A CN201811097944.XA CN201811097944A CN109056007A CN 109056007 A CN109056007 A CN 109056007A CN 201811097944 A CN201811097944 A CN 201811097944A CN 109056007 A CN109056007 A CN 109056007A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
一种室温有机溶剂体系电沉积制备铝钛合金镀层的方法，涉及一种制备合金镀层的方法，所述方法包括以下制备过程：镀液的制备，称取无水氯化铝和氢化铝锂；将无水四氯化钛缓慢地加入到无水氯化铝和氢化铝锂中；该过程苯和四氢呋喃的使用比例为4:1~4:3；铜基体处理，将铜片依次用400、800、1200目的砂纸打磨光滑，除油；恒电流电沉积，以石墨作阳极，铜片作阴极，控制电流密度为6‑38毫安/平方厘米，进行电沉积，即可获得纯净且颗粒大小均匀的铝钛合金，电沉积时间控制为3~5小时。该方法采用石墨作阳极，通过添加无水四氯化钛获得一定浓度的钛离子，该方法成本低，产生的铝钛合金纯净且颗粒大小均匀，钛含量高。A method for preparing an aluminum-titanium alloy coating by electrodeposition in an organic solvent system at room temperature relates to a method for preparing an alloy coating, and the method includes the following preparation process: preparing a plating solution, weighing anhydrous aluminum chloride and lithium aluminum hydride; Slowly add anhydrous titanium tetrachloride to anhydrous aluminum chloride and lithium aluminum hydride; the ratio of benzene and tetrahydrofuran used in this process is 4:1~4:3; the copper substrate is treated, and the copper sheet is sequentially used 400, 800, 1200 mesh sandpaper is smoothed and degreased; constant current electrodeposition, using graphite as anode and copper sheet as cathode, control the current density at 6‑38 mA/cm2, and conduct electrodeposition to obtain pure and fine particle size For uniform aluminum-titanium alloy, the electrodeposition time is controlled within 3-5 hours. In the method, graphite is used as an anode, and a certain concentration of titanium ions is obtained by adding anhydrous titanium tetrachloride. The method has low cost, and the produced aluminum-titanium alloy is pure and has uniform particle size and high titanium content.
Description
Technical field
The present invention relates to a kind of methods for preparing alloy layer, more particularly to a kind of Organic Solvent at Room Temperature system electro-deposition
The method for preparing aluminum titanium alloy coating.
Background technique
Aluminum titanium alloy has the excellent performances such as excellent corrosion resistance, biocompatibility and high specific strength, therefore wide
It is general to be applied to the fields such as space flight and aviation, automobile, medical treatment and electronic product.The preparation method of aluminum titanium alloy mainly has directly molten match
Method, sintering process, reduction method and four kinds of electrodeposition process.Direct mix-melting method can consume a large amount of titanium and heat in process of production, increase
Add production cost, and aluminum titanium alloy obtained is easy crystal grain segregation and oxidation, to raw material titanium recycling difficulty etc.；Sintering process is right
More demanding, the increase production cost of equipment；Reduction method, high production cost, and it is easy crystal grain segregation；Electrodeposition process, can be effective
The probability of crystal grain segregation and oxidation is reduced, surface property is improved, saves production cost.But at room temperature, the standard electric of aluminium and titanium
Electrode potential is defeated by the electrode potential of hydrogen, and electrochemical deposition aluminum titanium alloy has evolving hydrogen reaction generation in aqueous solution, influences coating
Quality.Even if to shuffle the reduction potential of titanium and aluminium, but liberation of hydrogen is anti-by increasing titanium ion and aluminum ions concentration in electrolyte
Can should still it occur, therefore the electrochemical deposition of aluminum titanium alloy can only carry out in non-aqueous solution electrolysis plastidome.Electrochemical deposition aluminium closes
Gold system have: ion liquid system, inorganic fused salt system and three kinds of organic molten salt system, ion liquid system it is environmentally protective and
Energy-saving and emission-reduction, but it is expensive；Inorganic fused salt system is easy to operate and coating is uniformly solid, but energy consumption is higher and deposition efficiency compared with
It is low；Wherein organic solvent system is using earliest, most widely used system.Organic solvent system is easy to operate and prepared
Coating purity is high can be weakened and avoid under standard operation although the volatilization of this system is larger and inflammable and explosive.It is right
It generally uses in the electro-deposition of aluminum titanium alloy using aluminium chloride-titanium chloride as the organic solvent system of main salt, the system is at room temperature
It is able to achieve the preparation of aluminum titanium alloy, consumption reduction is beneficial to energy conservation, and make anode with using titanium silk, introduces titanium ion and compare, titanium ion
Concentration obtains certain raising.
Summary of the invention
The purpose of the present invention is to provide a kind of method that the electro-deposition of Organic Solvent at Room Temperature system prepares aluminum titanium alloy coating,
This method makees anode using graphite, obtains certain density titanium ion by adding anhydrous titanium tetrachloride, this method is at low cost, produces
Raw aluminum titanium alloy is pure and even particle size, Ti content are high.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of method that the electro-deposition of Organic Solvent at Room Temperature system prepares aluminum titanium alloy coating, prepared the method includes following
Journey:
(1) preparation of plating solution
In the closed glove box full of argon gas, the ratio for being 2:1 ~ 3:1 according to molar ratio weighs anhydrous aluminum chloride and hydrogen respectively
Change aluminium lithium；First benzene is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction；It is stirred with magnetic stirring apparatus again, and
Under conditions of ice bath, tetrahydrofuran solution is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction, this process is released a large amount of
Heat；In ventilating kitchen, the ratio for being 12:1 ~ 4:1 according to aluminium chloride and anhydrous titanium tetrachloride molar ratio, with the black needle being protected from light
Pipe measures anhydrous titanium tetrachloride；Under condition of ice bath, anhydrous titanium tetrachloride is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction
In；Under condition of ice bath, places it on magnetic stirring apparatus and be mixed 3 hours, the use ratio of the process benzene and tetrahydrofuran
Example is 4:1 ~ 4:3；
(2) Copper substrate is handled
Copper sheet is successively polished smooth with the sand paper of 400,800,1200 mesh, electrochemical deoiling is then carried out, removes copper sheet surface
Greasy dirt, then pre-etching and weak corrosion removing oxidation film are carried out with dilute sulfuric acid, it is then washed, vacuum oven is put into after washing
Middle drying, for use；
(3) constant current electro-deposition
Make anode with graphite, copper sheet makees cathode, and control current density is 6-38 milliamps per square centimeter, carries out electro-deposition, can obtain
Pure and even particle size aluminum titanium alloy is obtained, electrodeposition time control is 3 ~ 5 hours.
The advantages and effects of the present invention are:
The present invention obtains titanium ion by adding anhydrous titanium tetrachloride, makees anode with using titanium silk, introduces titanium ion and compares, titanium from
Sub- concentration obtains certain raising, while overcoming and preparing alloy, component segregation and nonuniform organization with ingot metallurgy technology, closes
The aurification period is long, and impurity is readily incorporated in alloy process, thus the problem of influencing the performance of material, aluminium titanium prepared by this method
Alloy is pure, even particle size and Ti content are higher.
Detailed description of the invention
Fig. 1 is sample SEM photo；
Fig. 2 is sample EDS energy spectrum analysis；
Fig. 3 is the XRD map of sample.
Specific embodiment
The following describes the present invention in detail with reference to examples.
A kind of embodiment of the method that the electro-deposition of Organic Solvent at Room Temperature system prepares aluminum titanium alloy coating is as follows,
Embodiment 1
(1) preparation of plating solution
In the closed glove box full of argon gas, 8.01 grams of anhydrous aluminum chlorides and 0.57 gram of lithium aluminium hydride reduction are weighed respectively；First by 40
Milliliter benzene is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction；It is stirred with magnetic stirring apparatus again, and in ice bath
Under conditions of, 10 milliliters of tetrahydrofuran solutions are slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction, this process is released a large amount of
Heat；In ventilating kitchen, 0.95 gram of anhydrous titanium tetrachloride is measured with the black needle tubing being protected from light；Under condition of ice bath, in closed environment,
Anhydrous titanium tetrachloride is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction.Under condition of ice bath, places it in magnetic force and stir
It mixes and is mixed 3 hours on device.
(2) Copper substrate is handled
Copper sheet is successively polished smooth with the sand paper of 400,800,1200 mesh, electrochemical deoiling is then carried out, removes copper sheet surface
Greasy dirt, then pre-etching and weak corrosion removing oxidation film are carried out with dilute sulfuric acid, it is then washed, vacuum oven is put into after washing
Middle drying, for use.
(3) constant current electro-deposition
Make anode with graphite, copper sheet makees cathode, and control current density is 9.3 milliamps per square centimeter, carries out electro-deposition, can obtain
Obtain pure and even particle size aluminum titanium alloy, main component AlTi3、Al5Ti2And Al3Ti, sample SEM photograph, EDS
Energy spectrum analysis and XRD spectrum are shown in Fig. 1, Fig. 2 and Fig. 3.
Embodiment 2
(1) preparation of plating solution
In the closed glove box full of argon gas, 8.01 grams of anhydrous aluminum chlorides and 0.57 gram of lithium aluminium hydride reduction are weighed respectively；First by 40
Milliliter benzene is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction；It is stirred with magnetic stirring apparatus again, and in ice bath
Under conditions of, 10 milliliters of tetrahydrofuran solutions are slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction, this process is released a large amount of
Heat；In ventilating kitchen, 1.45 grams of anhydrous titanium tetrachlorides are measured with the black needle tubing being protected from light；Under condition of ice bath, in closed environment,
Anhydrous titanium tetrachloride is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction.Under condition of ice bath, places it in magnetic force and stir
It mixes and is mixed 3 hours on device.
(2) Copper substrate is handled
Copper sheet is successively polished smooth with the sand paper of 400,800,1200 mesh, electrochemical deoiling is then carried out, removes copper sheet surface
Greasy dirt, then pre-etching and weak corrosion removing oxidation film are carried out with dilute sulfuric acid, it is then washed, vacuum oven is put into after washing
Middle drying, for use.
(3) constant current electro-deposition
Make anode with graphite, copper sheet makees cathode, and control current density is 9.3 milliamps per square centimeter, carries out electro-deposition, can obtain
Obtain pure and even particle size aluminum titanium alloy.
Embodiment 3
(1) preparation of plating solution
In the closed glove box full of argon gas, 8.01 grams of anhydrous aluminum chlorides and 0.57 gram of lithium aluminium hydride reduction are weighed respectively；First by 40
Milliliter benzene is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction；It is stirred with magnetic stirring apparatus again, and in ice bath
Under conditions of, 10 milliliters of tetrahydrofuran solutions are slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction, this process is released a large amount of
Heat；In ventilating kitchen, 2.95 grams of anhydrous titanium tetrachlorides are measured with the black needle tubing being protected from light；Under condition of ice bath, in closed environment,
Anhydrous titanium tetrachloride is slowly added into anhydrous aluminum chloride and lithium aluminium hydride reduction.Under condition of ice bath, places it in magnetic force and stir
It mixes and is mixed 3 hours on device.
(2) Copper substrate is handled
Copper sheet is successively polished smooth with the sand paper of 400,800,1200 mesh, electrochemical deoiling is then carried out, removes copper sheet surface
Greasy dirt, then pre-etching and weak corrosion removing oxidation film are carried out with dilute sulfuric acid, it is then washed, vacuum oven is put into after washing
Middle drying, for use.
(3) constant current electro-deposition
Make anode with graphite, copper sheet makees cathode, and control current density is 9.3 milliamps per square centimeter, carries out electro-deposition, can obtain
Obtain pure and even particle size aluminum titanium alloy.
Claims (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113802148A (en) * | 2021-11-02 | 2021-12-17 | 东北大学 | A kind of method for preparing aluminum-titanium alloy at low temperature by using ionic liquid |
| CN114059113A (en) * | 2021-12-16 | 2022-02-18 | 沈阳大学 | A kind of method for preparing aluminum-tin alloy coating by electrodeposition of organic solvent system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4148204A (en) * | 1971-05-07 | 1979-04-10 | Siemens Aktiengesellschaft | Process of mechanically shaping metal articles |
| CN105112963A (en) * | 2015-10-10 | 2015-12-02 | 东北大学 | Fused salt electrodeposition method for preparing metallic aluminum and metallic aluminum alloys |
| CN107974699A (en) * | 2017-11-10 | 2018-05-01 | 沈阳大学 | A kind of method that room temperature electro-deposition prepares aluminium/titanium alloy film |
-
2018
- 2018-09-20 CN CN201811097944.XA patent/CN109056007A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4148204A (en) * | 1971-05-07 | 1979-04-10 | Siemens Aktiengesellschaft | Process of mechanically shaping metal articles |
| CN105112963A (en) * | 2015-10-10 | 2015-12-02 | 东北大学 | Fused salt electrodeposition method for preparing metallic aluminum and metallic aluminum alloys |
| CN107974699A (en) * | 2017-11-10 | 2018-05-01 | 沈阳大学 | A kind of method that room temperature electro-deposition prepares aluminium/titanium alloy film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113802148A (en) * | 2021-11-02 | 2021-12-17 | 东北大学 | A kind of method for preparing aluminum-titanium alloy at low temperature by using ionic liquid |
| CN114059113A (en) * | 2021-12-16 | 2022-02-18 | 沈阳大学 | A kind of method for preparing aluminum-tin alloy coating by electrodeposition of organic solvent system |
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Application publication date: 20181221 |