CN107460534A - The electrochemical polish liquid and polishing method of a kind of titanium or titanium alloy - Google Patents
The electrochemical polish liquid and polishing method of a kind of titanium or titanium alloy Download PDFInfo
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- CN107460534A CN107460534A CN201710789294.4A CN201710789294A CN107460534A CN 107460534 A CN107460534 A CN 107460534A CN 201710789294 A CN201710789294 A CN 201710789294A CN 107460534 A CN107460534 A CN 107460534A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
- C25F3/26—Polishing of heavy metals of refractory metals
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Abstract
The invention discloses a kind of electrochemical polish liquid of titanium or titanium alloy and polishing method.Each component and its content are in the electrochemical polish liquid：The 40g/L of sodium chloride 10；Glycerine 40 70%；Ethylene glycol 20 40%；Absolute ethyl alcohol 5 20%；Perchloric acid 0.1 1%；The 5g/L of additive 1；The additive is made up of accelerator, leveling agent and brightener.The electrochemical polish liquid contained substance is environment-protecting and non-poisonous, and is generated in electrochemical polishing process without toxic gas；Titanium or titanium alloy workpiece is after electrochemical polish of the present invention, and bright luster is presented in surface, and its mean roughness can be with as little as below 10nm；The corrosive power of the electrolytic polishing liquid is weak, small to electrolysis installation corrosion, can utilize for a long time；The electrochemical polish liquid only requires supplementation with mother liquor, repeats and utilizes more than 500 times, stability is strong.
Description
Technical field
The invention belongs to metal process field, and in particular to a kind of electrochemical polish liquid applied to titanium and its titanium alloy and
Polishing method.
Background technology
Titanium or titanium alloy has a series of excellent characteristics such as density is small, corrosion resistance is good, specific strength is high, thus extensively
Applied to every field such as Aeronautics and Astronautics, medical treatment.But with various industrially to the continuous of titanium or titanium alloy surfacing requirement
Improve, prepare the smooth titanium or titanium alloy of surface-brightening and be just particularly important.
At present, titanium or titanium alloy is surface flattening a variety of methods, is broadly divided into mechanical polishing, chemical polishing and electrification
Three kinds of methods of optical polishing.
Mechanical polishing is to remove to be polished the convex portion of part and obtain the polishing of even surface by cutting, material surface plastic deformation
Method, but cut caused by mechanically polishing is very difficult to remove, while it is mingled with polish abrasive, and sample surfaces leave residual stress.
Chemical polishing is acid corrosion, refers to allow surface microscopic protrudes in chemical mediator part compared with the preferential dissolving of recess point,
So as to obtain even surface, used chemical mediator is generally the acid solution of hydrofluoric acid or fluoride ion.Due to titanium and titanium
Alloy substrate carries out that vigorous reaction, F can occur during chemical polishing processing-With Ti4+The complex compound of ion is very stable, can closely inhale
Titanium or titanium alloy surface is attached to, makes titanium or titanium alloy matrix and air exclusion, therefore titanium or titanium alloy matrix surface can not generate
Passivating film, this be also most of titanium or titanium alloy plating and other surface treatments be used as by the use of the solution corrosion of hydrofluoric acid containing before locate
The reason for reason.But hydrofluoric acid is a kind of highly toxic substance, highly volatile is known from experience to environment and people into air and produces huge danger
Evil.
Electrochemical polish be based on metal anode electrochemical dissolution principle make metal surface progressively reach it is microcosmic it is smooth plus
Work method, polished part inside and surface residual stress can be greatly reduced, and not limited by titanium or titanium alloy device shape, had
The advantages that high in machining efficiency, corrosion-resistant, its finish and flatness after polishing are more preferable than mechanically polishing.
The electrolytic polishing liquid document analysis for being currently used for polishing titanium or titanium alloy is as follows：
《The environmentally friendly electrochemical polishing process of titanium alloy》(in U.S., Xu Yongzhen etc., University of Science ＆ Technology, Beijing's journal, 2009,31
(1)：68-73) disclose it is a kind of containing perchloric acid, sodium perchlorate, lactic acid, absolute ethyl alcohol titanium alloy polishing fluid, but use the throwing
During the processing of light liquid, titanium alloy substrate surface easily generates oxide-film, and the oxidation film hardness is high, and polishing difficulty is big, titanium alloy table
Face is also easy to produce polishing lines, it is difficult to reaches mirror effect.
Patent CN101798702 discloses a kind of hydrofluoric acid containing 1-3wt%, 20-30wt% deionized waters, and surplus is second two
The electrolytic polishing liquid of alcohol, but the polishing fluid still can produce harm to human body, and it is strong to the corrosivity of electrobrightening equipment, no
Beneficial to long-term use, and by the accompanying drawing 3 in patent application document it can be seen that under 10 micrometer resolutions, its surface still has
Lines is polished, is not reaching to complete mirror effect.
Patent CN1358240 discloses the electrolytic polishing liquid that sulfur acid, hydrofluoric acid and acetum are formed, and as above institute be present
That states produces harm to human body, and to shop equipment seriously corroded, the defects of being unfavorable for factory's long-term use, and titanium after polishing
Alloy surface mean roughness reaches more than 57nm.
The polishing fluid of other not hydrofluoric acid containings, as used substantial amounts of alcohol solvent, volatility in patent CN101148774
It is larger and easily catch fire, it is not suitable for factory and largely uses；Methanesulfonic acid is used in patent US2008/0217186, its electrolyte has
Larger toxicity, does not meet environmental requirement；Acetic acid and perchloric acid mixed solution are used in patent CN102899711, in its electrolyte
Containing substantial amounts of perchloric acid, and temperature serious to equipment corrosion is too high easily to be set off an explosion, and the technique is also required in low temperature environment
Lower operation, condition is harsh, is industrially difficult to mass produce.
To sum up, there is complicated component in the electrolyte for being currently used for titanium or titanium alloy electrochemical polish, contain to environment or people more
The harmful material of body, it is more difficult to prepare, the problems such as technology stability difference and highly acid electrolyte serious to equipment corrosion.Therefore research and develop
Electrochemical polish electrolyte and electrochemical polishing process less toxic, safe efficient, stability is good, small to equipment corrosion has
Obvious meaning.
The content of the invention
The purpose of the present invention is the defects of being directed to existing titanium or titanium alloy electrochemical polish liquid, there is provided a kind of safety, it is simple,
Stable, repeatable utilization, the electrochemical polish liquid of the titanium or titanium alloy small to equipment corrosion.
In order to realize the purpose of the present invention, the present inventor is finally obtained as follows by lot of experiments research and unremitting effort
Technical scheme：A kind of electrochemical polish liquid of titanium or titanium alloy, each component and its content are in electrochemical polish liquid：
The additive is made up of accelerator, leveling agent and brightener.
Described accelerator is selected from least one of oxalic acid, citric acid and tartaric acid, and described leveling agent is selected from amino sulphur
At least one of acid, sulfosalicylic acid and urea, described brightener is glucose.
It is further preferred that the electrochemical polish liquid of titanium or titanium alloy of the present invention, each group in the electrochemical polish liquid
Divide and its content is：
It is further preferred that the electrochemical polish liquid of titanium or titanium alloy of the present invention, each group in the electrochemical polish liquid
Divide and its content is：
It is further preferred that the electrochemical polish liquid of titanium or titanium alloy of the present invention, each group in the electrochemical polish liquid
Divide and its content is：
It should be noted that the electrochemical polish liquid of the above-mentioned titanium or titanium alloy of the present invention, glycerine during it is formulated, ethylene glycol without
The content of water-ethanol and perchloric acid is percentage by volume, such as, " glycerine 40-70% " refers to that the volumetric usage of glycerine accounts for finally
The percentage for the electrochemical polish liquid cumulative volume being formulated.
It is further preferred that the electrochemical polish liquid of titanium or titanium alloy of the present invention, wherein described accelerator is grass
Acid and citric acid, described leveling agent are sulfosalicylic acid, and described brightener is glucose.
The present invention also provides the method for carrying out electrochemical polish to titanium or titanium alloy using above-mentioned electrochemical polish liquid, uses
Electrochemical polish liquid as described above is as electrolyte, and each component and its content are in the electrochemical polish liquid：40-70% is sweet
Oil, 20-40% ethylene glycol, 5-20% absolute ethyl alcohols, 0.1-1% perchloric acid, 10-40g/L sodium chloride and 1-5g/L additives, institute
Additive is stated to be made up of accelerator, leveling agent and brightener.
Specifically, the electrochemical polishing method comprises the following steps：
(1) pre-process：Dried with sand paper polishing titanium or titanium alloy workpiece and cleaning；
(2) pickling：Put the workpiece in immersion and cleaning, drying in acid solution；
(3) electrolytic polishing liquid is prepared：According to each component in electrochemical polish liquid and its content：40-70% glycerine, 20-
40% ethylene glycol, 5-20% absolute ethyl alcohols, 0.1-1% perchloric acid, the ratio of 10-40g/L sodium chloride and 1-5g/L additives are matched somebody with somebody
Electrolytic polishing liquid processed；
(4) electrochemical polish：It is completely submerged in workpiece as anode, pure titanium sheet as negative electrode in electrolytic polishing liquid, profit
Electrochemical polish is carried out with D.C. regulated power supply；
(5) polishing terminates rear cleaning workpiece and dried.
Polished workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively in step (1),
And carry out ultrasonic wave cleaning according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water.
The mix acid liquor that acid solution described in step (2) is prepared for hydrofluoric acid with nitric acid, HF in the mix acid liquor：
HNO3：The volume ratio of water is (2-4)：(8-13)：(85-90).
The parameter of electrochemical polish is in step (4)：Voltage 20-50V, polishing time 60-360s are polished, is electrolysed during polishing
Liquid mixing speed is 100-2000rpm.
The present invention has the following technical effect that relative to prior art：
(1) the electrochemical polish liquid contained substance is environment-protecting and non-poisonous, and is generated in electrochemical polishing process without toxic gas；
(2) titanium or titanium alloy workpiece is after electrochemical polish, and bright luster is presented in surface, and its mean roughness can be as little as
Below 10nm；
(3) use glycerol as solvent while there is the effect for the formation for promoting diffusion layer, ethanol can then reduce solution
Overall viscosity promotes each several part to dissolve each other each other, ethylenediamine increase solution polarity, while accelerates the anti-of polishing fluid and titanium or titanium alloy
Should, NaCl plays synergy after being organically combined between each other as electrolyte, each component so that the corrosion energy of electrolytic polishing liquid
Power is weak, small to electrolysis installation corrosion, can utilize for a long time；
(4) electrochemical polish liquid only requires supplementation with mother liquor, repeats and utilizes more than 500 times, stability is strong.
Brief description of the drawings
Fig. 1 is that pure titanium workpiece surface SEM schemes before electrochemical polish in the embodiment of the present invention 11；
Fig. 2 is that pure titanium workpiece surface SEM schemes after electrochemical polish in the embodiment of the present invention 11；
Fig. 3 is that pure titanium workpiece AFM schemes after electrochemical polish in the embodiment of the present invention 11.
Fig. 4 is that titanium alloy workpiece surface SEM schemes before electrochemical polish in the embodiment of the present invention 12；
Fig. 5 is that titanium alloy workpiece surface SEM schemes after electrochemical polish in the embodiment of the present invention 12；
Fig. 6 is that titanium alloy workpiece AFM schemes after electrochemical polish in the embodiment of the present invention 12；
Embodiment
The embodiment of the present invention is described further below, wherein being used in following embodiments 1-10,12-14
Titanium alloy workpiece pass through electrochemical polishing method step (1) pretreated sample for same titanium alloy sheet, its surface is put down
Equal surface roughness is 870nm, and the pure titanium workpiece used in embodiment 11 is by electrochemical polishing method step (1) pretreatment
Afterwards, its surface average surface roughness is 765nm.
Embodiment 1
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 400mL is measured, 400ml ethylene glycol, 200mL second are sequentially added under stirring condition
Alcohol, 1mL perchloric acid, 40g sodium chloride, 1g citric acids, 0.5g glucose and 0.5g urea, are uniformly mixing to obtain electrolytic polishing liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 30V is polished, 20 DEG C, electrobrightening 300s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 6.87nm after polishing.
Embodiment 2
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium metal work-pieces with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 400mL is measured, 400ml ethylene glycol, 200mL second are sequentially added under stirring condition
Alcohol, 1mL perchloric acid, 40g sodium chloride, 1g citric acids, 0.5g glucose and 0.5g urea, are uniformly mixing to obtain electrolytic polishing liquid；
(4) titanium metal work-pieces are completely submerged in electrolyte, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 30V is polished, 20 DEG C, electrobrightening 300s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 8.85nm after polishing.
Embodiment 3
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, measure glycerine 700mL, sequentially added under stirring condition 250ml ethylene glycol, 50mL ethanol,
10mL perchloric acid, 15g sodium chloride, 1g tartaric acid, 0.5g sulfamic acids and 0.5g glucose, are uniformly mixing to obtain electrobrightening
Liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 50V is polished, 0 DEG C, electrobrightening 180s of polish temperature, does not stop to stir in polishing process, mixing speed 2000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 7.29nm after polishing.
Embodiment 4
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 400mL is measured, 400ml ethylene glycol, 200mL second are sequentially added under stirring condition
Alcohol, 2mL perchloric acid, 50g sodium chloride, 0.5g tartaric acid, 0.5g oxalic acid, 0.5g citric acids, 0.5g sulfamic acids, 0.5g urea and
0.5g glucose, is uniformly mixing to obtain electrolytic polishing liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 20V is polished, 50 DEG C, electrobrightening 60s of polish temperature, does not stop to stir in polishing process, mixing speed 100rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 8.71nm after polishing.
Embodiment 5
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 500mL is measured, 400ml ethylene glycol, 100mL second are sequentially added under stirring condition
Alcohol, 5mL perchloric acid, 35g sodium chloride, 0.5g oxalic acid, 0.5g sulfosalicylic acids, 0.5g citric acids, 0.5g tartaric acid, 0.5g urea
With 0.5g glucose, electrolytic polishing liquid is uniformly mixing to obtain；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 20V is polished, 20 DEG C, electrobrightening 360s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 7.68nm after polishing.
Embodiment 6
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 700mL is measured, 200ml ethylene glycol, 100mL second are sequentially added under stirring condition
Alcohol, 10mL perchloric acid, 10g sodium chloride, 0.5g oxalic acid, 0.5g sulfosalicylic acids, 0.5g tartaric acid and 0.5g glucose, stirring are equal
It is even to obtain electrolytic polishing liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 30V is polished, 25 DEG C, electrobrightening 120s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 6.95nm after polishing.
Embodiment 7
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 600mL is measured, 250ml ethylene glycol, 150mL second are sequentially added under stirring condition
Alcohol, 5mL perchloric acid, 20g sodium chloride, 1.0g oxalic acid, 0.5g citric acids, 0.5g sulfosalicylic acids and 0.5g glucose, stirring are equal
It is even to obtain electrolytic polishing liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 40V is polished, 20 DEG C, electrobrightening 360s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 5.63nm after polishing.
Embodiment 8
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 450mL is measured, 400ml ethylene glycol, 150mL second are sequentially added under stirring condition
Alcohol, 1mL perchloric acid, 12g sodium chloride, 1.5g tartaric acid, 0.5g sulfamic acids and 0.5g glucose, it is uniformly mixing to obtain electrolysis and throws
Light liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 50V is polished, 0 DEG C, electrobrightening 180s of polish temperature, does not stop to stir in polishing process, mixing speed 2000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 8.24nm after polishing.
Embodiment 9
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 700mL is measured, 200ml ethylene glycol, 100mL second are sequentially added under stirring condition
Alcohol, 10mL perchloric acid, 40g sodium chloride, 2.0g tartaric acid, 1.0g sulfamic acids and 1.0g glucose, are uniformly mixing to obtain electrolysis
Polishing fluid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 50V is polished, 0 DEG C, electrobrightening 180s of polish temperature, does not stop to stir in polishing process, mixing speed 2000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 6.53nm after polishing.
Embodiment 10
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 650mL is measured, 250ml ethylene glycol, 100mL second are sequentially added under stirring condition
Alcohol, 4mL perchloric acid, 35g sodium chloride, 1.0g oxalic acid, 1.0g citric acids, 1.5g sulfosalicylic acids and 1.0g glucose, stirring are equal
It is even to obtain electrolytic polishing liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 40V is polished, 20 DEG C, electrobrightening 360s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 4.37nm after polishing.
Embodiment 11
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium metal work-pieces with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 500mL is measured, 350ml ethylene glycol, 150mL second are sequentially added under stirring condition
Alcohol, 7mL perchloric acid, 16g sodium chloride, 0.5g oxalic acid, 0.5g citric acids, 0.5g sulfosalicylic acids and 0.3g glucose, stirring are equal
It is even to obtain electrolytic polishing liquid；
(4) titanium metal work-pieces are completely submerged in electrolyte, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 40V is polished, 20 DEG C, electrobrightening 360s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
As depicted in figs. 1 and 2, the workpiece respectively after step (1) processing is schemed with workpiece surface SEM after step (5) processing
Picture, workpiece after polishing is observed, its surface is in obvious bright luster, carries out AFM analyses to workpiece after polishing, obtains such as Fig. 3
Shown AFM analysis charts, it is known that the mean roughness of the workpiece is 5.46nm after polishing.
Embodiment 12
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 580mL is measured, 310ml ethylene glycol, 110mL second are sequentially added under stirring condition
Alcohol, 6mL perchloric acid, 28g sodium chloride, 1.0g oxalic acid, 1.5g sulfosalicylic acids, 0.5g tartaric acid and 0.8g glucose, stirring are equal
It is even to obtain electrolytic polishing liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 30V is polished, 25 DEG C, electrobrightening 120s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
As shown in Figure 4 and Figure 5, the workpiece respectively after step (1) processing is schemed with workpiece surface SEM after step (5) processing
Picture, workpiece after polishing is observed, its surface is in obvious bright luster, carries out AFM analyses to workpiece after polishing, obtains such as Fig. 6
Shown AFM analysis charts, it is known that the mean roughness of the workpiece is 1.92nm after polishing.
Embodiment 13
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 550mL is measured, 320ml ethylene glycol, 130mL second are sequentially added under stirring condition
Alcohol, 4mL perchloric acid, 23g sodium chloride, 0.5g oxalic acid, 0.5g sulfosalicylic acids, 0.5g tartaric acid and 0.5g glucose, stirring are equal
It is even to obtain electrolytic polishing liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 30V is polished, 25 DEG C, electrobrightening 120s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and the mean roughness of the workpiece is 2.54nm after polishing.
Embodiment 14
A kind of titanium or titanium alloy workpiece electrochemical polishing method, in turn includes the following steps：
(1) polished titanium alloy workpiece with the abrasive paper for metallograph of 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh successively,
Ultrasonic wave cleaning is carried out to workpiece according to the order of deionized water, acetone, absolute ethyl alcohol and deionized water after polishing；
(2) according to HF：HNO3：H2O volume ratio is 3：10：87 ratio prepares mix acid liquor, and workpiece is placed in into the acid solution
Middle immersion 1min, taking-up are dried after being rinsed well with deionized water；
(3) using glycerine as solvent, glycerine 600mL is measured, 300ml ethylene glycol, 100mL second are sequentially added under stirring condition
Alcohol, 5mL perchloric acid, 30g sodium chloride, 1.0g citric acids, 0.5g oxalic acid, 1.0g sulfosalicylic acids and 0.5g glucose, stirring are equal
It is even to obtain electrolytic polishing liquid；
(4) titanium alloy workpiece is totally submerged in the electrolytic solution, electrochemical polish is carried out using D.C. regulated power supply, wherein
Voltage 30V is polished, 25 DEG C, electrobrightening 120s of polish temperature, does not stop to stir in polishing process, mixing speed 1000rpm；
(5) workpiece is taken out after polishing terminates and cleans surface with a large amount of deionized waters and dries.
Workpiece after polishing shows obvious bright luster, finds to utilize the electrochemical polish work through micro- sem observation
Artistic skill enough removes substantially cut and impurity of titanium alloy surface etc., and its average surface roughness is 1.78nm.
Comparative example 1
5 kinds of electrolytic polishing liquids are prepared respectively：
Prepare electrolytic polishing liquid 1：Glycerine containing 590mL, 300mL ethylene glycol, the anhydrous second of 110mL in every liter of electrolytic polishing liquid
Alcohol, 6mL perchloric acid, 28g sodium chloride, 0.5g oxalic acid, 0.8g citric acids, 1.0g sulfosalicylic acids, 2.0g glucose.
Prepare electrolytic polishing liquid 2：Electrolytic polishing liquid is made up of glycerine, absolute ethyl alcohol and sodium chloride, every liter of electrolytic polishing liquid
In 845mL containing glycerine, absolute ethyl alcohol 160mL, sodium chloride 28g, then without other materials.
Prepare electrolytic polishing liquid 3：Ethylene glycol containing 725mL, 265mL absolute ethyl alcohols, the high chlorine of 15mL in every liter of electrolytic polishing liquid
Acid, 0.5g oxalic acid, 0.8g citric acids, 1.0g sulfosalicylic acids, 2.0g glucose, then without other materials.
Prepare electrolytic polishing liquid 4：Ethanol containing 340mL, 7mL perchloric acid, 660mL glycerine in every liter of electrolytic polishing liquid, then nothing
Other materials.
Prepare electrolytic polishing liquid 5：Ethylene glycol containing 980mL in every liter of electrolytic polishing liquid, 30mL perchloric acid, 0.5g oxalic acid,
0.8g citric acids, 1.0g sulfosalicylic acids, 2.0g glucose, then without other materials.
Respectively by 5 titanium alloy workpieces of identical component and specification according to the processing step and parameter of embodiment 14 at
Reason, only 5 kinds of electrolytic polishing liquids that the electrolyte in the step of embodiment 14 (3) is prepared with comparative example 1 respectively are replaced respectively.
The titanium alloy workpiece of 5 identical components and specification is after electrochemical polishing method step (1) pretreatment, its surface
Average surface roughness is respectively 885nm, 908nm, 875nm, 892nm and 864nm, respectively in order by electrolytic polishing liquid 1,
After electrolytic polishing liquid 2, electrolytic polishing liquid 3, electrolytic polishing liquid 4 and electrolytic polishing liquid 5 are handled, its surface average roughness is divided successively
Wei not 1.87nm, 620nm, 378nm, 583nm and 657nm.
Claims (10)
- A kind of 1. electrochemical polish liquid of titanium or titanium alloy, it is characterised in that：Each component and its content in the electrochemical polish liquid For：The additive is made up of accelerator, leveling agent and brightener.
- 2. the electrochemical polish liquid of titanium or titanium alloy according to claim 1, it is characterised in that：Described accelerator is selected from grass At least one of acid, citric acid and tartaric acid, described leveling agent is at least one in sulfamic acid, sulfosalicylic acid and urea Kind, described brightener is glucose.
- 3. the electrochemical polish liquid of titanium or titanium alloy according to claim 2, it is characterised in that：It is each in the electrochemical polish liquid Component and its content are：
- 4. the electrochemical polish liquid of titanium or titanium alloy according to claim 3, it is characterised in that：It is each in the electrochemical polish liquid Component and its content are：
- 5. the electrochemical polish liquid of titanium or titanium alloy according to claim 4, it is characterised in that：It is each in the electrochemical polish liquid Component and its content are：
- 6. the electrochemical polish liquid of any one of the claim 1-5 titanium or titanium alloy, it is characterised in that：Described accelerator is Oxalic acid and citric acid, described leveling agent are sulfosalicylic acid, and described brightener is glucose.
- A kind of 7. electrochemical polishing method of titanium or titanium alloy, it is characterised in that：Using electrochemical polish liquid as electrolyte, each component and its content are in the electrochemical polish liquid：40-70% is sweet Oil, 20-40% ethylene glycol, 5-20% absolute ethyl alcohols, 0.1-1% perchloric acid, 10-40g/L sodium chloride and 1-5g/L additives, institute Additive is stated to be made up of accelerator, leveling agent and brightener.
- 8. the electrochemical polishing method of titanium or titanium alloy according to claim 7, it is characterised in that in turn include the following steps：(1) pre-process：Dried with sand paper polishing titanium or titanium alloy workpiece and cleaning；(2) pickling：Put the workpiece in immersion and cleaning, drying in acid solution；(3) electrolytic polishing liquid is prepared：According to each component in electrochemical polish liquid and its content：40-70% glycerine, 20-40% second The ratio preparation of glycol, 5-20% absolute ethyl alcohols, 0.1-1% perchloric acid, 10-40g/L sodium chloride and 1-5g/L additives is electrolysed Polishing fluid；(4) electrochemical polish：Using workpiece as anode, pure titanium sheet is completely submerged in electrolytic polishing liquid as negative electrode, using straight Flow voltage-stabilized power supply and carry out electrochemical polish；(5) polishing terminates rear cleaning workpiece and dried.
- 9. the electrochemical polishing method of titanium or titanium alloy according to claim 8, it is characterised in that：Described in step (2) Acid solution is the mix acid liquor that hydrofluoric acid and nitric acid are prepared, HF in the mix acid liquor：HNO3：The volume ratio of water is (2-4)： (8-13)：(85-90).
- 10. the electrochemical polishing method of titanium or titanium alloy according to claim 8, it is characterised in that：Electrochemistry in step (4) The parameter of polishing is：Voltage 20-50V, polishing time 60-360s are polished, electrolyte mixing speed is 100- during polishing 2000rpm。
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| CN108360059A (en) * | 2018-04-24 | 2018-08-03 | 东北大学 | A kind of electrochemical polish liquid and polishing method of the special-shaped titanium alloy of laser gain material manufacture |
| CN108796597A (en) * | 2018-06-06 | 2018-11-13 | 重庆大学 | A kind of Al/Ti cold rolling composite plates electrolytic polishing method |
| CN109972193A (en) * | 2019-04-21 | 2019-07-05 | 山东理工大学 | A kind of polishing fluid and method of Nitinol pipe electrobrightening |
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