CN103122475B - A kind of aluminium alloy electric chemical brightening solution and a kind of aluminium alloy electric chemically polishing method - Google Patents
A kind of aluminium alloy electric chemical brightening solution and a kind of aluminium alloy electric chemically polishing method Download PDFInfo
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Abstract
The invention discloses a kind of aluminium alloy electric chemical brightening solution, this polishing fluid is the aqueous solution containing sodium hydroxide and disodium ethylene diamine tetraacetate; With the total amount of polishing fluid for benchmark, described sodium hydrate content is 8.3-15g/L, and described disodium ethylene diamine tetraacetate content is 9-18g/L, and surplus is water.The invention also discloses a kind of aluminium alloy electric chemically polishing method, the method is anode with Al alloy parts, take stainless steel plate as negative electrode, and described anode and negative electrode are placed in electropolishing liquid, carries out electrochemical etching, and described polishing fluid is polishing fluid provided by the invention.Aluminium alloy electric chemical rightenning liquid formula chromium-free environment-friendly provided by the invention, cost is low, good operational environment.
Description
Technical field
The invention relates to a kind of electrochemical polish liquid and a kind of electrochemical polishing method, particularly relate to a kind of aluminium alloy electric chemical brightening solution and a kind of aluminium alloy electric chemically polishing method.
Background technology
The method of existing conventional alkali electrochemical polishing is Brytal(Bu Laitafa) method, the alkaline tank liquor of this method is made up of sodium carbonate and tertiary sodium phosphate, and volts DS is at 12-16V, and service temperature is at 74-88 DEG C, and the electrochemical etching time is 5-20min.Comprise step: 1) pre-treatment: first take turns polishing with soft, then join alkali etching solution and carry out microcorrosion; 2) alkali etch treatment process: preparation 10%NaOH solution, temperature is 50 DEG C, process 20-30s; 3) electrochemical etching: join tank liquor (anhydrous Na2CO3 150g/L, Na3PO450g/L), temperature 80 DEG C, volts DS 15V, current density is 8A/dm2, process 8min; 4) aftertreatment: aluminium alloy moves on to tank washing at once, then moves on in the tank liquor of alkaline deoxidize, finally washes oven dry.5) demoulding technique: anhydrous Na2CO3 2%(Vol), Sodium chromate 5%(Vol) join groove, temperature 85 DEG C, process 2min.This method service temperature is high, chemical corrosion strong, aluminium loss is large, and solution easily lost efficacy, and seldom adopted at present.
What show domestic main employing is that three acid systems (Battelle method) process the polishing of Al alloy parts surface electrochemistry, and tank liquor is made up of phosphoric acid, sulfuric acid and chromic acid, and service temperature is at 70-90 DEG C.This method easily produces acid mist, and the waste water of discharge is containing heavy metal chromium, and solution toxicity is large, production cost is high, poor working environment.A kind of method of electropolishing aluminium alloy is disclosed in prior art, its component is sulfuric acid, phosphoric acid, aluminium, although polished to rafifinal, has lacked the effect of chromic acid ash disposal, and solution viscosity difficulty controls, and alloy surface burnt hair can be made even to turn black, produce pit to aluminium alloy polishing.Summary of the invention
For solving the problem that in prior art, Al alloy parts surface electrochemistry polished finish method production cost is high, environmental pollution is serious, operating environment is poor, the invention provides a kind of aluminium alloy electric chemical brightening solution, this polishing fluid is the aqueous solution containing sodium hydroxide and disodium ethylene diamine tetraacetate (EDTA-2Na); With the total amount of polishing fluid for benchmark, described sodium hydrate content is 8.3-15g/L, and described disodium ethylene diamine tetraacetate content is 9-18g/L, and surplus is water.
Present invention also offers a kind of aluminium alloy electric chemically polishing method, the method is anode with Al alloy parts, take stainless steel plate as negative electrode, and described anode and negative electrode are placed in electropolishing liquid, carries out electrochemical etching, and described polishing fluid is polishing fluid provided by the invention.
Aluminium alloy electric chemical rightenning liquid formula chromium-free environment-friendly provided by the invention, cost is low, good operational environment.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The invention provides a kind of aluminium alloy electric chemical brightening solution, this polishing fluid is the aqueous solution containing sodium hydroxide and disodium ethylene diamine tetraacetate.The aluminum ion that EDTA-2Na is dissolved out in order to complexing polishing, prevents the excessive hydrolysis of aluminum ion, keeps soltion viscosity good, makes aluminum alloy surface light simultaneously; Sodium hydroxide causes aluminium surface exposure in order to corrode aluminum alloy surface zone of oxidation, and then with aluminium surface, electrochemical reaction occurs, and forms mucous membrane on surface, controls convex-concave surface and removes speed, makes convex local dissolution rate faster, thus reduces surfaceness.The present inventor is found by a large amount of experiments, EDTA-2Na and sodium hydroxide is combined as polishing fluid basal liquid, improves the polishing effect of polishing fluid further.Aluminium alloy electric chemical brightening solution of the present invention, with the total amount of polishing fluid for benchmark, described sodium hydrate content is 8.3-15g/L, and described disodium ethylene diamine tetraacetate content is 9-18g/L, and surplus is water.
Preferably, also containing additive in polishing fluid of the present invention, with the total amount of polishing fluid for benchmark, described additive level is 1-5g/L.Described additive be selected from SODIUMNITRATE, sorbyl alcohol, trolamine, polyoxyethylene glycol, glycerine one or more.Above-mentioned additive, as ancillary reagents, mainly plays the effect of inhibition and promotion surface-brightening.
Preferably, also containing sodium sulphite in polishing fluid of the present invention, with the total amount of polishing fluid for benchmark, described sodium sulfide content is 0.05-1.5g/L.Sodium sulphite can reduce Zn content in solution, thus avoids occurring bright style defect, for the Al alloy parts better effects if that zinc content is higher.Here bright style defect refers to due to electropolishing liquid preferential etch and makes workpiece surface occur the phenomenon that crystal face glimmers, and is well known to a person skilled in the art technical terms.
Above obtain solution water used is water of the prior art, as one or the mixture of tap water, deionized water, pure water, distilled water.
Present invention also offers the polishing using method of above-mentioned aluminium alloy electric chemical brightening solution, an i.e. aluminium alloy electric chemically polishing method, the method is anode with Al alloy parts, take stainless steel plate as negative electrode, described anode and negative electrode are placed in electropolishing liquid, carry out electrochemical etching.
Preferably, described aluminium alloy electric chemically polishing method, use the pulse power, setting electrical parameter be voltage 180 ~ 270V, frequency 6 ~ 20KHz, dutycycle 10 ~ 40%, temperature at 40 ~ 60 DEG C, electropolishing 2-4min.Carry out electrochemical etching under this parameter after, the smooth effect of aluminum alloy surface light is best, and the tank liquor temperature of requirement is lower.
Further preferably, aluminium alloy electric chemically polishing method of the present invention, use the pulse power, setting electrical parameter be voltage 200 ~ 240V, frequency 10 ~ 15KHz, dutycycle 20 ~ 30%, temperature at 45 ~ 55 DEG C, electropolishing 2.5-3.5min.
Further preferably, aluminium alloy electric chemically polishing method of the present invention can also comprise step: carry out following process to before Al alloy parts polishing, Al alloy parts is immersed in Wax removal water, control temperature 65-80 DEG C of water bath with thermostatic control heated parts, then soaks in 65-80 DEG C of hot water.Wax removal water is generally meta-alkalescence PH7.0-7.5, is conducive to producing saponification reaction with the grease on workpiece, thus removes the grease of workpiece surface.The above treatment time can freely adjust, Al-alloy parts surface clean, and those skilled in the art freely can adjust according to practical situation, preferably can be: control temperature 65-80 DEG C of water bath with thermostatic control heated parts 1-4min, then soaks 20-30s in 65-80 DEG C of hot water.
Further preferably, aluminium alloy electric chemically polishing method of the present invention can also comprise step: carry out following process to after Al alloy parts polishing, Al alloy parts after polishing is washed 0.5-1min through 65-80 DEG C of hot water wash 1-2min, 60-70 DEG C of hot acid successively, and 1-4min washed by 65-80 DEG C of hot acid.The technical term that hot acid is known to the skilled person, generally refers to the solution of the acid being heated above room temperature, does not refer in particular to which kind of acid and which kind of concentration.Preferably, hot acid of the present invention refers to that temperature is at 60-80 DEG C, concentration 5-12%(VOL) the mixing solutions of sulfuric acid-acetic acid.
The above treatment time can freely adjust, Al-alloy parts surface clean, can be preferably: by the Al alloy parts after polishing successively through hot water wash 1-2min, 0.5-1min washed by hot acid, and 1-4min washed by hot acid.Preferably, above-mentioned hot water temperature is 65-80 DEG C, and hot acid temperature is 60-70 DEG C.
Preferably, aluminium alloy electric chemically polishing method of the present invention is described as: 1) carry out polishing pre-treatment to Al alloy parts; 2) Al alloy parts through pre-treatment is furnished with in polishing fluid of the present invention as anode immersion, imposes high-frequency narrow-pulse electric field and carry out plasma electric slurry polishing; 3) Al alloy parts after polishing washed through hot water wash, hot acid successively, after hot water wash, obtain the Al alloy parts that light is smooth.Wherein, the pre-treatment described in step 1) comprises the clean workpiece surface of use Wax removal water water bath with thermostatic control heating and hot water wash.Described Wax removal water is known in those skilled in the art, in order to remove surperficial foul (such as grease).Workpiece suspension to immerse by the present invention to be furnished with in the Wax removal water (PH is 7.0 ~ 7.5) that concentration is 5-10%, at 65-80 DEG C of water bath with thermostatic control heating 1-4 minute, then soaks 20-30s in 65 DEG C of-80 DEG C of hot water, obtains the Al alloy parts of clean surface.Preparation Wax removal water and washing step water used are water of the prior art, as one or the mixture of tap water, deionized water, pure water, distilled water.
According to the present invention, the formation condition of described hf and hv pulse electric field is: the direct impulse voltage of 180V ~ 270V, and pulse-repetition is 6-20KHz, and direct impulse dutycycle is 10-40%, continues 2-4min.
Further preferably, aluminium alloy electric chemically polishing method provided by the invention, strainer can also be set in each processing units, in order to filter during electricity is thrown compound precipitates and the meta-aluminate of the aluminium formed, be applicable to keep soltion viscosity and pre-process and post-process liquid clean, increase the service life, environmental protection.Here soltion viscosity is applicable to referring to soltion viscosity at 50-80cp.
Described electric slurry polishing is the polishing fluid Al alloy parts through pre-treatment being placed in alkalescence, and take Al alloy parts as anode, the stainless steel plate of polishing trough is negative electrode, and the spike pulse electric field imposing high-frequency and high-voltage carries out plasma electric slurry polishing.
Effects on surface is covered with impression, the coarse and shaping substrate of lusterless aluminium alloy carries out the Al alloy parts that plasma electric slurry polishing obtains having bright planarization effects.
The technology of the high voltagehigh frequency spike pulse that this technology uses, makes aluminum alloy surface obtain polishing effect better; Formula is not containing sexavalent chrome, and electricity throws the minute quantity heavy metal only having aluminium alloy stripping in waste liquid, and waste liquid easily processes, and does not pollute the environment; And because service temperature is low, corrodibility is little, do not produce alkali mist, Working environment is better; After treatment, workpiece surface light is smooth; Formula chromium-free environment-friendly, cost is low, good operational environment.Can not a step realize removing surface imperfection in prior art, will through the pre-treatment of mechanical polishing, and electricity is thrown the lower aluminium alloy of purity and be there will be that surperficial burnt hair even turns black, pitting attack serious, produce the defect of a large amount of pit, the present invention's formula a step can remove surface imperfection, realize the effect of aluminum alloy surface smooth. this formula overcomes the shortcoming of alkaline Brytal method, reduces service temperature, extend the work-ing life of solution, aluminium waste is few.
Below by embodiment, the present invention is further detailed.
Embodiment 1
The present embodiment is for illustration of polishing fluid disclosed by the invention and finishing method thereof.
Sodium hydroxide 8.0g/L, disodium ethylene diamine tetraacetate 8.5g/L, surplus is deionized water, is mixed with polishing fluid.Using aluminium alloy as anode, stainless steel plate is as negative electrode, and with above-mentioned polishing fluid for conducting medium, tank liquor temperature is 38 DEG C; Adjust electrical parameter: pulsed voltage is set to 175V, and frequency is set to 5KHz, and dutycycle is set to 8%, and pulse is set to positive pulse; Plasma electric slurry polishing 5min.Obtain Al alloy parts S1.
Embodiment 2
The present embodiment is for illustration of polishing fluid disclosed by the invention and finishing method thereof.
(a) pre-treatment: the Wax removal water of preparation 6% (Vol), thermostatically heating to 60 DEG C, hangs to be immersed by Al alloy parts and soaks 5min, take out; Soak in the deionized water of 60 DEG C, and stir 32s; Obtain the Al-alloy parts of surface clean.
B () electric slurry polishing: sodium hydroxide 8.3g/L, disodium ethylene diamine tetraacetate 9.0g/L, adds 2%(Vol) sorbyl alcohol and 1.2%(Vol) glycerine, surplus is deionized water, is mixed with polishing fluid.Using aluminium alloy good for pre-treatment as anode, stainless steel plate is as negative electrode, and with above-mentioned polishing fluid for conducting medium, tank liquor temperature is 50 DEG C; Adjust electrical parameter: pulsed voltage is set to 180V, and frequency is set to 10KHz, and dutycycle is set to 20%, and pulse is set to positive pulse; Plasma electric slurry polishing 3min.Obtain Al alloy parts S2.
Embodiment 3
The present embodiment is for illustration of polishing fluid disclosed by the invention and finishing method thereof.
(a) pre-treatment: the Wax removal water of preparation 6% (Vol), thermostatically heating to 65 DEG C, hung by Al alloy parts and be immersed, 4min is soaked in disturbance, takes out; Soak in the deionized water of 65 DEG C, and stir 15s; The above treatment time can freely adjust, Al-alloy parts surface clean.
B () electric slurry polishing: sodium hydroxide 12g/L, disodium ethylene diamine tetraacetate 18g/L, adds 0.05g/L sodium sulphite, 5%(Vol) sorbyl alcohol, surplus is deionized water, is mixed with polishing fluid.Using aluminium alloy good for pre-treatment as anode, stainless steel plate is as negative electrode, and with above-mentioned polishing fluid for conducting medium, tank liquor temperature is 60 DEG C; Adjust electrical parameter: pulsed voltage is set to 270V, and frequency is set to 6KHz, and dutycycle is set to 30%, and pulse is set to positive pulse; Plasma electric slurry polishing 2min.
(c) aftertreatment: the mixing solutions of preparation 8% (Vol) sulfuric acid and 5% (Vol) acetic acid, is heated to 60 DEG C.Workpiece after being thrown by electricity moves into rapidly in the deionized water of 60 DEG C and washes away, then moves in 60 DEG C of mixture heat acid solutions and wash away back and forth, then washes away in the deionized water of 80 DEG C, the above treatment time can freely adjust, till wash clean, finally dry up with pressurized air, obtain Al alloy parts S3.
Embodiment 4
The present embodiment is for illustration of polishing fluid disclosed by the invention and finishing method thereof.
(a) pre-treatment: the Wax removal water of preparation 8% (Vol), thermostatically heating to 70 DEG C, hangs to be immersed by Al alloy parts and soaks 3min, take out; Soak in the deionized water of 80 DEG C, and stir 20s; Time can freely adjust, Al-alloy parts surface clean.
B () electric slurry polishing: sodium hydroxide 15g/L, disodium ethylene diamine tetraacetate 15g/L, add 1.0g/L sodium sulphite, 0.91g/L sorbyl alcohol, 0.09g/L SODIUMNITRATE, surplus is deionized water, is mixed with polishing fluid.Using Al-alloy parts good for pre-treatment as anode, stainless steel plate is as negative electrode, and with above-mentioned polishing fluid for conducting medium, tank liquor temperature is 40 DEG C; Processing parameter is: pulsed voltage is set to 220V, and frequency is set to 20KHz, and dutycycle is set to 10%, and pulse is set to positive pulse; Plasma electric slurry polishing 4min.
(c) aftertreatment: the mixing solutions of preparation 10% (Vol) sulfuric acid and 5% (Vol) acetic acid, is heated to 65 DEG C and obtains mixture heat acid solution.Workpiece after being thrown by electricity moves into rapidly in the deionized water of 65 DEG C and washes away, then moves in 65 DEG C of mixture heat acid solutions and wash away back and forth, then washes away in the deionized water of 65 DEG C.The above treatment time can freely adjust, till wash clean.Finally dry up with pressurized air, obtain the Al alloy parts S4 that surface-brightening is smooth.
Embodiment 5
The present embodiment is for illustration of polishing fluid disclosed by the invention and finishing method thereof.
(a) pre-treatment: the Wax removal water of preparation 12% (Vol), thermostatically heating to 80 DEG C, hangs to be immersed by firm part and soaks 1min, take out; Soak in the deionized water of 70 DEG C, and stir 35s; The above treatment time can freely adjust, Al-alloy parts surface clean.
(b) electric slurry polishing: this step is identical with (b) electric slurry polishing step in embodiment 4.
(c) aftertreatment: the mixing solutions of preparation 10% (Vol) sulfuric acid and 8% (Vol) acetic acid, is heated to 80 DEG C and obtains mixture heat acid solution.Workpiece after being thrown by electricity moves into rapidly in the deionized water of 80 DEG C and washes away, then moves in 80 DEG C of mixture heat acid solutions and wash away back and forth, then washes away in the deionized water of 70 DEG C, time is not limit, till wash clean, finally dry up with pressurized air, obtain the Al alloy parts S5 that surface-brightening is smooth.
Embodiment 6
The present embodiment is for illustration of polishing fluid disclosed by the invention and finishing method thereof.
The present embodiment, compared with embodiment 5, lacks step (a); Step (b) is identical; And step (c) is different, difference is as follows:
(c) aftertreatment: the mixing solutions of preparation 10% (Vol) sulfuric acid and 8% (Vol) acetic acid, is heated to 70 DEG C and obtains mixture heat acid solution.Workpiece after being thrown by electricity moves into rapidly in the deionized water of 70 DEG C and washes away, then moves in 70 DEG C of mixture heat acid solutions and wash away back and forth, then washes away in the deionized water of 80 DEG C, time is not limit, till wash clean, finally dry up with pressurized air, obtain the Al alloy parts S6 that surface-brightening is smooth.
Comparative example 1
This comparative example is for illustration of existing disclosed polishing fluid and finishing method thereof.
Original Al alloy parts is done following process: the Wax removal water of preparation 8% (Vol), thermostatically heating to 70 DEG C, steel part is hung to be immersed and soaks 2min, take out; Soak in the deionized water of 70 DEG C, and stir, until clean up; Obtain the Al-alloy parts D1 of surface clean.
Comparative example 2
This comparative example is for illustration of existing disclosed polishing fluid base formulation technique and finishing method thereof.
(a) pre-treatment:
First take turns polishing with soft, 10%, 80 DEG C of Wax removal water degreasings, then join alkali etching solution and carry out microcorrosion, finally wash.Alkali etching solution microcorrosion treatment process: preparation 10%NaOH solution, temperature is 50 DEG C, process 25s.
(b) electrochemical etching:
Join tank liquor (anhydrous Na
2cO
3150g/L, Na
3pO
450g/L), tank liquor temperature 80 DEG C take Al alloy parts as anode, and stainless steel plate is negative electrode, volts DS 15V, and current density is 8A/dm2, process 8min.
(c) aftertreatment:
Al alloy parts after polishing is moved on at once tank washing, then move on in the tank liquor of alkaline deoxidize, finally wash oven dry, obtain the Al alloy parts D2 that surface-brightening is smooth.Demoulding technique: anhydrous Na
2cO
32%(Vol), Sodium chromate 5%(Vol) join groove, temperature 85 DEG C, process 2min.Obtain Al alloy parts D2
Above water washing process and the water configuring solution used are all deionized waters.
Performance test
Surfaceness
GB/T3505-2000 is adopted to carry out surfaceness test, measured by the TR200 Manual roughness devices of Beijing Time Incorporation.
Surface albedo
Adopt GB2680-1994 to carry out surface albedo test, the ETF-05A type surface albedo tester adopting Shenzhen to open special Science and Technology Ltd. measured.
Carry out performance test to Al alloy parts S1-6, D1-2, test result is as shown in the table:
| Sample number into spectrum | Ra（μm） | Surface albedo (%) |
| S1 | 0.071 | 70 |
| S2 | 0.055 | 80 |
| S3 | 0.049 | 83 |
| S4 | 0.030 | 90 |
| S5 | 0.036 | 90 |
| S6 | 0.042 | 87 |
| D1 | 0.932 | 30 |
| D2 | 0.056 | 82 |
Ra profile arithmetic average error, refers in sample length, the arithmetical av of profile offset distance absolute value.The planeness of the less presentation surface of Ra is better.
From upper table S1, S2, S3 test result, pre-treatment removes surperficial grease and booty, is conducive to the raising of the roughness of workpiece surface; And aftertreatment can prevent polishing unsalted surface Quick Oxidation out, aftertreatment is conducive to improving surface brightness; The test result of S1-6 and D1 is more known, and finishing method of the present invention can remove Al alloy parts surface imperfection largely, makes surfacing light, and very close to the effect of specular light; And the test result of S3-6 and D2 shows, utilize the Al-alloy parts surface brightness after the method for the invention and high-frequency narrow-pulse technology electric slurry polishing and roughness all good than existing base formulation.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. an aluminium alloy electric chemical brightening solution, is characterized in that, this polishing fluid is the aqueous solution containing sodium hydroxide and disodium ethylene diamine tetraacetate; With the total amount of polishing fluid for benchmark, described sodium hydrate content is 8.3-15g/L, and described disodium ethylene diamine tetraacetate content is 9-18g/L, and surplus is water;
Also containing additive in described polishing fluid, with the total amount of polishing fluid for benchmark, described additive level is 1-5g/L;
Described additive be selected from SODIUMNITRATE, sorbyl alcohol, trolamine, polyoxyethylene glycol, glycerine one or more;
Also containing sodium sulphite in described polishing fluid, with the total amount of polishing fluid for benchmark, described sodium sulfide content is 0.05-1.5g/L.
2. an aluminium alloy electric chemically polishing method, is characterized in that, the method take Al alloy parts as anode, take stainless steel plate as negative electrode, described anode and negative electrode are placed in electropolishing liquid, carry out electrochemical etching, described polishing fluid is polishing fluid according to claim 1.
3. electrochemical polishing method according to claim 2, is characterized in that, use the pulse power, setting electrical parameter be voltage 180-270V, frequency 6-20KHz, dutycycle 10-40%, temperature at 40-60 DEG C, electropolishing 2-4min.
4. electrochemical polishing method according to claim 3, is characterized in that, use the pulse power, setting electrical parameter be voltage 200-240V, frequency 10-15KHz, dutycycle 20-30%, temperature at 45-55 DEG C, electropolishing 2.5-3.5min.
5. the electrochemical polishing method according to any one of claim 2,3 or 4, it is characterized in that, also comprise step: carry out following process to before Al alloy parts polishing, Al alloy parts is immersed in Wax removal water, control temperature 65-80 DEG C of water bath with thermostatic control heated parts, then soak in 65-80 DEG C of hot water.
6. electrochemical polishing method according to claim 5, is characterized in that, also comprises step: carry out following process to after Al alloy parts polishing, and by the Al alloy parts after polishing successively through hot water wash, hot acid is washed, hot water wash.
7. electrochemical polishing method according to claim 6, is characterized in that, described hot water temperature is 65-80 DEG C, and described hot acid temperature is 60-70 DEG C.
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