CN105568345A - Method for metal plate anodizing - Google Patents
Method for metal plate anodizing Download PDFInfo
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- CN105568345A CN105568345A CN201610154289.1A CN201610154289A CN105568345A CN 105568345 A CN105568345 A CN 105568345A CN 201610154289 A CN201610154289 A CN 201610154289A CN 105568345 A CN105568345 A CN 105568345A
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- metal sheet
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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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 relates to the field of metal plate anodizing and discloses a method for metal plate anodizing. The method comprises the step of anodizing a metal plate by taking the metal plate as the anode, and taking 5%-15% by weight of sulfuric acid as an electrolytic solution. According to the technical scheme, the method can achieve the following technical effects that the production technique is simple and easy to operate; the developed electrolytic solution is low in cost and easy to prepare and has small influence on the environment and personal safety, and the coloring cost is greatly reduced; moreover, an obtained oxidation film is bright in color; substances such as an oxidation layer and grease on the surface are removed through preferable shot blasting treatment and/or degreasing treatment of the technique, on the one hand, the technique is more suitable for treating irregular parts and components, and on the other hand, the influence of residual liquid of degreasing liquid for traditional soaking or spray degreasing on subsequent surface treatment techniques is reduced, so that the effect that the irregular parts and components are used in the household appliance industry is made to be possible.
Description
Technical field
The present invention relates to the anodization of metal sheet, particularly, relate to the method for a kind of metal plate anode oxidation.
Background technology
Titanium or titanium alloy applies impressed current effect in corresponding electrolytic solution He under specific process conditions, and the process forming layer oxide film is on the surface of the workpiece called electrochemical oxidation, is also called anodic oxidation.The comprehensive row Performance Ratio of the rete that anodic oxidation obtains is better, and along with the difference of processing condition and oxidizing solution, the oxide film color obtained, thickness, and thickness also can difference to some extent.Its corrosion resistance nature of titanium alloy workpiece through electrochemical oxidation also can be greatly improved, and can improve the processing wettability of its high-temperature molding and tackyness and weather resistance.
But the oxide film color that existing technique is formed is comparatively dim, and outward appearance is not good.
Summary of the invention
The object of the invention is to overcome above defect, a kind of anodised method that can improve the vivid degree of oxide film is provided.
To achieve these goals, the invention provides the method for a kind of metal plate anode oxidation, wherein, the method comprises: with described metal sheet for anode, and the sulfuric acid of 5-15 % by weight is that electrolytic solution carries out anodic oxidation to described metal sheet.
Preferably, the method also comprises, before described anodic oxidation, Shot Blasting is carried out to described metal sheet, described Shot Blasting comprises: the particle using granularity to be less than or equal to 1mm carries out inject process to metal sheet, the metal sheet relative to every square metre, and the pressure of described injection is 1-4MPa.
Preferably, the method also comprises: carry out electrochemical polishing treatment to the metal sheet after inject process, and to remove the grease of metal sheet surface, wherein, the electrolytic solution of described electrochemical etching contains the sulfuric acid of 5-15 % by weight.
By technique scheme, following technique effect can be reached:
(1) the present invention uses production technique simple, easy to operate;
(2) this carries out titanium alloy sheet surface when carrying out anodised by this technique, and the electrolytic solution developed is cheap, easily prepares, and affects less, significantly reduce painted cost to environment and personnel safety.And gained oxide film is bright in colour;
(3) by after the Shot Blasting of this optimal process and/or skimming treatment, remove the material such as surface oxide layer, grease, on the one hand, make the process of this technique irregularity component preferably, on the other hand, decrease tradition soak or the degreasing liquid residual liquid of spray degreasing on the impact of sequent surface treatment process, be that irregular component use and become possibility in household electric appliances;
(4) to climb steel titanium, climb steel and start rolling titanium section product from 2010, design annual output 10000 tons of production capacities, if 3000 tons of titanium plates can be produced every year by this explained hereafter household electrical appliances component, with titanium plate profit 5000 yuan calculating per ton, the new returns of this technology are shown in shown in following formula (ten thousand yuan);
The benefit that Y-uses this process for treating surface to produce every year;
The profit on sales of A-titanium sheet metal per ton: 5000 yuan/ton;
The tonnage of the titanium plate that the annual household electric appliances of T-use: 3000 tons;
Then: Y=A × T=3000 × 5000=1500 (ten thousand yuan).
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, is used from explanation the present invention, but is not construed as limiting the invention with embodiment one below.In the accompanying drawings:
Fig. 1 is the picture on the titanium plate surface without any process.
Fig. 2 is the picture on the titanium plate surface after the inject process of a kind of embodiment of the application.
Fig. 3 is the picture on the titanium plate surface after the electrochemical polishing treatment of a kind of specific embodiments of the present invention.
Fig. 4 is the color of the oxide film that the titanium plate surface after using method of the present invention to carry out anodic oxidation under different voltage is formed.
Fig. 5 is the color of the oxide film that the titanium plate surface after using the method for reference to carry out anodic oxidation under different voltage is formed.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
On the one hand, the invention provides the method for a kind of metal plate anode oxidation, the method comprises: with described metal sheet for anode, and the sulfuric acid of 5-15 % by weight is that electrolytic solution carries out anodic oxidation to described metal sheet.
The present inventor finds in the process of research, and by metal sheet is carried out anodic oxidation treatment in the sulfuric acid electrolyte of 5-15 % by weight, the color of the oxide film formed is comparatively bright-coloured compared to existing electrolyte system color.
Preferably, described sulfuric acid is the dilute sulphuric acid of 8-12 % by weight.
Although use dilute sulphuric acid can realize object of the present invention as electrolytic solution, also be, improve the brightness of anodic oxidation gained oxide film, and make oxide film more firm, but the present inventor finds, by anodised condition is controlled under direct current condition, the area ratio of described anodised negative electrode and anode is 1-5:1, be preferably 1-3:1, temperature is 20-35 DEG C, and be preferably 25-30 DEG C, the time is 100-300s, be preferably 150-200s, the as above characteristic of gained oxide film can be promoted further.
According to the present invention, under electrolyte system of the present invention and anodic oxidation condition, when voltage changes between 5V to 70V, the color of gained oxide film can red to watermelon again to micro-Huang again to blueness again to redness from micro-Huang change, bright in color, outward appearance is all good.Therefore, the present invention is preferred for anodised voltage is 5-70V.
According to the present invention, in anodised process, in order to avoid making solution temperature raise due to chemical heat release, and be convenient to system diffusion further evenly, described anodic oxidation is preferably carried out under the condition stirred.Speed the present invention of described stirring has no particular limits, as long as can not destroy formed oxide film, preferably, the speed of described stirring is 50-100rpm.
According to the present invention, the method comprises: before anodic oxidation, and the particle using granularity to be less than or equal to 1mm carries out inject process to metal sheet, the metal sheet relative to every square metre, and the pressure of described injection is 1-4MPa.
Adopt Shot Blasting of the present invention, effectively can remove surface oxidation film, decrease traditional HF solution immersion and on the person and the impact of environment, be more suitable for irregular component; Also be the anodised voltage that reduces simultaneously, thus reduce energy consumption and cost.
Preferably, the condition of process makes the roughness of gained metal sheet surface be 1.5-0.8 μm.
The present inventor finds in the process of research, by the particle using granularity to be not more than 1mm, inject process is carried out to metal sheet, and, metal sheet relative to every square metre, controlling particle is 1-4MPa to the pressure that metal sheet is broken, the composition (such as, corrosion or other pollutents) that the zone of oxidation etc. can effectively removing its surface undesirably exists, reaches the polished finish of metal sheet surface.And the metal sheet after this process can reach homogeneous roughness and gloss.Preferred further, described pressure is 1.5-3MPa.
According to the present invention, described particle is preferably the grains of sand or steel ball.
Although carry out inject process according to mode as above to metal sheet can realize object of the present invention, but the discovery that the present inventor is surprising in the process of research, by particle being set to the particle diameter of 3 kinds of different stages, the surface contamination of the metal sheet after process can be removed further, and the roughness on surface and gloss more homogeneous, thus be more conducive to follow-up anodic oxidation treatment.Wherein, preferably, the granularity of volume particle size particle is 0.6-0.8mm, and the granularity of middle grain particles is 0.2-0.5mm, and the granularity of small size particle is 0.1-0.15mm.
According to the present invention, in as above preferred situation, the ratio of volume particle size particle, middle grain particles and small size particle can adjust in wider scope, in further preferred situation, ratio shared by the particle of middle granularity is maximum, and more preferably greater than the summation of small grain size and volume particle size particle proportion.Highly preferred, the ratio of described volume particle size particle, middle grain particles and small size particle is 1:(3-6): (0.5-1.2), is preferably 1:(4-5): (0.65-1).In this preferred situation, the pollutent (such as, zone of oxidation) of described metal sheet surface can obtain removing more thoroughly, make the roughness of metal sheet surface and gloss more homogeneous.
According to the present invention, the order of dishing out of the particle of different grain size scope too much restriction, and they can dish out simultaneously, successively can dish out according to the size of particle diameter yet.Use volume particle size particle to process metallic surface in the ban, when the processing metallic surface of particle of in use granularity and small grain size, the performance of the metal sheet obtained can be promoted further.
According to the present invention, metal sheet relative to every square metre, the density of described particle also can be selected in wider scope, but the factor such as the comprehensive polishing effect to metal sheet and destructiveness is considered, metal sheet relative to every square metre, the density of dishing out of described particle is 60-95kg.
According to the present invention, preferably, the present invention also comprises the step that the metal sheet after to inject process is washed, and described washing can be the purging method of this area routine, such as, can adopt the method for soaking and/or spraying.Preferred further, the method for described washing is by least 3 washings, and wherein, first time is spray washing, and second time is soaking and water washing, and third time is spray washing.Wherein, the temperature of described washing is preferably 65-75 DEG C, and for spray washing, the pressure of described spray is preferably 1-1.5MPa, and for soaking and water washing, the time of immersion is preferably 5-10min.
Surface due to metal parts is almost unavoidable will attach greasy dirt.Greasy dirt has three types, i.e. mineral oil, vegetables oil and animal oil.According to the chemical property of grease, can be divided into again: saponified oil and not saponifiable oil.All animal oil and the chemical composition of vegetables oil mainly lipid acid and glyceryl ester, owing to can generate soap with alkali effect, therefore is referred to as saponifiable oil; The chemical composition of mineral oil is various hydrocarbon polymers, can not and alkali reaction, therefore claim not saponifiable oil.Conventional degreasing method has: organic solvent degreasing, chemical degreasing and electrochemical degreasing.In the process of research, the present inventor finds further, because metallic surface is irregular, tradition degreasing mode there will be other positions " ponding " or " hydrops " phenomenon, degreasing fluid is caused to deposit, affect follow-up various facing operation, the present inventor finds further, before anodic oxidation, by carrying out electrochemical polishing treatment to the metal sheet after inject process, and select described electrolytic solution for containing 5-15 % by weight, the electrolytic solution of the sulfuric acid of preferred 8-12 % by weight, greatly can improve defect as above, and anodised voltage can be reduced further.
According to the present invention, the condition of described metal sheet being carried out to electrochemical etching can be the electrochemical etching condition of this area routine, and such as, the time of electrochemical etching is 120-250s, and voltage is 1-10V, and current density is 0.35-0.65A/cm
2.Preferred further, the time of described electrochemical etching is 150-220s, and voltage is 3-8V, and current density is 0.45-0.55A/cm
2.
According to the method for degreasing of the present invention, when metal parts immerses electrolyzer, the interfacial tension between oil and electrolytic solution dilute sulphuric acid can reduce greatly, and oil film just creates crackle.Meanwhile, because energising makes polarization of electrode, the surface tension of electrode and electrolytic solution reduces, and solution increases the wettability of metallic surface, and solution just and cracks discontinuous from oil film produces exclusion effect to oil film.Method of the present invention is preferably negative electrode degreasing, also, sample as negative electrode, negative electrode release hydrogen: 4H
2o+4e
-→ 2H
2↑+4OH
-.Wherein, hydrogen is overflowed with the form of a large amount of small bubbles, strong stirring and effect of impact are produced to solution, so oil film is torn be dispersed into a lot of tiny oil droplets, meanwhile, small bubbles are easily trapped in again on oil droplet, when bubble parameters is to certain size, can rise to solution surface with little oil droplet.Thus effective surface finish process achieved metal sheet.
According to the present invention, the anode for as above negative electrode degreasing can be various inert anode well known in the art, such as, and graphite, platinum etc.
According to the present invention, preferably, the present invention also comprises the step that the metal sheet after to electrochemical polishing treatment is washed, and described washing can be the purging method of this area routine, such as, can adopt the method for soaking and/or spraying.Preferred further, the method for described washing is by least 3 washings, and wherein, first time is spray washing, and second time is soaking and water washing, and third time is spray washing.
According to the present invention, described metal sheet can need for any the metal sheet removing the composition that surface oxide layer etc. undesirably exists, and such as, can be titanium plate, titanium alloy sheet etc.
According to the present invention, the thickness of described metal sheet is preferably greater than 2mm.
Below will be described the present invention by embodiment.
Embodiment 1
The present embodiment is for illustration of anodised method provided by the invention
(1) inject process
Be that the irregularity titanium plate of 5mm is put into shot-blasting machine and carried out Shot Blasting by thickness, the granularity of loading 15% in shot-blasting machine is the steel ball of 0.8mm, the granularity of 75% is the pill of 0.3mm, the granularity of 10% is the pill of 0.1mm, wherein, metal sheet relative to every square metre, the pressure of ball blast is 2MPa, and the density of particle is 70kg.Wherein, first carry out the inject process of volume particle size particle, then carry out the inject process of particle of middle granularity and small grain size.The roughness on the rear titanium plate surface of process is between 1.0-0.8 μm after measured.
(2) purifying treatment 1
Titanium plate after step (1) being processed carries out washing 3 times, and wherein, first time and third time are spray irrigation, and water temperature is 70 DEG C, and hydraulic pressure is 1MPa, and for the second time for immersion is washed, wherein, water temperature is 70 DEG C, and soak time is 5min;
Wherein, the surface of the titanium plate before inject process as shown in Figure 1, spray and the surface of titanium plate after washing as shown in Figure 2.
(3) skimming treatment
Titanium plate after step (2) being washed is negative electrode, and the dilute sulfuric acid solution with 10 % by weight is electrolytic solution, and graphite is that anode carries out electrochemical etching 180s, and wherein, voltage is 5V, and current density is 0.5A/cm
2.
(4) water-washing step of repeating step (2), obtains the titanium plate after polished finish of the present invention.Titanium plate surface after skimming treatment as shown in Figure 3.
(5) the titanium plate of step (4) gained is inserted in the dilution heat of sulfuric acid of 10 % by weight of 27 DEG C, with described titanium plate for anode, graphite is negative electrode, and the area ratio arranging negative electrode and anode is 1:1, volts DS changes between 5-70V, at the condition anodic oxygen 180s that 70rpm stirs.
Wherein, the oxide film color of described formation is vivid, and color red to watermelon again to micro-Huang again to blueness again to redness from micro-Huang change, the color of the anode oxide film formed between 5-47V voltage is as shown in Figure 4.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 2
The present embodiment is for illustration of anodised method provided by the invention
(1) inject process
Be that the irregularity titanium plate of 8mm is put into shot-blasting machine and carried out Shot Blasting by thickness, the granularity of loading 17% in shot-blasting machine is the steel ball of 0.6mm, the granularity of 68% is the pill of 0.4mm, the granularity of 15% is the pill of 0.15mm, wherein, metal sheet relative to every square metre, the pressure of ball blast is 3MPa, and the density of particle is 65kg.Wherein, first carry out the inject process of volume particle size particle, then carry out the inject process of particle of middle granularity and small grain size.The roughness on the rear titanium plate surface of process is between 1.2-1.0 μm after measured.
(2) purifying treatment 1
Titanium plate after step (1) being processed carries out washing 3 times, and wherein, first time and third time are spray irrigation, and wherein, water temperature is 65 DEG C, and hydraulic pressure is 1.2MPa, and for the second time for immersion is washed, wherein, water temperature is 75 DEG C, and soak time is 8min;
(3) skimming treatment
Titanium plate after step (2) being washed is negative electrode, and the dilute sulfuric acid solution with 8 % by weight is electrolytic solution, and graphite is that anode carries out electrochemical etching 220s, and wherein, voltage is 3V, and current density is 0.55A/cm
2.
(4) water-washing step of repeating step (2), obtains the titanium plate after polished finish of the present invention.
(5) the titanium plate of step (4) gained is inserted in the dilution heat of sulfuric acid of 12 % by weight of 25 DEG C, with described titanium plate for anode, graphite is negative electrode, and the area ratio arranging negative electrode and anode is 2:1, volts DS changes between 5-70V, at the condition anodic oxygen 200s that 50rpm stirs.
Wherein, the oxide film color of described formation is vivid, and color red to watermelon again to micro-Huang again to blueness again to redness from micro-Huang change.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 3
The present embodiment is for illustration of anodised method provided by the invention
(1) inject process
Be that the irregularity titanium plate of 2mm is put into shot-blasting machine and carried out Shot Blasting by thickness, the granularity of loading 15% in shot-blasting machine is the steel ball of 0.65mm, the granularity of 70% is the pill of 0.2mm, the granularity of 15% is the pill of 0.1mm, wherein, the pressure of ball blast is 1.5MPa, the metal sheet relative to every square metre, and the density of particle is 70kg.Wherein, first carry out the inject process of volume particle size particle, then carry out the inject process of particle of middle granularity and small grain size.The roughness on the rear titanium plate surface of process is between 1.3-1.1 μm after measured.
(2) purifying treatment 1
Titanium plate after step (1) being processed carries out washing 3 times, and wherein, first time and third time are spray irrigation, and wherein, water temperature is 75 DEG C, and hydraulic pressure is 1.0MPa, and for the second time for immersion is washed, wherein, water temperature is 65 DEG C, and soak time is 5min.
(3) skimming treatment
Titanium plate after step (2) being washed is negative electrode, and the dilute sulfuric acid solution with 12 % by weight is electrolytic solution, and graphite is that anode carries out electrochemical etching 150s, and wherein, voltage is 8V, and current density is 0.45A/cm
2.
(4) water-washing step of repeating step (2), obtains the titanium plate after polished finish of the present invention.
(5) the titanium plate of step (4) gained is inserted in the dilution heat of sulfuric acid of 8 % by weight of 30 DEG C, with described titanium plate for anode, graphite is negative electrode, and the area ratio arranging negative electrode and anode is 3:1, volts DS changes between 5-70V, at the condition anodic oxygen 150s that 100rpm stirs.
Wherein, the oxide film color of described formation is vivid, and color red to watermelon again to micro-Huang again to blueness again to redness from micro-Huang change.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 4
The present embodiment is for illustration of anodised method provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, the anodised time is 100s.The color of gained oxide film is very light, is close to disappearance.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 5
The present embodiment is for illustration of anodised method provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, the anodised time is 30min.The color of gained oxide film is very light.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 6
The present embodiment is for illustration of anodised method provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, described anodised temperature is 40 DEG C, and does not stir in the process of oxidation, and the area ratio of described anodised negative electrode and anode is 1:0.5.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 7
The present embodiment is for illustration of anodised method provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, described anodised temperature is 15 DEG C, and the area ratio of described anodised negative electrode and anode is 6:1.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 8
The present embodiment is for illustration of anodised method provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, in step (1), described particle is 2 kinds of different granularities, and wherein, 20%, the 0.4mm that occupies of 0.2mm occupies 80%.After measured after ball blast the roughness on titanium plate surface between 1.5-0.8 μm.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 9
The method that the present embodiment is oxidized for illustration of metal plate anode provided by the invention
Carry out the anodic oxidation of metal sheet surface according to the method for embodiment 1, all adopt first time for soaking and water washing unlike the washing in, step (2) and (4), second time and third time are spray washing.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 10
The method that the present embodiment is oxidized for illustration of metal plate anode provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, in step (1), first carry out the inject process of the particle of middle granularity and small grain size, then carry out the inject process of volume particle size particle.The roughness on the rear titanium plate surface of process is between 1.5-0.8 μm after measured.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 11
The method that the present embodiment is oxidized for illustration of metal plate anode provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, in step (3), described degreasing is gasoline degreasing.Also namely, soaked by the titanium plate of step after (2) process and carry out skimming treatment in the oil, the time of described immersion is 5min.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 12
The method that the present embodiment is oxidized for illustration of metal plate anode provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, the electrolytic solution in step (3) is the phosphoric acid of 10%.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 13
The method that the present embodiment is oxidized for illustration of metal plate anode provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, do not carry out the step of degreasing.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 14
The method that the present embodiment is oxidized for illustration of metal plate anode provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, do not carry out the step of Shot Blasting, but adopt polishing machine to carry out polished finish to metal sheet.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 15
The method that the present embodiment is oxidized for illustration of metal plate anode provided by the invention
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, between step (2) and (3), add the step that gasoline soaks, the time of described immersion is 5min.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 16
The method of the metal plate anode oxidation that the present embodiment provides for illustration of reference
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, in the steel ball of use, the granularity of large-size particles is 2mm.The roughness on the rear titanium plate surface of process is between 1.9-0.8 μm after measured.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 17
The method of the metal plate anode oxidation that the present embodiment provides for illustration of reference
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, the spraying pressure of steel ball is 0.5MPa.The roughness on the rear titanium plate surface of process is between 1.5-0.4 μm after measured.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 18
The method of the metal plate anode oxidation that the present embodiment provides for illustration of reference
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, the spraying pressure of steel ball is 5MPa.The roughness on the rear titanium plate surface of process is between 2.5-1.3 μm after measured.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Embodiment 19
The method of the metal plate anode oxidation that the present embodiment provides for illustration of reference
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, the electrolytic solution in step (3) is the electrolytic solution containing 500g/L dehydrated alcohol, 400gg/L lactic acid, 88g/L perchloric acid and 7.5g/L sodium perchlorate.Required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Comparative example 1
The method of the metal plate anode oxidation that this comparative example provides for illustration of reference
The anodic oxidation of metal sheet surface is carried out according to the method for embodiment 1, unlike, the sodium hydroxide solution for 10g/L used.Wherein, the color of the anode oxide film formed between 5-47V voltage as shown in Figure 5.Required voltage when record oxide film is red, required voltage when record oxide film is red, and record the shading value of gained oxide film, the results are shown in Table 1.
Test case 1
Use the aberration of vancometer (German BYK) to the red oxidization film that as above embodiment 1-19 is formed to measure, wherein, the numerical value between any two points is less than 4 and thinks qualified, and numerical value is about little shows that aberration is less.Test result is as shown in table 1.
Test case 2
For the red oxidization film obtained, by the 180 ° of doublings of titanium plate, whether then use plastic, transparent adhesive tape to paste at folding line place, detecting oxide film has obscission.The results are shown in Table 1.
Table 1
| Numbering | Aberration | Lightness | Voltage (V) | Whether qualified |
| Embodiment 1 | 0.8 | Bright | 15 | Do not come off |
| Embodiment 2 | 1.5 | Bright | 15 | Do not come off |
| Embodiment 3 | 1.3 | Bright | 15 | Do not come off |
| Embodiment 4 | 1.2 | Bright | 30 | Do not come off |
| Embodiment 5 | 1.5 | Bright | 26 | Do not come off |
| Embodiment 6 | 3.5 | Bright | 24 | Do not come off |
| Embodiment 7 | 3.9 | Bright | 25 | Do not come off |
| Embodiment 8 | 2.4 | Bright | 16 | Substantially do not come off |
| Embodiment 9 | 3.1 | Bright | 17 | Substantially do not come off |
| Embodiment 10 | 4.0 | Bright | 17 | Substantially do not come off |
| Embodiment 11 | 4.1 | Bright | 19 | A littlely to come off |
| Embodiment 12 | 3.8 | Bright | 18 | Substantially do not come off |
| Embodiment 13 | 4.7 | Bright | 22 | Come off |
| Embodiment 14 | 4.1 | Bright | 17 | A littlely to come off |
| Embodiment 15 | 0.5 | Bright | 14 | Do not come off |
| Embodiment 16 | 1.6 | Bright | 19 | Do not come off |
| Embodiment 17 | 3.4 | Bright | 20 | Substantially do not come off |
| Embodiment 18 | 2.1 | Bright | 19 | Do not come off |
| Embodiment 19 | 3.2 | Bright | 19 | Do not come off |
| Comparative example 1 | 1.1 | Secretly | 15 | Do not come off |
As can be seen from Table 1, the technical scheme of the application can improve the vivid degree of gained oxide film effectively, and in preferred scope, the aberration of gained oxide film can also be improved further, reduce and reach described in same color and need voltage, and avoid the situation such as to come off of oxide film.
Test case 3
The sensory evaluation of titanium plate surfaceness, glossiness and ponding situation
The senior personnel choosing 5 this areas carry out the evaluation of surfaceness and glossiness homogeneity to the titanium plate of embodiment 1-3, embodiment 8-19 and comparative example 1 before Anodic Oxidation, and the evaluation to ponding situation in the titanium plate after rinsing.Wherein, surfaceness, glossiness are very homogeneous is 5 points, and comparatively homogeneous is 4 points, is generally 3 points, and comparatively heterogeneity is 2 points, and very heterogeneity is 1 point.Be 5 points without ponding, carefully distinguish that slightly ponding is 4 points, ponding is visible as 3 points, and ponding is much 2 points, and it is 1 point that ponding overflows.Net result calculates with the average often organized, and the results are shown in Table 2.
Table 2
| Roughness | Glossiness | Ponding situation | |
| Embodiment 1 | 4.6 | 4.7 | 4.9 |
| Embodiment 2 | 4.6 | 4.6 | 4.7 |
| Embodiment 3 | 4.5 | 4.8 | 4.7 |
| Embodiment 8 | 4.3 | 4.2 | 4.1 |
| Embodiment 9 | 4.6 | 4.6 | 4.5 |
| Embodiment 10 | 3.9 | 4.0 | 3.8 |
| Embodiment 11 | 4.5 | 4.5 | 3.5 |
| Embodiment 12 | 4.3 | 4.4 | 3.2 |
| Embodiment 13 | 4.0 | 3.9 | 2.8 |
| Embodiment 14 | 4.0 | 3.9 | 3.0 |
| Embodiment 15 | 4.9 | 5.0 | 5.0 |
| Embodiment 16 | 3.5 | 3.3 | 3.4 |
| Embodiment 17 | 2.8 | 2.5 | 3.8 |
| Embodiment 18 | 3.0 | 4.0 | 2.5 |
| Embodiment 19 | 4.1 | 4.0 | 3.9 |
Test case 4
The evaluation of titanium polishing surface plate situation is carried out according to following step
The first step: be immersed in by sample in distilled water, leaves standstill 2 minutes;
Second step: taken out from distilled water by sample, whether complete half-twist, observe moisture film, if moisture film is complete, and do not break for a long time, and card polishing is comparatively successful.The record integrity of moisture film and moisture film are at the rupture event of 1min, 5min, 10min, 20min and 30min.The results are shown in Table 3.
Table 3
| Whether moisture film is complete | 1min | 5min | 10min | 20min | 30min | |
| Embodiment 1 | Be | N | N | N | N | N |
| Embodiment 2 | Be | N | N | N | N | N |
| Embodiment 3 | Be | N | N | N | N | N |
| Embodiment 8 | Be | N | N | N | N | Y |
| Embodiment 9 | Be | N | N | N | Y | |
| Embodiment 10 | Be | N | N | N | Y | |
| Embodiment 11 | Be | N | N | N | Y | |
| Embodiment 12 | Be | N | N | N | Y | |
| Embodiment 13 | Be | N | Y | |||
| Embodiment 14 | Be | N | N | Y | ||
| Embodiment 15 | Be | N | N | N | N | N |
| Embodiment 16 | Be | N | N | Y | ||
| Embodiment 17 | Be | Y | ||||
| Embodiment 18 | Be | N | N | Y | ||
| Embodiment 19 | Be | N | N | N | Y |
Note: wherein, N is not for break, and Y is for breaking.
Can be found out by table 2-3 as above, in the preferred case, the roughness on pre-processing titanium plate surface, glossiness can also be taken into account, skimming treatment ponding problem can also be solved.Further, the dead angle place that can penetrate into metal sheet due to method of the present invention carries out polishing, therefore, is particularly suitable for the process of irregularity component.
Fig. 1-3 as the application can find out, adopts technical scheme of the present invention effectively can remove the zone of oxidation on titanium mesh surface, and when further preferably degreasing, the titanium plate surface obtained more smooth homogeneous, color is brighter.In addition, as Fig. 4-5 can find out, adopt the electrolytic solution of the application to carry out the color of the oxide film that anodic oxidation obtains brighter, and adopt existing NaOH electrolyte carry out anodic oxidation the color of oxide film comparatively dim.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each the concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode.In order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (13)
1. a method for metal plate anode oxidation, the method comprises: with described metal sheet for anode, and the sulfuric acid of 5-15 % by weight is that electrolytic solution carries out anodic oxidation to described metal sheet.
2. method according to claim 1, wherein, described anodised condition comprises: under direct current condition, and the area ratio of described anodised negative electrode and anode is 1-5:1, and anodised temperature is 20-35 DEG C, and the time is 100-300s.
3. according to the method in claim 1-3 described in any one, wherein, described anodised voltage is 5-70V.
4. according to the method in claim 1-3 described in any one, wherein, described anodic oxidation is carried out under the condition stirred.
5. according to the method in claim 1-4 described in any one, wherein, the method also comprises, before described anodic oxidation, Shot Blasting is carried out to described metal sheet, described Shot Blasting comprises: the particle using granularity to be less than or equal to 1mm carries out inject process to metal sheet, the metal sheet relative to every square metre, and the pressure of described injection is 1-4MPa.
6. method according to claim 4, wherein, described particle is by the granulometric composition of 3 kinds of granularities, and the granularity of volume particle size particle is 0.6-0.8mm, and the granularity of middle grain particles is 0.2-0.5mm, and the granularity of small size particle is 0.1-0.15mm.
7. method according to claim 6, wherein, the ratio of described volume particle size particle, middle grain particles and small size particle is 1:3-6:0.5-1.2.
8. according to the method in claim 5-7 described in any one, wherein, the metal sheet relative to every square metre, the density of described particle is 60-95kg.
9. method according to claim 5, wherein, first carries out the inject process of volume particle size particle, then carries out the inject process of particle of middle granularity and small grain size.
10. according to the method in claim 5-9 described in any one, wherein, the method also comprises: carry out electrochemical polishing treatment to the metal sheet after inject process, to remove the grease of metal sheet surface, wherein, the electrolytic solution of described electrochemical etching contains the sulfuric acid of 5-15 % by weight.
11. methods according to claim 10, wherein, the time of described electrochemical etching is 120-250s, and voltage is 1-10V, and current density is 0.35-0.65A/cm
2;
Preferably, the time of described electrochemical etching is 150-220s, and voltage is 3-8V, and current density is 0.45-0.55A/cm
2.
12. according to the method in claim 5-11 described in any one, wherein, the metal sheet after the method also comprises the metal sheet after by the inject process in claim 5-9 described in any one and/or the electrochemical polishing treatment described in claim 10 or 11 carries out the step of washing.
13. according to the method in claim 1-12 described in any one, and wherein, described metal sheet is titanium plate and/or titanium alloy sheet, and preferably, the thickness of described metal sheet is greater than 2mm.
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| CN108301029A (en) * | 2018-01-31 | 2018-07-20 | 沈阳建筑大学 | A kind of titanium alloy anode oxidation coloring process |
| CN108796581A (en) * | 2018-08-03 | 2018-11-13 | 南方科技大学 | Titanium-based material colored drawing device and titanium-based material colored drawing method |
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