CN103436922B - Utilize ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould - Google Patents
Utilize ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould Download PDFInfo
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- CN103436922B CN103436922B CN201310388232.4A CN201310388232A CN103436922B CN 103436922 B CN103436922 B CN 103436922B CN 201310388232 A CN201310388232 A CN 201310388232A CN 103436922 B CN103436922 B CN 103436922B
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Abstract
Utilize ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould, relate to microprism. Preparation electroforming solution: add hot water in electrotyping bath, add successively again six hydration nickel sulfate, nickel chloride, in container, add hot water, after adding again boric acid, boil, then add lauryl sodium sulfate, after dissolving, pour in electrotyping bath, in electrotyping bath, add asccharin and 1,4-butynediols, the water that reinjects is filled it up with electrotyping bath, and regulating pH is 4.2; Anode nickel plates is put into anode basket access positive pole, by grand master pattern access negative pole processed nickel, carry out electroforming, after the negative electrode demoulding, obtain high reflectance microprism reflective membrane Working mould. Can utilize easily aborning supersonic cleaning machine to regulate ultrasound parameter; Can control by adjusting ultrasound parameter and formulation of electroforming solution the retro-reflecting coefficient of microsize microprism reflective membrane Working mould.
Description
Technical field
The present invention relates to microprism, especially relate to and a kind ofly utilize ultrasonic electroforming to prepare high reflectance microprism reflective membrane Working mouldMethod.
Background technology
Stir under electroforming process condition in common mechanical, electroformed nickel can only obtain more coarse surface, and its reflex reflection performance is not high.Microprism reflective membrane is that the pyramid array of tens micron dimensions forms, and cannot after processing, carry out other machine glazed finishes. Reflective membraneRequire Working mould to there is very high retro-reflecting coefficient, namely must after electroforming, just obtain high reflectance.
Nickel is a kind of common electroforming and plated material, is widely used with its superperformance, most research be electroplate liquid formulation,Electroplating device, direct current electroforming and Deposit appearance aspect, less for the research of ultrasonic electroforming, for electroforming surface retro-reflecting coefficientThe research of height has no report. Nickel is applied to the work of microprism reflective membrane with characteristics such as the high and higher hardness of its chemical stabilityMould.
For ultrasonic electroforming, there is the data to show to utilize hyperacoustic mechanical disturbance effectiveness and cavitation effect, greatly improve electroforming solutionMass transfer effect, effectively reduces concentration polarization. Meanwhile, the energy that ultrasonic cavitation produces has reduced electrode surface metal ionReduction potential energy, reduced critical nucleus radius, thereby improved nucleation rate. In addition, micro-at cavitation HTHP and high speedUnder jet impingement function, deposit to the broken compared with coarse grain of cathode surface, formed less nucleus (Liu Lanbo, Wu MengChina, Wang Yuangang, etc. the ultrasonic-impact of pulse electroforming technological parameter on nickel cast layer crystallite dimension. mechanical engineering material, 2012,3:22-25). In addition, there is data to show that the ultrasonic agitation sound intensity is 12～14W/cm2Time, nickel micro element buildup, pin hole etc. that electroforming goes outDefect is few, and the angle of collapsing, round edge phenomenon obviously reduce, surfacing (Ming Pingmei, Zhu Di, Hu Yangyang, etc. ultrasonic micro electroforming examinationTest research. China Mechanical Engineering, 2008,6:644-647). But for microprism reflective membrane Working mould, except controlling castingLayer grain size and defect are how many, more require to obtain the high reflectance in cast layer surface.
Summary of the invention
The object of the invention is to the problems such as the reflectance for restive its reflective membrane Working mould of existing microprism, provide onePlanting utilizes ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould.
The present invention includes following steps:
1) preparation electroforming solution, its concrete grammar is as follows:
In electrotyping bath, add hot water, then add successively six hydration nickel sulfate, nickel chloride, in container, add hot water, then addAfter boric acid, boil, then add lauryl sodium sulfate, after dissolving, pour in electrotyping bath, to add in electrotyping bath asccharin and Isosorbide-5-Nitrae-Butynediols, the water that reinjects is filled it up with electrotyping bath, and regulating pH is 4.2;
2) anode nickel plates is put into anode basket access positive pole, by grand master pattern access negative pole processed nickel, carried out electroforming, through the negative electrode demouldingAfter obtain high reflectance microprism reflective membrane Working mould.
In step 1), the temperature of described hot water can be 50～60 DEG C, is preferably 55 DEG C; Described six hydration nickel sulfate, chlorinationThe addition of nickel, boric acid, lauryl sodium sulfate, asccharin and Isosorbide-5-Nitrae-butynediols can be (6000～12000) in mass ratio:(600～1400): (600～1500): (1～20): (2～20): (4～10); Described six hydration nickel sulfateQuality-volumetric concentration can be 300～600g/L, and the quality-volumetric concentration of nickel chloride can be 30～70g/L, the quality-body of boric acidVolume concentrations can be 30～75g/L, and the quality-volumetric concentration of lauryl sodium sulfate can be 0.05～1g/L, the quality-body of asccharinVolume concentrations can be 0.1～1g/L, and the quality-volumetric concentration of Isosorbide-5-Nitrae-butynediols can be 0.2～0.5g/L; The described time of boilingCan be 30～50min, be preferably 40min; Described adjusting pH is that 4.2 can to adopt quality-volumetric concentration be 30% sulfuric acid solutionRegulate, regulate pH can at 45～55 DEG C, be incubated 8～12h after 4.2, be preferably at 50 DEG C and be incubated 10h.
In step 2) in, it is 4～10A/dm that the condition of described electroforming can be current density2, ultrasonic power is 210～300W, frequentlyRate is 30～50kHz, and the time of electroforming is 2～4h.
Prepared high reflectance microprism reflective membrane Working mould goods can, after washed with de-ionized water is dried, be used retro-reflecting coefficient instrumentMeasure its retro-reflecting coefficient, with observation by light microscope and take a picture.
The invention has the advantages that:
1) can utilize easily aborning supersonic cleaning machine to regulate ultrasound parameter;
2) preferred suitable formulation of electroforming solution.
3) while preparing microsize microprism reflective membrane Working mould in nickelous sulfate electroforming solution, control the method for retro-reflecting coefficient, canControl the retro-reflecting coefficient of microsize microprism reflective membrane Working mould by adjusting ultrasound parameter and formulation of electroforming solution.
4) measure its retro-reflecting coefficient through retro-reflecting coefficient instrument, with observation by light microscope and take a picture and show, existing machinery stirsThe microprism reflective membrane Working mould reflectance of mixing electroforming is not high, and the high reflectance microprism reflective membrane work that adopts the present invention to prepareMould has obtained high reflectance in certain parameter situation.
Brief description of the drawings
Fig. 1 is existing mechanical agitation electroforming microprism reflective membrane Working mould micrograph.
Fig. 2 is high reflectance microprism reflective membrane Working mould micrograph prepared by the present invention.
Detailed description of the invention
Embodiment 1
Electroforming solution preparation: according to the total measurement (volume) of electrotyping bath, weigh respectively nickelous sulfate 450g, nickel chloride 50g, boric acid 50g, tenSodium dialkyl sulfate 0.07g, asccharin 0.5g and Isosorbide-5-Nitrae-butynediols 0.35g. Electrotyping bath adds deionized water, is heated to 50DEG C, add successively load weighted nickelous sulfate, nickel chloride, stirring and be incubated 4h. Separately get beaker deionized water rinsing, drying,Add deionized water, be stirred and heated to boiling, add load weighted boric acid to boil 0.5h, then add lauryl sodium sulfate,After lauryl sodium sulfate is fully dissolved, it is slowly poured in electrotyping bath, and add asccharin and butynediols in casting groove,Add again deionized water to being full of electrotyping bath, fully stir, at 45 DEG C of insulation 12h, measure its pH value with pH test paper, use30% sulfuric acid solution is adjusted to pH=4.2. Ensure the quality of products-volumetric concentration of casting liquid: nickelous sulfate 450g/L, nickel chloride 50g/L, boronAcid 50g/L, lauryl sodium sulfate 0.07g/L, asccharin 0.5g/L, butynediols 0.35g/L.
The pre-treatment of anode and negative electrode: anode nickel plates is put into hydrochloric acid 25min, and surface is fully after activation, rushes by deionized waterWash clean. Cathode nickel mould first carries out sensitization 6s with tin chloride solution, rinses well by deionized water; Potassium bichromate is moltenLiquid is evenly sprayed at cathode surface 6s, carries out Passivation Treatment, rinses well afterwards by deionized water; Putting into nitric acid 5min entersRow surface passivation, then deionized water rinsing.
Electroforming: nickel plate is put into anode basket access positive pole, through the nickel microprism reflective membrane processed grand master pattern access negative pole of pre-treatment,Adjusting current density is 4A/dm2, adjusting ultrasonic power is 240W, frequency is 40kHz, carries out electroforming 4h.
The demoulding: take out negative electrode and carry out the demoulding, Working mould is fully rinsed by deionized water, dry.
Measure retro-reflecting coefficient: the retro-reflecting coefficient of touching with retroreflective marking measuring instrument and vehicle body reflection mark measuring instrument surveying workBe respectively 1448 and 1470cdlx-1·m-2, and the Working mould retro-reflecting coefficient that common mechanical stirring electroforming obtains is respectively 820And 851cdlx-1·m-2。
Microexamination: at optical microphotograph Microscopic observation Working mould, and take a picture. Fig. 2 obtains the high reflectance of microprism reflective membraneWorking mould. Can find out from Fig. 1 and 2, the microprism reflective membrane Working mould reflectance of existing mechanical agitation electroforming is not high (to be seenFig. 1), adopt ultrasonic electroforming in certain parameter situation, to obtain the Working mould (see figure 2) of high reflectance.
Embodiment 2
Nickelous sulfate electroforming solution preparation: according to the total measurement (volume) of electrotyping bath, first weigh nickelous sulfate 300g, nickel chloride 30g, boric acid 30g,Lauryl sodium sulfate 0.05g, asccharin 0.1g and Isosorbide-5-Nitrae-butynediols 0.2g. Electrotyping bath adds deionized water, is heated to 55 DEG C,Add successively load weighted nickelous sulfate, nickel chloride, stirring and be incubated 3.5h. Separately get beaker deionized water rinsing, drying,Add deionized water, be stirred and heated to boiling, add load weighted boric acid to boil 40min, then add lauryl sodium sulfate,After lauryl sodium sulfate is fully dissolved, it is slowly poured in electrotyping bath, and add asccharin and butynediols in casting groove,Add again deionized water to being full of electrotyping bath, fully stir, at 50 DEG C of insulation 10h, measure its pH value with pH test paper, use30% sulfuric acid solution is adjusted to pH=4.2. Ensure the quality of products-volumetric concentration of casting liquid: nickelous sulfate 300g/L, nickel chloride 30g/L, boronAcid 30g/L, lauryl sodium sulfate 0.05g/L, asccharin 0.1g/L, butynediols 0.2g/L.
The pre-treatment of anode and negative electrode: anode nickel plates is put into hydrochloric acid 25min, and surface is fully after activation, rushes by deionized waterWash clean. Cathode nickel mould first carries out sensitization 7s with tin chloride solution, rinses well by deionized water; Potassium bichromate is moltenLiquid is evenly sprayed at cathode surface 6s, carries out Passivation Treatment, rinses well afterwards by deionized water. Putting into nitric acid 5min entersRow surface passivation, then deionized water rinsing.
Electroforming: nickel plate is put into anode basket access positive pole, through the nickel microprism reflective membrane processed grand master pattern access negative pole of pre-treatment,Adjusting current density is 7A/dm2, adjusting ultrasonic power is 210W, frequency is 50kHz, carries out electroforming 3h.
The demoulding: take out negative electrode and carry out the demoulding, Working mould is fully rinsed by deionized water, dry.
Measure retro-reflecting coefficient: the retro-reflecting coefficient of touching with retroreflective marking measuring instrument and vehicle body reflection mark measuring instrument surveying workBe respectively 1421 and 1463cdlx-1·m-2。
Embodiment 3
Nickelous sulfate electroforming solution preparation: according to the total measurement (volume) of electrotyping bath, first weigh nickelous sulfate 600g, nickel chloride 70g, boric acid 75g,Lauryl sodium sulfate 1g, asccharin 1g and Isosorbide-5-Nitrae-butynediols 0.5g. Electrotyping bath adds the deionized water of 1/2 volume, heatingTo 60 DEG C, add successively load weighted nickelous sulfate, nickel chloride, stirring and be incubated 3h. Separately get a deionized water rinsing for beaker,Dry, add deionized water, be stirred and heated to boiling, add load weighted boric acid to boil 50min, then add dodecylSodium sulphate, after lauryl sodium sulfate is fully dissolved, slowly pours it in electrotyping bath into, and adds asccharin and fourth in casting grooveAcetylenic glycols, then add deionized water to being full of electrotyping bath, fully stirs, and at 55 DEG C of insulation 8h, measures its pH with pH test paperValue, is adjusted to pH=4.2 with 30% sulfuric acid solution. Ensure the quality of products-volumetric concentration of casting liquid: nickelous sulfate 600g/L, nickel chloride 70g/L,Boric acid 75g/L, lauryl sodium sulfate 1g/L, asccharin 1g/L, butynediols 0.5g/L.
The pre-treatment of anode and negative electrode: anode nickel plates is put into hydrochloric acid 25min, and surface is fully after activation, rushes by deionized waterWash clean. Cathode nickel mould first carries out sensitization 6s with tin chloride solution, rinses well by deionized water; Potassium bichromate is moltenLiquid is evenly sprayed at cathode surface 7s, carries out Passivation Treatment, rinses well afterwards by deionized water. Putting into nitric acid 5min entersRow surface passivation, then deionized water rinsing.
Electroforming: nickel plate is put into anode basket access positive pole, through the nickel microprism reflective membrane processed grand master pattern access negative pole of pre-treatment,Adjusting current density is 10A/dm2, adjusting ultrasonic power is 300W, frequency is 30kHz, carries out electroforming 2h.
The demoulding: take out negative electrode and carry out the demoulding, Working mould is fully rinsed by deionized water, dry.
Measure retro-reflecting coefficient: the retro-reflecting coefficient of touching with retroreflective marking measuring instrument and vehicle body reflection mark measuring instrument surveying workBe respectively 1436 and 1449cdlx-1·m-2。
Claims (7)
1. utilize ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould, it is characterized in that comprising the following steps:
1) preparation electroforming solution, its concrete grammar is as follows:
In electrotyping bath, add hot water, then add successively six hydration nickel sulfate, nickel chloride, in container, add hot water, then addAfter boric acid, boil, then add lauryl sodium sulfate, after dissolving, pour in electrotyping bath, to add in electrotyping bath asccharin and Isosorbide-5-Nitrae-Butynediols, the water that reinjects is filled it up with electrotyping bath, and regulating pH is 4.2; Described six hydration nickel sulfate, nickel chloride, boric acid, 12The addition of sodium alkyl sulfate, asccharin and Isosorbide-5-Nitrae-butynediols is (6000～12000) in mass ratio: (600～1400):(600～1500): (1～20): (2～20): (4～10); Quality-the volumetric concentration of described six hydration nickel sulfate is300～600g/L, the quality-volumetric concentration of nickel chloride is 30～70g/L, the quality-volumetric concentration of boric acid is 30～75g/L,Quality-the volumetric concentration of lauryl sodium sulfate is 0.05～1g/L, and the quality-volumetric concentration of asccharin is 0.1～1g/L, Isosorbide-5-Nitrae-Quality-the volumetric concentration of butynediols is 0.2～0.5g/L; The described time of boiling is 30～50min;
2) anode nickel plates is put into anode basket access positive pole, by grand master pattern access negative pole processed nickel, carried out electroforming, through the negative electrode demouldingAfter obtain high reflectance microprism reflective membrane Working mould; The condition of described electroforming is that current density is 4～10A/dm2, ultrasonic powerBe 210～300W, frequency is 30～50kHz, and the time of electroforming is 2～4h.
2. utilize as claimed in claim 1 ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould, its feature existsIn in step 1) in, the temperature of described hot water is 50～60 DEG C.
3. utilize as claimed in claim 2 ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould, its feature existsIn, the temperature of described hot water is 55 DEG C.
4. utilize as claimed in claim 1 ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould, its feature existsIn, described in time of boiling be 40min.
5. utilize as claimed in claim 1 ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould, its feature existsIn in step 1) in, described adjusting pH is that the sulfuric acid solution that 4.2 employing mass percent concentrations are 30% regulates.
6. utilize as claimed in claim 1 ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould, its feature existsIn in step 1) in, regulate pH at 45～55 DEG C, to be incubated 8～12h after 4.2.
7. utilize as claimed in claim 6 ultrasonic electroforming to prepare the method for high reflectance microprism reflective membrane Working mould, its feature existsAfter regulating pH to be 4.2, at 50 DEG C, be incubated 10h.
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| CN103882483B (en) * | 2014-04-11 | 2016-06-15 | 集美大学 | High reflectance microprism Working mould preparation facilities and its preparation method |
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| CN101571606A (en) * | 2009-06-01 | 2009-11-04 | 浙江工业大学 | Large-size micro-prism type reflecting material die and preparation method thereof |
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| JP4971061B2 (en) * | 2007-07-23 | 2012-07-11 | 東洋鋼鈑株式会社 | Light reflecting plate, method for manufacturing the same, and light reflecting device |
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| CN101571606A (en) * | 2009-06-01 | 2009-11-04 | 浙江工业大学 | Large-size micro-prism type reflecting material die and preparation method thereof |
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