CN103409777A - Electroplating auxiliary as well as preparation method and application thereof - Google Patents

Electroplating auxiliary as well as preparation method and application thereof Download PDF

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CN103409777A
CN103409777A CN2013103314311A CN201310331431A CN103409777A CN 103409777 A CN103409777 A CN 103409777A CN 2013103314311 A CN2013103314311 A CN 2013103314311A CN 201310331431 A CN201310331431 A CN 201310331431A CN 103409777 A CN103409777 A CN 103409777A
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electroplating
gram
coating
electrode
plating
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CN2013103314311A
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张岩
马艳
张红红
薛健
杨仲年
贺娟
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张岩
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Abstract

The invention discloses an electroplating auxiliary as well as a preparation method and application thereof. The electroplating auxiliary comprises the following components of 0.3 gram of sodium benzoate, 0.7 gram of gluside, and 0.06 gram of ascorbic acid dissolved into per 100 ml plating solution. The electroplating auxiliary is prepared by electroplating preprocessing, electroplating and electroplating post-processing. Visual inspection proves that plating is bright, and leveling capability is better. Observation under an invert metallographic microscope proves that the plating is compact. The binding force of 9.37 MPa of the plating and a basal body is obtained through an adhesive attraction tester, an electrochemical workstation is adopted for testing a Tafel curve and an electrochemistry impedance spectrogram, and the results show that the corrosion resistance is improved with the comparison to that of electroplating which is not added with the electroplating auxiliary. Measuring a magnetic hysteresis loop and a magnetic curve by a vibration magnetometer proves that the magnetic respond capability of the plating sample is better, but the magnetic property is worse.

Description

A kind of electroplating additives and its preparation method and application
Technical field
The present invention relates to a kind of chemical reagent, the chemical assistant of using while being specifically related to a kind of the plating.
Background technology
Electroplating additives (electroplating additives) is to join in electroplating solution the general name that plating solution and coating character is had to a class chemical of special role.Nd-Fe-B permanent magnet prepared by traditional sintering method causes its erosion resistance poor because of its preparation technology's defect, and prepared by galvanic deposit, nanocrystallinely have higher density and a minimum porosity, have unique advantage and cause widely and pay close attention to preparing aspect nano metal material [1].By great many of experiments, observation and theoretical analysis, show in plating solution and only contain the coating that can not be obtained having the special premium properties needed in ornamental, functional and other actual production practices by the salt of metallizing, must add therein additive.Electroplating additive not only plays most important effect to performances such as the outward appearance of coating, light, electricity, magnetic.But also can change the superpotential of electrode reaction, the deposition of accelerating metal makes the plated film grain refining, change crystalline orientation, can improve in addition internal stress, ductility, compactness, leveling, the hardness of plated film and improve the bath stability performance, having effect very significantly to improving electroplating effect [2].By updating additive and proportioning thereof, can draw the good film of coating performance under different condition.Therefore, the progress of electroplating additive also just indicates the progress of electroplating industry.
It is a kind of more novel and in theory very feasible method that electric plating method prepares neodymium iron boron, and has made some progress Pei Ling [3]Deng by electric plating method, having prepared the neodymium iron boron film, but find by the revision test to it, do not adding under the main salt system of any additive, the sticking power of the neodymium iron boron film compactness of electroplating out, leveling property, luminance brightness, erosion resistance and film and copper matrix is poor.Be apparent that especially the non-constant of stability of plating solution, plate out two samples and find that afterwards there are many precipitations russet bottom and are suspended in the suspended substance in there-necked flask.Therefore extremely be necessary to carry out the height coating performance, improve bath stability by the method that adds additive, thereby prepare the nano level neodymium iron boron film of excellent property.And then by follow-up research, realize the suitability for industrialized production of galvanic deposit nanometer neodymium iron boron film, to substitute the application of existing Sintered Nd-Fe-B Permanent in some field.
Summary of the invention
The object of the invention is to solve above-mentioned the deficiencies in the prior art, provide a kind of and can improve the luminance brightness of electroplating rear metal, the auxiliary agent of resistance to corrosion.
For achieving the above object, the present invention is by the following technical solutions:
A kind of electroplating additives, be comprised of Sodium Benzoate, asccharin and xitix, and in every 100ml electroplating solution, add 0.2-0.8 gram Sodium Benzoate, 0.2-1.0 gram asccharin and 0.05-1.0 gram xitix.
A kind of electroplating solution, composed of the following components:
In every 100ml aqueous solution, add 7.2 gram glycine, 3.6 gram boric acid, 3.0 gram ammonium chlorides, 1.2 gram neodymium chloride six hydrates, 4.0 gram four water iron protochlorides, 0.2-1.0 gram Vanillin, 0.2-0.8 gram Sodium Benzoate, 0.2-1.0 gram asccharin and 0.05-1.0 gram xitix.
Preferably, adding adjust pH before iron protochloride is 3.15.
Preferred Vanillin: 0.4000-0.6000g; Sodium Benzoate: 0.2000-0.4000g; Asccharin: 0.5000-0.7000g; Xitix: 0.0500-0.2000g.Sodium Benzoate: 0.3g most preferably; Asccharin: 0.7g; Xitix: 0.05g.
The preparation process of electroplating additives of the present invention is:
In every 100ml aqueous solution, add 7.2 gram glycine, 3.6 gram boric acid, 3.0 gram ammonium chlorides, 1.2 gram neodymium chloride six hydrates and 4.0 gram four water iron protochlorides; Adding adjust pH before iron protochloride is 3.15, then adds successively respectively Vanillin, Sodium Benzoate, asccharin and xitix.
The invention also discloses a kind of using method of described electroplating additives, comprise the following steps:
1, pre-electroplating treatment
Pre-electroplating treatment is link extremely important, very basic in electroplating technology, and the quality of pre-treatment effect is directly connected to the quality of plated item quality.The bonding force of coating and matrix for example, ornamental, the erosion resistance of coating, planarization, extension power etc.Below introduce respectively each process of pre-treatment:
1.1. polishing
Polishing is in order to improve the surface finish of part, removes the surperficial macroscopic defects, corrosion trace, cut, burr, weld seam, sand holes of part etc., be used to improving quality of coating.This experiment bruting process be in order 03,800CCR, 04, polish above 05 paper, arrangement of this order is the degree of roughness according to coated abrasive surface.
1.2. upper extension
Upper extension just is placed on copper electrode on a carrier, can in flat mouthful of special bottle, electroplate.
1.3. mechanical polishing
Polishing is mainly used for the plating pre-treatment of the part that the effects on surface roughness has relatively high expectations, and makes goods obtain decorative appearance, improves the erosion resistance of goods.The principle of mechanical polishing is the fine cut that utilizes grinding between rubbing paste and polished surface and roll extrusion to be used for eliminating electrode surface, thereby obtains the smooth matrix face of light.1.4. oil removing
Oil removing process is divided into mechanical oil removing, solvent oil removing, electrochemical deoiling, electrolytic degreasing, is in order to go out the greasy dirt of electrode surface, guarantees the bonding strength of coating and substrate.The machinery oil removing generally refers to the employing mechanical means, carrys out oil removing as cylinder and mechanical hairbrush, and it relatively is applicable to the oil removing of large-scale instrument.The solvent oil removing is that electrode is placed in the middle of organic solvent, and the greasy dirt of electrode surface is dissolved in the middle of organic solvent, and commonly used have gasoline, ketone etc. except Oil solvent.The electrochemical deoiling that this experiment is adopted is to utilize the saponification of sodium hydroxide to remove the electrode surface greasy dirt, is applicable to all parts.
1.5. washing
Utilize distilled water that surperficial oil removing medium is rinsed well.
1.6. acid-wash activation
Electrode soaks in acid medium, the sull of electrode surface is removed, and makes it be in a kind of state of activation.
2. electroplate
Use described electroplating additives to electroplate.Preferred holding current density J=0.7958A.dm -2, 45 ℃ of bath temperatures, electroplating time 20min.
3. plating aftertreatment
The aftertreatment of electroplating is mainly the processing for coating, namely how coating is processed and is made it keep the just that state from taking out plating solution, and it is not damaged.This experiment mainly comprises for the processing of coating: wash, dry up, three links of kept dry.
3.1. washing: gently coating surface is rinsed with deionized water, remove the impurity of coating surface, the flushing dynamics is unsuitable excessive, otherwise coating is very easily come off, because just very poor from the binding force of cladding material of taking out plating solution, the dry bonding force that just can make later improves.
3.2. dry up: moisture and a little solution of not rinsing well of with blower, drying up coating surface.
3.3. kept dry: be with coated electrode to put into loft drier to preserve after drying up.
Advantage of the present invention is: during plating, use described electroplating additives to improve greatly the brightness of coating, coating is very fine and close, even inclusion-free, and leveling property is very good; And the coating that does not add electroplating additives has micro-hole, coarse injustice seems; And the erosion resistance of coating also is greatly improved.
The accompanying drawing explanation
Fig. 1 electroplates schema, and the part before electroplating in schema is called pre-treatment, and the part after electroplating is called aftertreatment.
Fig. 2 cyclic voltammetry curve: initial potential E (V)=-1.3, noble potential E (V)=0.8, low potential E (V)=-1.3, initial p/N=P, sweep velocity (V/s)=0.1, sensitivity (A/V)=0.1.
Fig. 3 alternating-current impedance figure.
Fig. 4 fitting circuit figure.
Fig. 5 Ta Feier curve relatively.
Fig. 6 magnetic hysteresis loop: saturation magnetization=0.84emu, residual magnetization=0.16emu, Mr/Ms=0.189, HCJ=12.8KA/m d61.27Oe), remanent magnetism put Mr 90% the time corresponding magneticstrength=9900A/m (124.40Oe).
Fig. 7 magnetzation curve.
Embodiment
In this embodiment, operating process is shown in Fig. 1:
1, pre-electroplating treatment
Pre-electroplating treatment is link extremely important, very basic in electroplating technology, and the quality of pre-treatment effect is directly connected to the quality of plated item quality.The bonding force of coating and matrix for example, ornamental, the erosion resistance of coating, planarization, extension power etc.Below introduce respectively each process of pre-treatment:
1.1. polishing
Polishing is in order to improve the surface finish of part, removes the surperficial macroscopic defects, corrosion trace, cut, burr, weld seam, sand holes of part etc., be used to improving quality of coating.This experiment bruting process be in order 03,800CCR, 04, polish above 05 paper, arrangement of this order is the degree of roughness according to coated abrasive surface.
1.2. upper extension
Upper extension just is placed on copper electrode on a carrier, can in flat mouthful of special bottle, electroplate.
1.3. mechanical polishing
Polishing is mainly used for the plating pre-treatment of the part that the effects on surface roughness has relatively high expectations, and makes goods obtain decorative appearance, improves the erosion resistance of goods.The principle of mechanical polishing is the fine cut that utilizes grinding between rubbing paste and polished surface and roll extrusion to be used for eliminating electrode surface, thereby obtains the smooth matrix face of light.1.4. oil removing
Oil removing process is divided into mechanical oil removing, solvent oil removing, electrochemical deoiling, electrolytic degreasing, is in order to go out the greasy dirt of electrode surface, guarantees the bonding strength of coating and substrate.The machinery oil removing generally refers to the employing mechanical means, carrys out oil removing as cylinder and mechanical hairbrush, and it relatively is applicable to the oil removing of large-scale instrument.The solvent oil removing is that electrode is placed in the middle of organic solvent, and the greasy dirt of electrode surface is dissolved in the middle of organic solvent, and commonly used have gasoline, ketone etc. except Oil solvent.The electrochemical deoiling that this experiment is adopted is to utilize the saponification of sodium hydroxide to remove the electrode surface greasy dirt, is applicable to all parts.
1.5. washing
Utilize distilled water that surperficial oil removing medium is rinsed well.
1.6. acid-wash activation
Electrode soaks in acid medium, the sull of electrode surface is removed, and makes it be in a kind of state of activation.
2. electroplate
Use described electroplating additives to electroplate.Preferred holding current density J=0.7958A.dm -2, 45 ℃ of bath temperatures, electroplating time 20min.
3. plating aftertreatment
The aftertreatment of electroplating is mainly the processing for coating, namely how coating is processed and is made it keep the just that state from taking out plating solution, and it is not damaged.This experiment mainly comprises for the processing of coating: wash, dry up, three links of kept dry.
3.1. washing: gently coating surface is rinsed with deionized water, remove the impurity of coating surface, the flushing dynamics is unsuitable excessive, otherwise coating is very easily come off, because just very poor from the binding force of cladding material of taking out plating solution, the dry bonding force that just can make later improves.
3.2. dry up: moisture and a little solution of not rinsing well of with blower, drying up coating surface.
3.3. kept dry: be with coated electrode to put into loft drier to preserve after drying up.
The design of single factor experiment
1. Vanillin adds the impact on quality of coating
Main salt system selects every 100ml to add 7.2 gram glycine, 3.6 gram boric acid, 3.0 gram ammonium chlorides, 1.2 gram six water. Neodymium trichloride, 4.0 gram four water iron protochlorides.Adding adjust pH before iron protochloride is 3.15, holding current density J=0.7958A.dm -2, 45 ℃ of bath temperatures, electroplating time 20min.Experimental result such as table 1
The experiment of table 1 Vanillin
2. Sodium Benzoate adds the impact on quality of coating
Guaranteeing to add therein Sodium Benzoate under the constant prerequisite such as main salt system, current density, temperature, pH value, time, observe its impact on quality of coating.Experimental result such as table 2
The experiment of table 2 Sodium Benzoate
2. asccharin adds the impact on quality of coating
Guaranteeing to add therein asccharin under the constant prerequisite such as main salt system, current density, temperature, pH value, time, observe its impact on quality of coating.Experimental result such as table 3
The experiment of table 3 asccharin
4. xitix adds the impact on quality of coating
Guaranteeing to add therein the asccharin xitix under the constant prerequisite such as main salt system, current density, temperature, pH value, time, observe its impact on quality of coating.Experimental result such as table 4
The experiment of table 4 xitix
Orthogonal test
Equally also to guarantee to add therein composite additive under the constant prerequisite such as main salt system, current density, temperature, pH value, time, observing its impact on quality of coating.Experimental result such as table 5
Table 5 orthogonal test one
Wherein implication such as table 6 of each letter representative
Each alphabetical implication in table on table 6
Table 7 orthogonal experiment two
Each alphabetical implication in table on table 8
Electroplate the electrochemical behavior of neodymium iron boron
The Shanghai occasion China CHI660C electrochemical workstation of employing standard three-electrode system, using copper electrode or glass-carbon electrode as working electrode, does supporting electrode with platinum plate electrode, usings saturated calomel electrode as reference electrode.
The cyclic voltammetry curve of system
Cyclic voltammetry curve can reflect the microreaction process of electrode surface and the reversibility of electrode reaction [11].Under best conditions of mixture ratios, adopt copper electrode as working electrode.Before test, first to copper electrode, process, successively 03, polish on 800CCR, 04, No. 05 sand paper, then use above metallographic-sample polisher, the particle diameter of take carries out polished finish as the rubbing paste of 0.25 micron.Then it is identical while wanting state between holding anode and negative electrode to test with plating on electrochemical workstation, to carry out cyclic voltammetry when test, and sweep velocity is 0.1V/s, and the scanning current potential is-1.3~1V.
The coating performance testing method
The observation of Deposit appearance and analysis
By visual inspection, can find bright degree and whether jagged, the surface phenomena such as edge is burnt, pin hole of coating, the further observation of use inverted metallurgic microscope can detect the compactness extent of its atomic arrangement, microdefect etc.
The coating porosity detects
1. detection method: paste filter paper method [12]
2. test solution forms: etching reagent: 20g/L sodium-chlor.Indicator is the Tripotassium iron hexacyanide of 10g/L.
3. operation steps: sample is check immediately after plating.Clean filter paper is immersed to test solution, and the filter paper that then will infiltrate test solution is close on sample, between filter paper and sample, can not have bubble residual.Filter paper, after on coating surface, pasting 10min, is taken filter paper off, uses distilled water flushing, is affixed on sheet glass and dries.
4. detection and assessment as a result
Under natural light or luminescent lamp, directly observe the blue spot number of corresponding coating, according to filter paper and sample contact area, calculate porosity: porosity=N/S (individual/cm 2), wherein IV is dropout count (individual), S is the area (cm that is verified sample 2).Arithmetical av evaluation porosity test result with 3 tests.
Coating and basal body binding force test
Adopt PosiTest AT type sticking power detector to carry out quantitative test to binding force of cladding material, can directly from indicating meter, read the size of bonding force, convenient and swift, accurately.
Corrosion of coating behavior curve
For the research of the electrochemical behavior of coating, usually adopt 2 kinds of methods of method of polarization curve and AC impedence method, 2 kinds of test-results have been combined in to analysis.Method of polarization curve is a kind of pressure corrosion, artificially electric current is added on coating and makes it reach corrosion potential.And alternating-current impedance is as a kind of electrochemical techniques of transient state; research be electrochemical system in AC signal disturbance lower frequency response characteristic by a small margin; it is the important means of Electrode process kinetics and surface phenomena thereof; the method that this paper combines by polarization curve and alternating-current impedance; the solidity to corrosion of research coating, from the protective value of electrochemistry angle evaluation coating.
The Ta Feier curve
The Ta Feier curve refers to it is the curve that meets the Tafel relation, refers generally in polarization curve one section of strong polarized area.(Tafel district) presents linear relationship to this section curve (E-logi curve) in certain zone.Research Ta Feier curve can be explained the basic law of alloy corrosion, and controls the corrosion approach.
The alternating-current impedance curve
The alternating-current impedance spectral technology is the stable state electrical measurement method of a kind of sinusoidal wave current potential of take little amplitude as disturbance, to treat examining system by variation research of measuring impedance in the range of frequency to very wide, have test speed fast, research system is disturbed to the characteristics such as little, thereby be used widely [10-13].Testing tool and the same three-electrode system that adopts of mensuration cyclic voltammetry curve, working electrode is neodymium iron boron coating, and supporting electrode is platinized platinum, and reference electrode is saturated calomel electrode.The solution of test is that mass percent is 3.0% standard sodium-chlor etchant solution, and frequency is 0.01-100000HZ, and initial potential is open circuit potential.
The magnetism testing of coating
The JDAW-2000 type vibrating sample magnetometer that adopts the general magnetoelectricity technological development of Changchun English company limited to produce can be under the condition of not inputting sample quality and density, the magnetzation curve of measure sample and magnetic hysteresis loop.Because the value of material Mr/Ms is not subjected to the impact of quality of materials and density [15].By the size of the value of Mr/Ms relatively, can judge the relatively strong and weak of material remanent magnetism.Its size is between 0-1, and the remanent magnetism that is worth larger expression material is just larger, be worth littlely, means that the remanent magnetism of material is just less, and magnetic hysteresis loop is narrower, is worth greatlyr, and the remanent magnetism of expression material is larger, and magnetic hysteresis loop is wider [16].
Auxiliary agent is selected the experiment of single factor result
After the single factor experiment result was analyzed, we had tentatively obtained the scope of application of the various additives under the constant condition of the conditions such as main salt system, current density, temperature, pH value.Addition in every 100ml solution is respectively: Vanillin: 0.4000-0.6000g; Sodium Benzoate: 0.2000-0.4000g; Asccharin:
0.5000-0.7000g; Xitix: 0.0500-0.2000g.-
The orthogonal experiments that auxiliary agent is selected
By first group of orthogonal test, find, the quadrature of four kinds of additives can not obtain a kind of more effectively formula, and the result obtained is generally poor, does not even almost plate thing.And that second group of orthogonal test can obtain is brighter, density is better.According to experimental phenomena, in conjunction with the result of range analysis, show that the additive formulations of plating solution the best should be: Sodium Benzoate: 0.3g; Asccharin: 0.7g; Xitix: 0.05g.
The cyclic voltammetry curve of system
The cyclic voltammetry curve of system such as Fig. 2.
Cyclic voltammetry curve by Fig. 2 can find out, the scanning current potential is from-1.3-0.8V scope, and sweep velocity is 0.1V/s, and sensitivity is 0.1A/V.In the anode scanning process, when sweep voltage, occur that an oxidation peak current is approximately 0.055A during at-0.5297V, in the reverse scan process, when being 0.3797v, sweep voltage there will be a reduction peak current with the similar size of oxidation peak current, its peak value is approximately-0.602A, therefore it can be regarded as to one will definitely be against system, in conjunction with the measuring result of magnetic, the appearance that can find oxidation peak current should be that iron and neodymium codeposition cause.The principal reaction occurred in system should be:
Fe 2++2e -→Fe
Nd 3++3e -→Nd。
The performance test results of neodymium iron boron coating
According to the visualize luminance brightness.
Add additive and the contrast of not doping luminance brightness to find out, add the sample brightness plated out after additive than the good brightness of the coating that does not add additive.
3.4.2MR-5000 inverted metallurgic microscope observations
(the object lens parameter is 20/0.40D) observes the following Fig. 3 of coating in conjunction with Canon's slr camera.
Very fine and close from figure, finding to add additive coating afterwards, even inclusion-free, leveling property is very good.And the coating that does not add additive has micro-hole, coarse injustice seems.
The test of coating porosity
According to the auxiliary agent optimization formula, do ten groups of parallel tests, therefrom select ten samples and test.Obtain result such as following table 9
Table 9 porosity
The binding force of cladding material test result
From upper ten groups of parallel laboratory tests, selecting in addition ten samples to carry out the bonding force test.Experimental result such as following table 10
The test of table 10 bonding force
The corrosion resistance of coating
The alternating-current impedance curve
In the sodium chloride solution of 3.0% (mass percent), adopt three-electrode system, the alternating-current impedance figure that records respectively the coating after 0.5h, 1h, 2h is illustrated in fig. 4 shown below.
According to zsimpwin software match open circuit potential such as Fig. 5.
Concrete match numerical value such as following table 11
Table 11 match numerical tabular
As can be known in conjunction with alternating-current impedance figure and fitting circuit figure, the capacitive reactance arc only appears in material, and oblique line does not appear in the reduction along with frequency, and the corrosion process of this explanation coating is the diffusion control by electrochemical control rather than solution.And be typical electrochemical control feature.Also the corrosion resistance of illustrative material is better for this.
The Ta Feier curve
In standard sodium-chlor etchant solution, namely in the solution of 3.0% (wt%), record respectively Ta Feier curve such as Fig. 6 of containing additive plating solution gained coating and not containing additive gained coating.
Icorr (corrosion current density) density is larger, corrosion speed is faster, the ordinate zou of Ta Feier curve the two poles of the earth intersection point is the log value of Icorr, the size that can reflect Icorr, thereby the corrosion speed of reaction style, by contrasting these two curves, can find, the Icorr of the coating in containing the system of additive decreases, and the erosion resistance of this illustrative material strengthens to some extent.
The magnetism testing of coating
The magnetic hysteresis loop of coating
As Fig. 7
Following table 12 is Mr/Ms value comparisons of the neodymium iron boron for preparing of pure iron, plating sample and quick quenching technique
The Mr/Ms value of three kinds of products of table 12 relatively
Because the quality of the size of the Mr/Ms value of magneticsubstance and measured magnet is irrelevant, so compare how can draw next performance by the Mr/Ms value with pure iron and fast quenching neodymium iron boron.The neodymium iron boron film amount of this experiment preparation is considerably less, so be difficult to its quality of weighing.So when measuring, do not input its quality and density.The Mr/Ms value of the plating sample as can be known of the data in figure is 0.189, and the Mr/Ms value of pure iron is 0.104, and neodymium iron boron Mr/Ms value prepared by quick quenching technique is 0.819, and the magnetic property of the sample that this explanation is electroplated out does not have the magnetic property of neodymium iron boron prepared by quick quenching technique good.From the figure of magnetic hysteresis loop, it is slightly narrow, long and narrow in addition, and the area enclosed is less.When measuring magnetic, magneticsubstance can forward, magnetic reversal in magnetic field, and meeting produces heat in this process, the generation of these heats is paid by externally-applied magnetic field certainly, the size of magneticsubstance energy waste in the remagnetization process directly and the size that surrounds of magnetic hysteresis loop be directly proportional.So this figure can also illustrate, energy dissipation is fewer, and state easily reaches capacity while magnetizing.By above analysis, show that plating sample magnetic property is poor, can not use as permanent magnet material.Can also draw in the sample plated out and should contain neodymium element in addition.
The magnetzation curve of coating
As seen from Figure 8, increase with externally-applied magnetic field intensity, the specific magnetising moment of plating sample constantly increases, when externally-applied magnetic field reaches certain value. the magnetization of plating sample reaches capacity, its specific magnetising moment is tending towards definite value: 0.8emu, when reaching 5000oe, externally-applied magnetic field intensity have sample all to reach the magneticsaturation state. and this neodymium iron boron of preparing of explanation the method has magnetic response ability preferably, can be in the situation that magneticstrength is less works.
Bath stability relatively
When relatively adding respectively additive and not adding additive, plating 3 plating solution colors after sample:
Still the plating solution than adding assistant not is shallow in the color of the plating solution that only plates out 3 samples after plating out 3 samples for the plating solution that adds auxiliary agent, and yellow color is due to the oxidized generation of ferrous iron in plating solution.This explanation, add the stability of plating solution after additive to obtain significantly improving.
Conclusion:
By a series of experiment of single factor and orthogonal experiment, drawn the optimum formula of electroplating the neodymium iron boron additive, namely at main salt system and electroplating parameter, arranged under constant condition and dissolve 0.3g Sodium Benzoate, 0.7g asccharin, 0.05g xitix in every 100ml solution.Under this experiment condition, can plate out light, fine and close coating, and the bonding force of the stability of the erosion resistance of coating, plating solution and coating and matrix has all improved much when not adding additive.
Reference
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Claims (7)

1. an electroplating additives, be comprised of Sodium Benzoate, asccharin and xitix, and in every 100ml electroplating solution, add 0.2-0.8 gram Sodium Benzoate, 0.2-1.0 gram asccharin and 0.05-1.0 gram xitix.
2. electroplating additives as claimed in claim 1, wherein, described electroplating solution is composed of the following components:
7.2 gram glycine, 3.6 gram boric acid, 3.0 gram ammonium chlorides, 1.2 gram neodymium chloride six hydrates, 4.0 gram four water iron protochlorides and 0.2-1.0 gram Vanillin are dissolved in the 100mL aqueous solution.-
3. electroplating additives as claimed in claim 2, wherein, adjust pH is 3.15 before adding iron protochloride.
4. electroplating additives as claimed in claim 1, wherein, Vanillin: 0.4-0.6g; Sodium Benzoate: 0.2-0.4g; Asccharin: 0.5-0.7g; Xitix: 0.05-0.2g.
5. electroplating additives as claimed in claim 4, wherein, Sodium Benzoate: 0.3g; Asccharin: 0.7g; Xitix: 0.05g.
6. the using method of the described electroplating additives of claim 1-5 comprises the following steps:
(1), pre-electroplating treatment
(1.1) polishing
By sample in order 03,800CCR, 04, polish above 05 paper;
(1.2) the upper extension
Copper electrode is placed on a carrier, can in flat mouthful of special bottle, electroplates;
(1.3). mechanical polishing
The fine cut that utilizes grinding between rubbing paste and polished surface and roll extrusion to be used for eliminating electrode surface, thus the smooth matrix face of light obtained;
(1.4). oil removing
Remove the greasy dirt of electrode surface, guarantee the bonding strength of coating and substrate;
(1.5). washing
Utilize distilled water that surperficial oil removing medium is rinsed well;
(1.6). acid-wash activation
Electrode soaks in acid medium, the sull of electrode surface is removed, and makes it be in a kind of state of activation;
(2). electroplate
Use described electroplating additives to electroplate;
(3). electroplate aftertreatment
By coating successively through the washing, dry up and three links of kept dry.
7. application as claimed in claim 6, wherein, holding current density J=0.7958A.dm while electroplating in (2) -2, 45 ℃ of bath temperatures, electroplating time 20min.
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