CN105937028A - Compound cyanide-free gold plating solution and preparation method thereof - Google Patents
Compound cyanide-free gold plating solution and preparation method thereof Download PDFInfo
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- CN105937028A CN105937028A CN201610348948.5A CN201610348948A CN105937028A CN 105937028 A CN105937028 A CN 105937028A CN 201610348948 A CN201610348948 A CN 201610348948A CN 105937028 A CN105937028 A CN 105937028A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
Abstract
The invention relates to the technical field of light industry and chemical materials, in particular to a compound cyanide-free gold plating solution and a preparation method thereof. The compound cyanide-free gold plating solution is characterized by being composed of cyanide-free gold salt, soft base type coordination agents, non-soft base type coordination agents, reducing agents, impurity shielding agents, additives, pH buffering agents and water, wherein the content of the cyanide-free gold salt is 0.8-6g/L, the content of the soft base type coordination agents is 8-50g/L, the content of the non-soft base type coordination agents is 3-20g/L, the content of the reducing agents is 1-10g/L, the content of the impurity shielding agents is 5-20g/L, the content of the additives is 1-10g/L and the content of the pH buffering agents is 10-40g/L. The compound cyanide-free gold plating solution is small in corrosion to nickel layers and has the advantages that the stability is good, the plating effect is good and the utilization rate of the gold salt is high. The preparation method has the advantages of being simple and low in production cost.
Description
Technical field
The present invention relates to the technical field of light industry, chemical materials, particularly relate to a kind of compounding cyanogen-less gold liquid and system thereof
Preparation Method.
Background technology
Gold utensil has good physical property and stable chemical property, be therefore widely used in high-end decoration, electronics,
Numerous industrial circle such as instrument, space flight.Traditional Gold-plating technique mainly uses cyanide gold-plated, although the effect that cyanide is gold-plated
Good, but the negative effect brought is the biggest.It is known that the CN in cyanide-There is severe toxicity, human body not only be there are safety
Hidden danger, and its waste water is the biggest to the pollution of environment, country is proposed a series of environmental practice in recent years, answering of cyanogen-containing gold-plated
With by strict control, therefore, more and more urgent to the demand of non-cyanogen gold-plating technique.
Carry out substantial amounts of work to capture this technical barrier, lot of domestic and foreign enterprises and research unit, wherein had
The representational application having citric acid gold potassium (Bing Erjin) gold-plated, this material is a kind of gold salt without Cyanide, but right
The judgement of its character is the most disputable, and along with the progress of determination techniques, this kind of material is accredited as organonitrile compound, belongs to acute
Poison chemicals, so also without really realize gold-plated field without cyaniding.
Gold-plated industry early application trivalent gold salt is more, but auric reduction needs more reducing agent or higher
Electrode potential, can increase industrial cost, and the less stable of plating solution.And then people turn to aurous research,
And make some progress, including monovalence gold salt such as sulfurous acid gold, gold aurothiosulfate, citric acid gold, Hydrogen thiocyanate gold.
At present most study has sulfurous acid gold and gold chloride the two system, according to gold complex stability constant, inferior sulfate radical with
Chloride ion and gold ion have bigger ligand stability constant, and therefore most researcheres can select both materials right as research
As.But, owing to the existence of the sulfur in sulfurous acid gold can be greatly increased the corrosion of nickel, excessive the asking of the corrosion of coating degree of depth can be caused
Topic, nickel dam is corroded big defect by the gold plating liquid existence of sulfurous acid the most of the prior art gold, it addition, the prior art Central Asia
The gold plating liquid of auric sulfate there is also the problems such as less stable, plating poor effect, gold salt utilization rate be the highest.
Summary of the invention
An object of the present invention is to provide a kind of compounding cyanogen-less gold liquid for weak point of the prior art,
This compounding cyanogen-less gold liquid is little to the corrosion of nickel dam, and there is good stability, plating effect is good, gold salt utilization rate is high advantage.
The two of the purpose of the present invention are to provide a kind of compounding cyanogen-less gold liquid for weak point of the prior art
Preparation method.
For reaching one of above-mentioned purpose, the present invention is achieved through the following technical solutions.
There is provided one compounding cyanogen-less gold liquid, be by without cyanogen gold salt, soft base class complexant, non-soft base class complexant, reduction
Agent, impurity screening agent, additive, pH buffer agent and water composition；
Wherein, in described compounding cyanogen-less gold liquid, the content of described non-cyanogen gold salt is 0.8～6g/L, described soft base class
The content of complexant is 8～50g/L, and the content of described non-soft base class complexant is 3～20g/L, and the content of described reducing agent is 1
～10g/L, the content of described impurity screening agent is 5～20g/L, and the content of described additive is 1～10g/L, and described pH buffers
The content of agent is 10～40g/L.
Described gold salt without cyanogen is gold sodium sulfide.
Described soft base class complexant is sodium rhodanate, thiosemicarbazides, ethylene thiourea, 2-amino-5-sulfydryl-1,3,4 thiophene
A kind of or the most two or more compounding mixture in azoles, 6-MP.
Described non-soft base class complexant be potassium pyrophosphate, tripolycyanamide, sulfamate, iminodiacetic acid, glycine,
A kind of or the most two or more compounding mixture in tetren, uridnine, caffeine, ammonium citrate, tartaric acid.
Described reducing agent is a kind of or the most two or more in sodium hypophosphite, anhydrous sodium sulfite, formaldehyde, hydrazine hydrate
Compounding mixture.
Described impurity screening agent is diethyl pentetic acid, ATMP, 1-hydroxy ethylidene-1,1-diphosphonic acid, second two
A kind of or the most two or more compounding mixture in amine tetramethylene phosphonic acid, diethylenetriamine pentamethylene fork phosphonic acids.
Described additive is a kind of or the most two or more in sodium ascorbate, carmine, sunset yellow, D-Sorbitol
Compounding mixture.
Described pH buffer agent is the one in sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium hexameta phosphate, Sodium Acid Pyrophosphate
Or the most two or more compounding mixture；
Described pH buffer agent makes the pH of described compounding cyanogen-less gold liquid control between 5.0～7.0.
For reaching the two of above-mentioned purpose, the present invention is achieved through the following technical solutions.
Thering is provided the preparation method of a kind of compounding cyanogen-less gold liquid, it comprises the following steps:
Step one, prepares the first mixed liquor: first by after the soft base class complexant of formula ratio and the mixing of non-soft base class complexant,
Add without cyanogen gold salt, be subsequently adding water, mix homogeneously, prepare the first mixed liquor；
Step 2, prepares the second mixed liquor: after reducing agent, impurity screening agent, additive and pH buffer agent being mixed, adds
Water, mix homogeneously, prepare the second mixed liquor；
Step 3, prepares cyanogen-less gold liquid: the second mixing that the first mixed liquor step one prepared and step 2 prepare
After liquid is according to certain volume ratio mixing, then after dilute with water, i.e. prepare described compounding cyanogen-less gold liquid.
In technique scheme, described step one is prepared in the step of the first mixed liquor, described soft base class complexant, institute
The mass ratio of the quality summation and described water of stating non-soft base class complexant and described gold salt without cyanogen is 2～4:6～8；
Described step 2 is prepared in the step of the second mixed liquor, described reducing agent, described impurity screening agent, described additive
It is 2～4:6～8 with the quality summation of described pH buffer agent and the mass ratio of described water；
Described step 3 is prepared in the step of cyanogen-less gold liquid, and the first mixed liquor and the step 2 that step one are prepared prepare
The second mixed liquor mix according to the volume ratio of 1:2～4 after, then after dilute with water 4～6 times, i.e. prepare described compounding non-cyanide plating
Gold liquid.
Beneficial effects of the present invention:
(1) present invention provide one compound cyanogen-less gold liquid, the soft base class complexant in this compounding cyanogen-less gold liquid and
After non-soft base class complexant is compounding, can be to without the Au in cyanogen gold salt+Coordination ability have the effect of collaborative enhancing, and can be effective
Prevent obtained compounding cyanogen-less gold liquid generation spontaneous reaction, therefore, it is possible to make this compounding cyanogen-less gold liquid more stable,
Thus extend the service life of this compounding cyanogen-less gold liquid.
(2) one that the present invention provides compounds cyanogen-less gold liquid, reducing agent sodium hypophosphite in this compounding cyanogen-less gold liquid,
Anhydrous sodium sulfite, formaldehyde or hydrazine hydrate, owing to having stronger reducing power, it is possible to well by Au+It is reduced to Au, passes through
The control of process conditions makes rate of reduction be maintained at a stable level, thus obtain densification, coating that porosity is low.
(3) present invention provide one compound cyanogen-less gold liquid, plating whole during have one more or less
The introducing of a little heteroions, mainly has Cu2+、Ni2+、Pd2+Deng metal ion, these heteroions can slowly increase during plating
Many, affect the stability of plating solution and the quality of coating, if untreated meeting makes the lost of life of plating solution, cause greater loss.
Impurity screening agent can complexation Cu effectively2+、Ni2+、Pd2+Deng metal ion, form stable complex, thus avoid these
The impact of heteroion so that the effective ion in this compounding cyanogen-less gold liquid can be maintained at a stable environment, and then one
Determine in degree, to ensure the Au in this compounding cyanogen-less gold liquid+Activity.
(4) one that the present invention provides compounds cyanogen-less gold liquid, and the adding of additive in this compounding cyanogen-less gold liquid becomes owner of
Contribute to reaction rate, make plating speed be maintained at one suitably within the scope of so that plated layer compact, it is thus achieved that good
Good coating；It addition, the additive in this compounding cyanogen-less gold liquid can also increase the brightness of coating.
(5) one that the present invention provides compounds cyanogen-less gold liquid, and the pH buffer agent in this compounding cyanogen-less gold liquid makes executing
During plating, pH is maintained at proper range so that each component in this compounding cyanogen-less gold liquid can be in a suitable environment
React, to ensure the stable of this compounding cyanogen-less gold liquid and to plate speed normally.
(6) one that the present invention provides compounds cyanogen-less gold liquid, due to the synergism between each component so that this compounds
Cyanogen-less gold liquid is little to the corrosion of nickel dam, and there is good stability, plating effect is good, gold salt utilization rate is high advantage.After plating
Light, fine and close coating can be obtained.
(7) one that the present invention provides compounds cyanogen-less gold liquid, this compounding cyanogen-less gold liquid and other gold plating liquids both at home and abroad
Formula compare, without CN-And other heavy metal ion, there is production safety, waste liquid is easily handled, and environmental pollution is less
Advantage.
(8) preparation method of a kind of compounding cyanogen-less gold liquid that the present invention provides, has preparation method simple, production cost
Low, and the feature of large-scale production can be applicable to.
Accompanying drawing illustrates:
Fig. 1 be the gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid that embodiment 1 prepares Electronic Speculum figure with cut
Sheet figure；
Fig. 2 be the gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid that embodiment 2 prepares Electronic Speculum figure with cut
Sheet figure；
Fig. 3 be the gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid that embodiment 3 prepares Electronic Speculum figure with cut
Sheet figure；
Fig. 4 be the gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid that embodiment 4 prepares Electronic Speculum figure with cut
Sheet figure；
Fig. 5 be the gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid that embodiment 5 prepares Electronic Speculum figure with cut
Sheet figure；
Fig. 6 be the gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid that embodiment 6 prepares Electronic Speculum figure with cut
Sheet figure.
Detailed description of the invention
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with enforcement
Example, is further elaborated to the present invention.Should be appreciated that specific embodiment described herein is only in order to explain this
Bright, it is not intended to limit the present invention.
Embodiment 1.
The one of the present embodiment compounds cyanogen-less gold liquid, is by gold sodium sulfide, ethylene thiourea, sulfamic acid sodium, lemon
Lemon acid ammonium, anhydrous sodium sulfite, 1-hydroxy ethylidene-1,1-diphosphonic acid, sodium ascorbate, sodium dihydrogen phosphate, disodium hydrogen phosphate and water composition.
Wherein, in this compounding cyanogen-less gold liquid, the content of gold sodium sulfide is 2.5g/L, and the content of ethylene thiourea is
20g/L, the content of sulfamic acid sodium is 10g/L, ammonium citrate 5g/L, and the content of anhydrous sodium sulfite is 2g/L, hydroxy ethylidene
The content of di 2 ethylhexyl phosphonic acid is 8g/L, and the content of sodium ascorbate is 10g/L, and the content of sodium dihydrogen phosphate is 12g/L, disodium hydrogen phosphate
Content be 5g/L.
Wherein, pH buffer agent sodium dihydrogen phosphate and disodium hydrogen phosphate make the pH value of this compounding cyanogen-less gold liquid control
6.5。
The preparation method of above-mentioned a kind of compounding cyanogen-less gold liquid, it comprises the following steps:
Step one, prepares the first mixed liquor: first the ethylene thiourea of formula ratio, sulfamic acid sodium and ammonium citrate are mixed
After, add gold sodium sulfide, be subsequently adding water, mix homogeneously, prepare the first mixed liquor；Wherein, ethylene thiourea, sulfamic acid
The quality summation of sodium and ammonium citrate and the mass ratio of water are 3:7；
Step 2, prepares the second mixed liquor: by anhydrous sodium sulfite, 1-hydroxy ethylidene-1,1-diphosphonic acid, sodium ascorbate, di(2-ethylhexyl)phosphate
After hydrogen sodium and disodium hydrogen phosphate mixing, add water, mix homogeneously, prepare the second mixed liquor；Wherein, anhydrous sodium sulfite, hydroxyl
The quality summation of ethylene-diphosphonic acid, sodium ascorbate, sodium dihydrogen phosphate and disodium hydrogen phosphate and the mass ratio of water are 3:7；
Step 3, prepares cyanogen-less gold liquid: the second mixing that the first mixed liquor step one prepared and step 2 prepare
After liquid mixes according to the volume ratio of 1:3, then after dilute with water 5 times, i.e. prepare compounding cyanogen-less gold liquid.
Embodiment 2.
The one of the present embodiment compounds cyanogen-less gold liquid, is by gold sodium sulfide, 2-amino-5-sulfydryl-1,3,4 thiazoles,
Tetren, tripolycyanamide, sodium hypophosphite, ATMP, diethyl pentetic acid, carmine, phosphoric acid
Sodium dihydrogen, disodium hydrogen phosphate and water composition.
Wherein, in this compounding cyanogen-less gold liquid, the content of gold sodium sulfide is 2.5g/L, 2-amino-5-sulfydryl-1,3,
The content of 4 thiazoles is 10g/L, and the content of tetren is 8g/L, and the content of tripolycyanamide is 3g/L, containing of sodium hypophosphite
Amount is 1.5g/L, and the content of ATMP is 2g/L, and the content of diethyl pentetic acid is 3g/L, carmine
Content is 1g/L, and the content of sodium dihydrogen phosphate is 15g/L, and the content of disodium hydrogen phosphate is 5g/L.
Wherein, pH buffer agent sodium dihydrogen phosphate and disodium hydrogen phosphate make the pH value of this compounding cyanogen-less gold liquid control
7.0。
The preparation method of above-mentioned a kind of compounding cyanogen-less gold liquid, it comprises the following steps:
Step one, prepares the first mixed liquor: first by 2-amino-5-sulfydryl-1 of formula ratio, 3,4 thiazoles, four ethylidene five
After amine and tripolycyanamide mixing, add gold sodium sulfide, be subsequently adding water, mix homogeneously, prepare the first mixed liquor；Wherein, 2-
Amino-5-sulfydryl-1,3,4 thiazole, tetren and the quality summation of tripolycyanamide and the mass ratio of water are 2:8；
Step 2, prepares the second mixed liquor: by sodium hypophosphite, ATMP, diethyl pentetic acid, rouge
Fat is red, sodium dihydrogen phosphate and disodium hydrogen phosphate mixing after, add water, mix homogeneously, prepare the second mixed liquor；Wherein, hypophosphorous acid
The quality summation of sodium, ATMP, diethyl pentetic acid, carmine, sodium dihydrogen phosphate and disodium hydrogen phosphate
It is 2:8 with the mass ratio of water；
Step 3, prepares cyanogen-less gold liquid: the second mixing that the first mixed liquor step one prepared and step 2 prepare
After liquid mixes according to the volume ratio of 1:2, then after dilute with water 4 times, i.e. prepare compounding cyanogen-less gold liquid.
Embodiment 3.
The one of the present embodiment compounds cyanogen-less gold liquid, is by gold sodium sulfide, 6-MP, thiosemicarbazides, amino sulphur
Acid potassium, potassium pyrophosphate, sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, D-Sorbitol, Sodium Acid Pyrophosphate and water composition.
Wherein, in this compounding cyanogen-less gold liquid, the content of gold sodium sulfide is 2.5g/L, and the content of 6-MP is
15g/L, the content of thiosemicarbazides is 10g/L, and the content of sulfamic acid potassium is 5g/L, and the content of potassium pyrophosphate is 5g/L, secondary phosphorus
Acid sodium content be 1.5g/L, the content of 1-hydroxy ethylidene-1,1-diphosphonic acid be the content of 20g/L, D-Sorbitol be 8g/L, pyrophosphoric acid
The content of disodium dihydrogen is 10g/L.
Wherein, pH buffer agent Sodium Acid Pyrophosphate makes the pH value of this compounding cyanogen-less gold liquid control 6.8.
The preparation method of above-mentioned a kind of compounding cyanogen-less gold liquid, it comprises the following steps:
Step one, prepares the first mixed liquor: first by the 6-MP of formula ratio, thiosemicarbazides, sulfamic acid potassium and burnt phosphorus
After acid potassium mixing, add gold sodium sulfide, be subsequently adding water, mix homogeneously, prepare the first mixed liquor；Wherein, 6-MP, ammonia
The quality summation of base thiourea, sulfamic acid potassium and potassium pyrophosphate and the mass ratio of water are 4:6；
Step 2, prepares the second mixed liquor: by sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, D-Sorbitol and pyrophosphoric acid two
After disodium hydrogen mixing, add water, mix homogeneously, prepare the second mixed liquor；Wherein, sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, D-mountain
The quality summation of pears sugar alcohol and Sodium Acid Pyrophosphate and the mass ratio of water are 4:6；
Step 3, prepares cyanogen-less gold liquid: the second mixing that the first mixed liquor step one prepared and step 2 prepare
After liquid mixes according to the volume ratio of 1:4, then after dilute with water 6 times, i.e. prepare compounding cyanogen-less gold liquid.
Embodiment 4.
The one of the present embodiment compounds cyanogen-less gold liquid, be by gold sodium sulfide, thiosemicarbazides, potassium pyrophosphate, formaldehyde, two
Ethyl pentaacetic acid, sodium ascorbate, sodium dihydrogen phosphate, disodium hydrogen phosphate and water composition.
Wherein, in this compounding cyanogen-less gold liquid, the content of gold sodium sulfide is 2.5g/L, and the content of thiosemicarbazides is
8g/L, the content of potassium pyrophosphate is 8g/L, and the content of formaldehyde is 2g/L, and the content of diethyl pentetic acid is 5g/L, anti-bad
The content of hematic acid sodium is 10g/L, and the content of sodium dihydrogen phosphate is 5g/L, and the content of disodium hydrogen phosphate is 10g/L.
Wherein, pH buffer agent sodium dihydrogen phosphate and disodium hydrogen phosphate make the pH value of this compounding cyanogen-less gold liquid control
6.5。
The preparation method of above-mentioned a kind of compounding cyanogen-less gold liquid, it comprises the following steps:
Step one, prepares the first mixed liquor: first by after the thiosemicarbazides of formula ratio and potassium pyrophosphate mixing, add sulfurous acid
Gold sodium, is subsequently adding water, mix homogeneously, prepares the first mixed liquor；Wherein, the quality summation of thiosemicarbazides and potassium pyrophosphate and water
Mass ratio be 2.5:7.5；
Step 2, prepares the second mixed liquor: by formaldehyde, diethyl pentetic acid, sodium ascorbate, sodium dihydrogen phosphate and
After disodium hydrogen phosphate mixing, add water, mix homogeneously, prepare the second mixed liquor；Wherein, formaldehyde, diethyl pentetic acid, anti-
The quality summation of bad hematic acid sodium, sodium dihydrogen phosphate and disodium hydrogen phosphate and the mass ratio of water are 2.5:7.5；
Step 3, prepares cyanogen-less gold liquid: the second mixing that the first mixed liquor step one prepared and step 2 prepare
After liquid mixes according to the volume ratio of 1:2.5, then after dilute with water 5 times, i.e. prepare compounding cyanogen-less gold liquid.
Embodiment 5.
The one of the present embodiment compounds cyanogen-less gold liquid, is by gold sodium sulfide, thiosemicarbazides, iminodiacetic acid, sweet
Propylhomoserin, sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, sunset yellow, sodium dihydrogen phosphate, disodium hydrogen phosphate and water composition.
Wherein, in this compounding cyanogen-less gold liquid, the content of gold sodium sulfide is 2.5g/L, and the content of thiosemicarbazides is
10g/L, the content of iminodiacetic acid is 8g/L, and the content of glycine is 5g/L, and the content of sodium hypophosphite is 1.5g/L, hydroxyl
The content of ethylene-diphosphonic acid is 10g/L, and the content of sunset yellow is 5g/L, and the content of sodium dihydrogen phosphate is 10g/L, disodium hydrogen phosphate
Content be 5g/L.
Wherein, pH buffer agent sodium dihydrogen phosphate and disodium hydrogen phosphate make the pH value of this compounding cyanogen-less gold liquid control
7.0。
The preparation method of above-mentioned a kind of compounding cyanogen-less gold liquid, it comprises the following steps:
Step one, prepares the first mixed liquor: first the thiosemicarbazides of formula ratio, iminodiacetic acid and glycine are mixed
After, add gold sodium sulfide, be subsequently adding water, mix homogeneously, prepare the first mixed liquor；Wherein, thiosemicarbazides, iminodiacetic acid (salt)
The quality summation of acid and glycine is 3.5:6.5 with the mass ratio of water；
Step 2, prepares the second mixed liquor: by sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, sunset yellow, sodium dihydrogen phosphate and phosphorus
After acid disodium hydrogen mixing, add water, mix homogeneously, prepare the second mixed liquor；Wherein, sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, day
The quality summation of Huang, sodium dihydrogen phosphate and disodium hydrogen phosphate that falls and the mass ratio of water are 3.5:6.5；
Step 3, prepares cyanogen-less gold liquid: the second mixing that the first mixed liquor step one prepared and step 2 prepare
After liquid mixes according to the volume ratio of 1:3.5, then after dilute with water 4 times, i.e. prepare compounding cyanogen-less gold liquid.
Embodiment 6.
The one of the present embodiment compounds cyanogen-less gold liquid, is by gold sodium sulfide, sodium rhodanate, 6-MP, uridnine, Asia
Ethyl thiourea, caffeine, tartaric acid, formaldehyde, hydrazine hydrate, ethylenediamine tetramethylene phosphonic acid, diethylenetriamine pentamethylene fork phosphine
Acid, sodium ascorbate, sodium hexameta phosphate and water composition.
Wherein, in this compounding cyanogen-less gold liquid, the content of gold sodium sulfide is 6g/L, and the content of sodium rhodanate is 30g/
L, the content of 6-MP is 3g/L, and the content of uridnine is 4g/L, and the content of ethylene thiourea is 5g/L, and the content of caffeine is
5g/L, tartaric content is 2g/L, and the content of formaldehyde is 4g/L, and the content of hydrazine hydrate is 2g/L, ethylenediamine tetramethylene phosphine
The content of acid is 10g/L, and the content of diethylenetriamine pentamethylene fork phosphonic acids is 5g/L, and the content of sodium ascorbate is 6g/L,
The content of sodium hexameta phosphate is 40g/L.
Wherein, pH buffer agent sodium hexameta phosphate makes the pH value of this compounding cyanogen-less gold liquid control 5.5.
The preparation method of above-mentioned a kind of compounding cyanogen-less gold liquid, it comprises the following steps:
Step one, prepares the first mixed liquor: first by the sodium rhodanate of formula ratio, 6-MP, uridnine, ethylene thiourea,
After caffeine and tartaric acid mixing, add gold sodium sulfide, be subsequently adding water, mix homogeneously, prepare the first mixed liquor；Wherein,
Sodium rhodanate, 6-MP, uridnine, ethylene thiourea, caffeine and tartaric quality summation are 3:7 with the mass ratio of water；
Step 2, prepares the second mixed liquor: by ethylenediamine tetramethylene phosphonic acid, diethylenetriamine pentamethylene fork phosphonic acids,
After sodium ascorbate and sodium hexameta phosphate mixing, add water, mix homogeneously, prepare the second mixed liquor；Wherein, ethylenediamine tetraacetic methylene
The quality summation of base phosphonic acids, diethylenetriamine pentamethylene fork phosphonic acids, sodium ascorbate and sodium hexameta phosphate and the mass ratio of water
For 2:8；
Step 3, prepares cyanogen-less gold liquid: the second mixing that the first mixed liquor step one prepared and step 2 prepare
After liquid mixes according to the volume ratio of 1:4, then after dilute with water 6 times, i.e. prepare compounding cyanogen-less gold liquid.
Performance test.
The compounding cyanogen-less gold liquid preparing above-described embodiment 1 to embodiment 6 carries out performance test, embodiment 1 to enforcement
The compounding cyanogen-less gold liquid that example 6 prepares all is tested on the copper coin that specification is identical, according to oil removing, washing, microetch, washing, pickling,
Activation, washing, chemical nickel, washing, chemistry gold, the technological process of washing complete experiment, to obtain embodiment 1 to embodiment 6 institute
Corresponding Gold plated Layer；Wherein, the gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid that embodiment 1 is prepared, such as Fig. 1
Shown in, the left side is to move back the Electronic Speculum figure in nickel dam face after gold, and the right is slice map, finds no nickel corrosion；Wherein, embodiment 2 is made
The gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid, as in figure 2 it is shown, the left side is to move back the Electronic Speculum in nickel dam face after gold
Figure, the right is slice map, is found to have nickel corrosion, and corrosion depth is less than 1/4；Wherein, compounding cyanogen-less gold embodiment 3 prepared
The gold-plated Gold plated Layer obtained on copper coin of liquid, as it is shown on figure 3, the left side is to move back the Electronic Speculum figure in nickel dam face after gold, the right is slice map,
Do not occur that nickel corrodes；Wherein, the gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid that embodiment 4 is prepared, such as Fig. 4
Shown in, the left side is to move back the Electronic Speculum figure in nickel dam face after gold, and the right is slice map, does not occurs that nickel corrodes；Wherein, embodiment 5 is prepared
The gold-plated Gold plated Layer obtained on copper coin of compounding cyanogen-less gold liquid, as it is shown in figure 5, the left side is to move back the Electronic Speculum in nickel dam face after gold
Figure, the right is slice map, is found to have nickel corrosion, and corrosion depth is less than 1/6；Wherein, compounding cyanogen-less gold embodiment 6 prepared
The gold-plated Gold plated Layer obtained on copper coin of liquid, as shown in Figure 6, the left side is to move back the Electronic Speculum figure in nickel dam face after gold, and the right is slice map,
Do not occur that nickel corrodes.
It addition, carry out the Gold plated Layer corresponding to embodiment 1 to embodiment 6 estimating surface topography, gold-plated speed, nickel gold knot
Make a concerted effort, nickel corrosion depth, plating weldability, welding pulling force, the test event such as porosity, the evaluation criterion of concrete test sees table
1, test result sees table 2.
The evaluation table of the gold-plated effect of table 1
The performance test results table of the compounding cyanogen-less gold liquid that table 2 embodiment 1 to embodiment 6 prepares
Knowable to the performance test results of table 2, the Gold plated Layer that a kind of compounding cyanogen-less gold liquid of the present invention is obtained in application,
Surface topography is the finest and close, smooth, and wherein, gold-plated speed is fast, the golden adhesion of nickel is good, nickel corrosion depth is shallow, and it is solderable to have coating
Property and the good advantage of Joint Strength.
It is last it should be noted that, above example is merely to illustrate technical scheme rather than protects the present invention
The restriction of scope, although being explained in detail the present invention with reference to preferred embodiment, those of ordinary skill in the art should manage
Solve, technical scheme can be modified or equivalent, without deviating from technical solution of the present invention essence and
Scope.
Claims (10)
1. a compounding cyanogen-less gold liquid, it is characterised in that: be by without cyanogen gold salt, soft base class complexant, non-soft base class complexant,
Reducing agent, impurity screening agent, additive, pH buffer agent and water composition；
Wherein, in described compounding cyanogen-less gold liquid, the content of described non-cyanogen gold salt is 0.8 ~ 6g/L, described soft base class complexant
Content be 8 ~ 50g/L, the content of described non-soft base class complexant is 3 ~ 20g/L, and the content of described reducing agent is 1 ~ 10g/L,
The content of described impurity screening agent is 5 ~ 20g/L, and the content of described additive is 1 ~ 10g/L, and the content of described pH buffer agent is
10~40g/L。
One the most according to claim 1 compounds cyanogen-less gold liquid, it is characterised in that: described gold salt without cyanogen is sulfurous acid gold
Sodium.
One the most according to claim 1 compounds cyanogen-less gold liquid, it is characterised in that: described soft base class complexant is sulfur cyanogen
Acid sodium, thiosemicarbazides, ethylene thiourea, 2-amino-5-sulfydryl-1,3,4 thiazole, 6-MP in one or any two kinds with
On compounding mixture.
One the most according to claim 1 compounds cyanogen-less gold liquid, it is characterised in that: described non-soft base class complexant is burnt
Potassium phosphate, tripolycyanamide, sulfamate, iminodiacetic acid, glycine, tetren, uridnine, caffeine, Fructus Citri Limoniae
A kind of or the most two or more compounding mixture in acid ammonium, tartaric acid.
One the most according to claim 1 compounds cyanogen-less gold liquid, it is characterised in that: described reducing agent be sodium hypophosphite,
A kind of or the most two or more compounding mixture in formaldehyde, anhydrous sodium sulfite, hydrazine hydrate.
One the most according to claim 1 compounds cyanogen-less gold liquid, it is characterised in that: described impurity screening agent is diethyl
Pentaacetic acid, ATMP, 1-hydroxy ethylidene-1,1-diphosphonic acid, ethylenediamine tetramethylene phosphonic acid, diethylenetriamine five are sub-
A kind of or the most two or more compounding mixture in methyl fork phosphonic acids.
One the most according to claim 1 compounds cyanogen-less gold liquid, it is characterised in that: described additive is ascorbic acid
A kind of or the most two or more compounding mixture in sodium, carmine, sunset yellow, D-Sorbitol.
One the most according to claim 1 compounds cyanogen-less gold liquid, it is characterised in that: described pH buffer agent is biphosphate
A kind of or the most two or more compounding mixture in sodium, disodium hydrogen phosphate, sodium hexameta phosphate, Sodium Acid Pyrophosphate；
Described pH buffer agent makes the pH of described compounding cyanogen-less gold liquid control between 5.0 ~ 7.0.
9. the preparation method of a kind of compounding cyanogen-less gold liquid described in claim 1 to 8 any one, it is characterised in that: its bag
Include following steps:
Step one, prepares the first mixed liquor: first by after the soft base class complexant of formula ratio and the mixing of non-soft base class complexant, add
Gold salt without cyanogen, is subsequently adding water, mix homogeneously, prepares the first mixed liquor；
Step 2, prepares the second mixed liquor: after reducing agent, impurity screening agent, additive and pH buffer agent being mixed, adds water,
Mix homogeneously, prepares the second mixed liquor；
Step 3, prepares cyanogen-less gold liquid: the second mixed liquor that the first mixed liquor step one prepared and step 2 prepare is pressed
After certain volume ratio mixing, then after dilute with water, i.e. prepare described compounding cyanogen-less gold liquid.
The preparation method of a kind of compounding cyanogen-less gold liquid the most according to claim 9, it is characterised in that: described step one
Prepare in the step of the first mixed liquor, described soft base class complexant, described non-soft base class complexant and the matter of described gold salt without cyanogen
Amount summation is 2 ~ 4:6 ~ 8 with the mass ratio of described water；
Described step 2 is prepared in the step of the second mixed liquor, described reducing agent, described impurity screening agent, described additive and institute
The mass ratio of the quality summation and described water of stating pH buffer agent is 2 ~ 4:6 ~ 8；
Described step 3 is prepared in the step of cyanogen-less gold liquid, the first mixed liquor that step one is prepared and step 2 prepare the
After two mixed liquors mix according to the volume ratio of 1:2 ~ 4, then after dilute with water 4 ~ 6 times, i.e. prepare described compounding cyanogen-less gold liquid.
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