CN105937028B - A kind of compounding cyanogen-less gold liquid and preparation method thereof - Google Patents
A kind of compounding cyanogen-less gold liquid and preparation method thereof Download PDFInfo
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- CN105937028B CN105937028B CN201610348948.5A CN201610348948A CN105937028B CN 105937028 B CN105937028 B CN 105937028B CN 201610348948 A CN201610348948 A CN 201610348948A CN 105937028 B CN105937028 B CN 105937028B
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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 present invention relates to the technical fields of light industry, chemical materials, more particularly to a kind of compounding cyanogen-less gold liquid and preparation method thereof, the compounding cyanogen-less gold liquid, it is characterised in that: be made of no cyanogen gold salt, soft base class complexant, non-soft base class complexant, reducing agent, impurity screening agent, additive, pH buffer and water；Wherein, the content of non-cyanogen gold salt is 0.8 ~ 6g/L, the content of soft base class complexant is 8 ~ 50g/L, the content of non-soft base class complexant is 3 ~ 20g/L, the content of reducing agent is 1 ~ 10g/L, the content of impurity screening agent is 5 ~ 20g/L, and the content of additive is 1 ~ 10g/L, and the content of pH buffer is 10 ~ 40g/L.The compounding cyanogen-less gold liquid has the advantages that stability is good, plating effect is good, gold salt utilization rate is high to the corrosion very little of nickel layer.Also have the characteristics that preparation method is simple and production cost is low.
Description
Technical field
The present invention relates to the technical fields of light industry, chemical materials, more particularly to a kind of compounding cyanogen-less gold liquid and its system
Preparation Method.
Background technique
Fitting has good physical property and stable chemical property, be therefore widely used in high-end decoration, electronics,
Numerous industrial circles such as instrument, space flight.Traditional Gold-plating technique mainly uses cyanide gold-plated, although the effect that cyanide is gold-plated
It is good, but bring negative effect is also very big.It is well known that the CN in cyanide-There is severe toxicity, not only there are safety to human body
Hidden danger, and its waste water is also very big to the pollution of environment, country is proposed a series of environmental protection measure in recent years, and cyanogen-containing gold-plated is answered
With by stringent control, therefore, the demand to non-cyanogen gold-plating technique is more more and more urgent.
In order to capture this technical problem, lot of domestic and foreign enterprises and research unit have carried out a large amount of work, wherein having
The representative application for having citric acid gold potassium (Bing Erjin) gold-plated, this substance are a kind of gold salts without Cyanide, but right
The judgement of its property is disputable always, and with the progress of determination techniques, such substance is accredited as organonitrile compound, belongs to play
Malicious chemicals, thus do not realize really yet 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 will increase industrial cost, and the stability of plating solution is poor.And then people turn to aurous research,
And it makes some progress, including monovalencies gold salts such as sulfurous acid gold, gold aurothiosulfate, citric acid gold, thiocyanic acid gold.
Most study has sulfurous acid gold and gold chloride the two systems at present, according to gold complex stability constant it is found that inferior sulfate radical and
Chloride ion and gold ion have biggish ligand stability constant, therefore most researchers can select both substances as research pair
As.However, since the presence of the sulphur in sulfurous acid gold can greatly increase the corrosion of nickel, it will cause that corrosion of coating depth is excessive to ask
Topic, therefore the gold plating liquid of sulfurous acid in the prior art gold haves the defects that the corrosion to nickel layer is big, in addition, the prior art Central Asia
The gold plating liquid of auric sulfate there is also less stable, plating is ineffective, gold salt utilization rate is not high the problems such as.
Summary of the invention
It is an object of the present invention to providing a kind of compounding cyanogen-less gold liquid aiming at the deficiencies in the prior art,
The compounding cyanogen-less gold liquid is small to the corrosion of nickel layer, and has the advantages that stability is good, plating effect is good, gold salt utilization rate is high.
The second object of the present invention is to provide a kind of compounding cyanogen-less gold liquid aiming at the deficiencies in the prior art
Preparation method.
One of in order to achieve the above objectives, the present invention is achieved through the following technical solutions.
A kind of compounding cyanogen-less gold liquid is provided, is by no cyanogen gold salt, soft base class complexant, non-soft base class complexant, reduction
Agent, impurity screening agent, additive, pH buffer and water composition；
Wherein, in the compounding cyanogen-less gold liquid, the content of the non-cyanogen gold salt is 0.8~6g/L, the soft base class
The content of complexant is 8~50g/L, and the content of the non-soft base class complexant is 3~20g/L, and the content of the reducing agent is 1
~10g/L, the content of the impurity screening agent are 5~20g/L, and the content of the additive is 1~10g/L, the pH buffering
The content of agent is 10~40g/L.
The no cyanogen gold salt is gold sodium sulfide.
The soft base class complexant is sodium sulfocyanate, thiosemicarbazides, ethylene thiourea, -1,3,4 thiophene of 2- amino -5- sulfydryl
One of azoles, 6-MP or any two or more compounding mixture.
The non-soft base class complexant be potassium pyrophosphate, melamine, sulfamate, iminodiacetic acid, glycine,
One of tetren, uridine, caffeine, ammonium citrate, tartaric acid or any two or more compounding mixture.
The reducing agent is one of sodium hypophosphite, anhydrous sodium sulfite, formaldehyde, hydrazine hydrate or any two or more
Compound mixture.
The impurity screening agent is diethyl pentetic acid, aminotrimethylenephosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, second two
One of amine tetramethylene phosphonic acid, diethylenetriamine pentamethylene fork phosphonic acids or any two or more compounding mixture.
The additive is one of sodium ascorbate, famille rose, sunset yellow, D- D-sorbite or any two or more
Compounding mixture.
The pH buffer is one of sodium dihydrogen phosphate, disodium hydrogen phosphate, calgon, Sodium Acid Pyrophosphate
Or any two or more compounding mixture；
The pH buffer controls the pH of the compounding cyanogen-less gold liquid between 5.0~7.0.
In order to achieve the above objectives two, the present invention is achieved through the following technical solutions.
There is provided it is a kind of compound cyanogen-less gold liquid preparation method, it the following steps are included:
Step 1 prepares the first mixed liquor: after first the soft base class complexant of formula ratio and non-soft base class complexant are mixed,
It is added without cyanogen gold salt, water is then added, be uniformly mixed, the first mixed liquor is made；
Step 2 prepares the second mixed liquor: after reducing agent, impurity screening agent, additive and pH buffer are mixed, being added
Water is uniformly mixed, and the second mixed liquor is made；
Step 3 prepares cyanogen-less gold liquid: by the second mixing made from the first mixed liquor made from step 1 and step 2
After liquid is according to certain volume ratio mixing, then after being diluted with water, the compounding cyanogen-less gold liquid is obtained.
It is the soft base class complexant, described in the step of step 1 prepares the first mixed liquor in above-mentioned technical proposal
The mass ratio of the quality summation of non-soft base class complexant and the no cyanogen gold salt and the water is 2~4:6~8；
The step 2 was prepared in the step of the second mixed liquor, the reducing agent, the impurity screening agent, the additive
It is 2~4:6~8 with the quality summation of the pH buffer and the mass ratio of the water；
The step 3 was prepared in the step of cyanogen-less gold liquid, and the first mixed liquor and step 2 made from step 1 are made
The second mixed liquor according to the volume ratio mixing of 1:2~4 after, then after being diluted with water 4~6 times, obtain the compounding non-cyanide plating
Golden liquid.
Beneficial effects of the present invention:
(1) a kind of compounding cyanogen-less gold liquid provided by the invention, soft base class complexant in the compounding cyanogen-less gold liquid and
It, can be to the Au in no cyanogen gold salt after non-soft base class complexant compounding+Coordination ability play the role of collaboration enhancing, and can be effective
Therefore preventing obtained compounding cyanogen-less gold liquid from spontaneous reaction occurs enables to the compounding cyanogen-less gold liquid more stable,
To extend the service life of the compounding cyanogen-less gold liquid.
(2) a kind of compounding cyanogen-less gold liquid provided by the invention, reducing agent sodium hypophosphite in the compounding cyanogen-less gold liquid,
Anhydrous sodium sulfite, formaldehyde or hydrazine hydrate can be well by Au due to stronger reducing power+It is reduced to Au, is passed through
The control of process conditions makes rate of reduction be maintained at a stable level, to obtain coating fine and close, that porosity is low.
(3) a kind of compounding cyanogen-less gold liquid provided by the invention, more or less has one during the entire process of plating
The introducing of a little heteroions, mainly there is Cu2+、Ni2+、Pd2+Equal metal ions, these heteroions can slowly increase during plating
It is more, influence the stability of plating solution and the quality of coating, if untreated meeting so that plating solution the lost of life, cause greater loss.
Cu can be effectively complexed in impurity screening agent2+、Ni2+、Pd2+Equal metal ions, form stable complex compound, to avoid these
The influence of heteroion, so that the effective ion in the compounding cyanogen-less gold liquid is able to maintain in a stable environment, and then one
Determine to guarantee the Au in the compounding cyanogen-less gold liquid in degree+Activity.
(4) a kind of compounding cyanogen-less gold liquid provided by the invention, the addition master of the additive in the compounding cyanogen-less gold liquid
Contribute to regulation reaction rate, make to plate speed be maintained at one it is appropriate within the scope of so that plated layer compact, obtain good
Good coating；In addition, the additive in the compounding cyanogen-less gold liquid can also increase the brightness of coating.
(5) a kind of compounding cyanogen-less gold liquid provided by the invention, the pH buffer in the compounding cyanogen-less gold liquid make applying
PH is maintained at proper range during plating, enables each component in the compounding cyanogen-less gold liquid in a suitable environment
It is reacted, to guarantee the stabilization and normal plating speed of the compounding cyanogen-less gold liquid.
(6) a kind of compounding cyanogen-less gold liquid provided by the invention, due to the synergistic effect between each component, so that the compounding
Cyanogen-less gold liquid is small to the corrosion of nickel layer, and has the advantages that stability is good, plating effect is good, gold salt utilization rate is high.After plating
It can obtain bright, fine and close coating.
(7) a kind of compounding cyanogen-less gold liquid provided by the invention, the compounding cyanogen-less gold liquid and other domestic and international gold plating liquids
Formula compare, be free of CN-And other heavy metal ion, there is production safety, waste liquid is easily handled, and environmental pollution is lesser
Advantage.
(8) a kind of preparation method for compounding cyanogen-less gold liquid provided by the invention, has preparation method simple, production cost
It is low, and the characteristics of being mass produced can be suitable for.
Detailed description of the invention:
Fig. 1 be the compounding gold-plated Gold plated Layer obtained on copper sheet of cyanogen-less gold liquid obtained of embodiment 1 electron microscope with cut
Piece figure；
Fig. 2 be the compounding gold-plated Gold plated Layer obtained on copper sheet of cyanogen-less gold liquid obtained of embodiment 2 electron microscope with cut
Piece figure；
Fig. 3 be the compounding gold-plated Gold plated Layer obtained on copper sheet of cyanogen-less gold liquid obtained of embodiment 3 electron microscope with cut
Piece figure；
Fig. 4 be the compounding gold-plated Gold plated Layer obtained on copper sheet of cyanogen-less gold liquid obtained of embodiment 4 electron microscope with cut
Piece figure；
Fig. 5 be the compounding gold-plated Gold plated Layer obtained on copper sheet of cyanogen-less gold liquid obtained of embodiment 5 electron microscope with cut
Piece figure；
Fig. 6 be the compounding gold-plated Gold plated Layer obtained on copper sheet of cyanogen-less gold liquid obtained of embodiment 6 electron microscope with cut
Piece figure.
Specific embodiment
In order to keep the technical problems, technical solutions and beneficial effects solved by the present invention clearer, below in conjunction with implementation
Example, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only to explain this hair
It is bright, it is not intended to limit the present invention.
Embodiment 1.
A kind of compounding cyanogen-less gold liquid of the present embodiment 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 the 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 are 10g/L, and ammonium citrate 5g/L, 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 sodium dihydrogen phosphate and disodium hydrogen phosphate control the pH value of the compounding cyanogen-less gold liquid
6.5。
It is above-mentioned it is a kind of compound cyanogen-less gold liquid preparation method, it the following steps are included:
Step 1 prepares the first mixed liquor: first mixing the ethylene thiourea of formula ratio, sulfamic acid sodium and ammonium citrate
Afterwards, gold sodium sulfide is added, water is then added, is uniformly mixed, the first mixed liquor is made；Wherein, ethylene thiourea, sulfamic acid
The mass ratio of the quality summation and water of sodium and ammonium citrate is 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, water is added, is uniformly mixed, the second mixed liquor is made；Wherein, anhydrous sodium sulfite, hydroxyl
Ethylene-diphosphonic acid, sodium ascorbate, sodium dihydrogen phosphate and the quality summation of disodium hydrogen phosphate and the mass ratio of water are 3:7；
Step 3 prepares cyanogen-less gold liquid: by the second mixing made from the first mixed liquor made from step 1 and step 2
After liquid is according to the volume ratio mixing of 1:3, then after being diluted with water 5 times, compounding cyanogen-less gold liquid is obtained.
Embodiment 2.
A kind of compounding cyanogen-less gold liquid of the present embodiment, be by gold sodium sulfide, 2- amino -5- sulfydryl -1,3,4 thiazoles,
Tetren, melamine, sodium hypophosphite, aminotrimethylenephosphonic acid, diethyl pentetic acid, famille rose, phosphoric acid
Sodium dihydrogen, disodium hydrogen phosphate and water composition.
Wherein, in the 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 melamine is 3g/L, and sodium hypophosphite contains
Amount is 1.5g/L, and the content of aminotrimethylenephosphonic acid 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 sodium dihydrogen phosphate and disodium hydrogen phosphate control the pH value of the compounding cyanogen-less gold liquid
7.0。
It is above-mentioned it is a kind of compound cyanogen-less gold liquid preparation method, it the following steps are included:
Step 1 prepares the first mixed liquor: first by 2- amino -5- sulfydryl -1,3 of formula ratio, 4 thiazoles, four ethylidene five
After amine and melamine mixing, gold sodium sulfide is added, water is then added, is uniformly mixed, the first mixed liquor is made；Wherein, 2-
The mass ratio of -1,3,4 thiazole of amino -5- sulfydryl, the quality summation of tetren and melamine and water is 2:8；
Step 2 prepares the second mixed liquor: by sodium hypophosphite, aminotrimethylenephosphonic acid, diethyl pentetic acid, rouge
Rouge is red, after sodium dihydrogen phosphate and disodium hydrogen phosphate mixing, and water is added, is uniformly mixed, the second mixed liquor is made；Wherein, hypophosphorous acid
Sodium, aminotrimethylenephosphonic acid, the quality summation of diethyl pentetic acid, famille rose, sodium dihydrogen phosphate and disodium hydrogen phosphate
Mass ratio with water is 2:8；
Step 3 prepares cyanogen-less gold liquid: by the second mixing made from the first mixed liquor made from step 1 and step 2
After liquid is according to the volume ratio mixing of 1:2, then after being diluted with water 4 times, compounding cyanogen-less gold liquid is obtained.
Embodiment 3.
A kind of compounding cyanogen-less gold liquid of the present embodiment is by gold sodium sulfide, 6-MP, thiosemicarbazides, amino sulphur
Sour potassium, potassium pyrophosphate, sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, D- D-sorbite, Sodium Acid Pyrophosphate and water composition.
Wherein, in the 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 are 10g/L, and the content of sulfamic acid potassium is 5g/L, and the content of potassium pyrophosphate is 5g/L, secondary phosphorus
The content of sour sodium is 1.5g/L, and the content of 1-hydroxy ethylidene-1,1-diphosphonic acid is 20g/L, and the content of D- D-sorbite is 8g/L, pyrophosphoric acid
The content of disodium dihydrogen is 10g/L.
Wherein, pH buffer Sodium Acid Pyrophosphate controls the pH value of the compounding cyanogen-less gold liquid 6.8.
It is above-mentioned it is a kind of compound cyanogen-less gold liquid preparation method, it the following steps are included:
Step 1 prepares the first mixed liquor: first by the 6-MP of formula ratio, thiosemicarbazides, sulfamic acid potassium and burnt phosphorus
After sour potassium mixing, gold sodium sulfide is added, water is then added, is uniformly mixed, the first mixed liquor is made；Wherein, 6-MP, ammonia
The quality summation of base thiocarbamide, 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- D-sorbite and pyrophosphoric acid two
After disodium hydrogen mixing, water is added, is uniformly mixed, the second mixed liquor is made；Wherein, sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, the mountain D-
The mass ratio of the quality summation and water of pears sugar alcohol and Sodium Acid Pyrophosphate is 4:6；
Step 3 prepares cyanogen-less gold liquid: by the second mixing made from the first mixed liquor made from step 1 and step 2
After liquid is according to the volume ratio mixing of 1:4, then after being diluted with water 6 times, compounding cyanogen-less gold liquid is obtained.
Embodiment 4.
A kind of compounding cyanogen-less gold liquid of the present embodiment, is 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 the 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 are 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 sodium dihydrogen phosphate and disodium hydrogen phosphate control the pH value of the compounding cyanogen-less gold liquid
6.5。
It is above-mentioned it is a kind of compound cyanogen-less gold liquid preparation method, it the following steps are included:
Step 1 prepares the first mixed liquor: after first mixing the thiosemicarbazides of formula ratio and potassium pyrophosphate, sulfurous acid is added
Golden sodium, is then added water, is uniformly mixed, and the first mixed liquor is made；Wherein, the quality summation and water of thiosemicarbazides and potassium pyrophosphate
Mass ratio be 2.5:7.5；
Step 2, prepare the second mixed liquor: by formaldehyde, diethyl pentetic acid, sodium ascorbate, sodium dihydrogen phosphate and
After disodium hydrogen phosphate mixing, water is added, is uniformly mixed, the second mixed liquor is made；Wherein, formaldehyde, diethyl pentetic acid, anti-
The mass ratio of bad hematic acid sodium, the quality summation of sodium dihydrogen phosphate and disodium hydrogen phosphate and water is 2.5:7.5；
Step 3 prepares cyanogen-less gold liquid: by the second mixing made from the first mixed liquor made from step 1 and step 2
After liquid is according to the volume ratio mixing of 1:2.5, then after being diluted with water 5 times, compounding cyanogen-less gold liquid is obtained.
Embodiment 5.
A kind of compounding cyanogen-less gold liquid of the present embodiment 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 the 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 are 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 sodium dihydrogen phosphate and disodium hydrogen phosphate control the pH value of the compounding cyanogen-less gold liquid
7.0。
It is above-mentioned it is a kind of compound cyanogen-less gold liquid preparation method, it the following steps are included:
Step 1 prepares the first mixed liquor: first mixing the thiosemicarbazides of formula ratio, iminodiacetic acid and glycine
Afterwards, gold sodium sulfide is added, water is then added, is uniformly mixed, the first mixed liquor is made；Wherein, thiosemicarbazides, iminodiacetic acid (salt)
The mass ratio of the quality summation and water of acid and glycine is 3.5:6.5；
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 sour disodium hydrogen mixing, water is added, is uniformly mixed, the second mixed liquor is made；Wherein, sodium hypophosphite, 1-hydroxy ethylidene-1,1-diphosphonic acid, day
The mass ratio of the quality summation and water that fall yellow, sodium dihydrogen phosphate and disodium hydrogen phosphate is 3.5:6.5；
Step 3 prepares cyanogen-less gold liquid: by the second mixing made from the first mixed liquor made from step 1 and step 2
After liquid is according to the volume ratio mixing of 1:3.5, then after being diluted with water 4 times, compounding cyanogen-less gold liquid is obtained.
Embodiment 6.
A kind of compounding cyanogen-less gold liquid of the present embodiment, is by gold sodium sulfide, sodium sulfocyanate, 6-MP, uridine, Asia
Ethyl thiourea, caffeine, tartaric acid, formaldehyde, hydrazine hydrate, ethylenediamine tetramethylene phosphonic acid, diethylenetriamine pentamethylene pitch phosphine
Acid, sodium ascorbate, calgon and water composition.
Wherein, in the compounding cyanogen-less gold liquid, the content of gold sodium sulfide is 6g/L, and the content of sodium sulfocyanate is 30g/
L, the content of 6-MP are 3g/L, and the content of uridine is 4g/L, and the content of ethylene thiourea is 5g/L, and the content of caffeine is
5g/L, the content of tartaric acid are 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 that diethylenetriamine pentamethylene pitches phosphonic acids is 5g/L, and the content of sodium ascorbate is 6g/L,
The content of calgon is 40g/L.
Wherein, pH buffer calgon controls the pH value of the compounding cyanogen-less gold liquid 5.5.
It is above-mentioned it is a kind of compound cyanogen-less gold liquid preparation method, it the following steps are included:
Step 1, prepare the first mixed liquor: first by the sodium sulfocyanate of formula ratio, 6-MP, uridine, ethylene thiourea,
After caffeine and tartaric acid mixing, gold sodium sulfide is added, water is then added, is uniformly mixed, the first mixed liquor is made；Wherein,
Sodium sulfocyanate, 6-MP, uridine, ethylene thiourea, caffeine and the quality summation of tartaric acid and the mass ratio of water are 3:7；
Step 2, prepare the second mixed liquor: by ethylenediamine tetramethylene phosphonic acid, diethylenetriamine pentamethylene fork phosphonic acids,
After sodium ascorbate and calgon mixing, water is added, is uniformly mixed, the second mixed liquor is made；Wherein, ethylenediamine tetraacetic methylene
Base phosphonic acids, diethylenetriamine pentamethylene pitch the quality summation of phosphonic acids, sodium ascorbate and calgon and the mass ratio of water
For 2:8；
Step 3 prepares cyanogen-less gold liquid: by the second mixing made from the first mixed liquor made from step 1 and step 2
After liquid is according to the volume ratio mixing of 1:4, then after being diluted with water 6 times, compounding cyanogen-less gold liquid is obtained.
Performance test.
Compounding cyanogen-less gold liquid made from above-described embodiment 1 to embodiment 6 is tested for the property, embodiment 1 to implementation
The compounding cyanogen-less gold liquid obtained of example 6 is tested on the identical copper sheet of specification, according to oil removing, washing, microetch, washing, pickling,
Experiment is completed in activation, washing, chemical nickel, washing, chemistry gold, the process flow washed, to obtain embodiment 1 to 6 institute of embodiment
Corresponding Gold plated Layer；Wherein, the compounding gold-plated Gold plated Layer obtained on copper sheet of cyanogen-less gold liquid, such as Fig. 1 made from embodiment 1
Shown, the left side is the electron microscope in nickel layer face after moving back 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 sheet of compounding cyanogen-less gold liquid obtained, as shown in Fig. 2, the left side is the Electronic Speculum in nickel layer face after moving back gold
Figure, the right is slice map, and discovery has nickel corrosion, and corrosion depth is less than 1/4；Wherein, compounding cyanogen-less gold made from embodiment 3
The gold-plated Gold plated Layer obtained on copper sheet of liquid, as shown in figure 3, the left side is the electron microscope in nickel layer face after moving back gold, the right is slice map,
Do not occur nickel corrosion；Wherein, the compounding gold-plated Gold plated Layer obtained on copper sheet of cyanogen-less gold liquid, such as Fig. 4 made from embodiment 4
Shown, the left side is the electron microscope in nickel layer face after moving back gold, and the right is slice map, does not occur nickel corrosion；Wherein, embodiment 5 is made
The gold-plated Gold plated Layer obtained on copper sheet of compounding cyanogen-less gold liquid, as shown in figure 5, the left side is the Electronic Speculum in nickel layer face after moving back gold
Figure, the right is slice map, and discovery has nickel corrosion, and corrosion depth is less than 1/6；Wherein, compounding cyanogen-less gold made from embodiment 6
The gold-plated Gold plated Layer obtained on copper sheet of liquid, as shown in fig. 6, the left side is the electron microscope in nickel layer face after moving back gold, the right is slice map,
Do not occur nickel corrosion.
In addition, carrying out range estimation surface topography, gold-plated rate, nickel gold knot to Gold plated Layer corresponding to embodiment 1 to embodiment 6
With joint efforts, the test items such as nickel corrosion depth, plating weldability, welding pulling force, porosity, the evaluation criterion specifically tested is referring to table
1, test result is referring to table 2.
The evaluation table of the gold-plated effect of table 1
The performance test results table of cyanogen-less gold liquid is compounded made from 2 embodiment 1 to embodiment 6 of table
From the performance test results of table 2 it is found that a kind of compounding cyanogen-less gold liquid of the present invention is applying Gold plated Layer obtained,
Surface topography is fine and close, smooth, wherein gold-plated rate is fast, the golden binding force of nickel is good, nickel corrosion depth is shallow, and has coating solderable
Property and the good advantage of Joint Strength.
Finally it should be noted that the above examples are only used to illustrate the technical scheme of the present invention rather than protects to the present invention
The limitation of range, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should be managed
Solution, can with modification or equivalent replacement of the technical solution of the present invention are made, without departing from technical solution of the present invention essence and
Range.
Claims (5)
1. a kind of compounding cyanogen-less gold liquid, it is characterised in that: be by no cyanogen gold salt, soft base class complexant, non-soft base class complexant,
Reducing agent, impurity screening agent, additive, pH buffer and water composition；
Wherein, in the compounding cyanogen-less gold liquid, the content of the no cyanogen gold salt is 0.8~6g/L, the soft base class coordination
The content of agent is 8~50g/L, and the content of the non-soft base class complexant is 3~20g/L, the content of the reducing agent is 1~
10g/L, the content of the impurity screening agent are 5~20g/L, and the content of the additive is 1~10g/L, the pH buffer
Content be 10~40g/L；
The soft base class complexant is sodium sulfocyanate, thiosemicarbazides, ethylene thiourea, -1,3,4 thiazole of 2- amino -5- sulfydryl, 6-
One of mercaptopurine or any two or more compounding mixture；
The non-soft base class complexant is potassium pyrophosphate, melamine, sulfamate, iminodiacetic acid, glycine, four Asias
One of five amine of ethyl, uridine or caffeine or any two or more compounding mixture；
The reducing agent is one of sodium hypophosphite, formaldehyde, anhydrous sodium sulfite, hydrazine hydrate or any two or more compounding
Mixture；
The additive is one of sodium ascorbate, famille rose, sunset yellow, D- D-sorbite or any two or more answers
With mixture；
The impurity screening agent is diethyl pentetic acid, aminotrimethylenephosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, ethylenediamine tetraacetic
One of methylene phosphonic acid, diethylenetriamine pentamethylene fork phosphonic acids or any two or more compounding mixture.
2. a kind of compounding cyanogen-less gold liquid according to claim 1, it is characterised in that: the no cyanogen gold salt is sulfurous acid gold
Sodium.
3. a kind of compounding cyanogen-less gold liquid according to claim 1, it is characterised in that: the pH buffer is biphosphate
One of sodium, disodium hydrogen phosphate, calgon, Sodium Acid Pyrophosphate or any two or more compounding mixture；
The pH buffer controls the pH of the compounding cyanogen-less gold liquid between 5.0~7.0.
4. a kind of preparation method of compounding cyanogen-less gold liquid described in claims 1 to 3 any one, it is characterised in that: it is wrapped
Include following steps:
Step 1 prepares the first mixed liquor: after first mixing the soft base class complexant of formula ratio and non-soft base class complexant, being added
Without cyanogen gold salt, water is then added, is uniformly mixed, the first mixed liquor is made；
Step 2 prepares the second mixed liquor: after reducing agent, impurity screening agent, additive and pH buffer are mixed, water is added,
It is uniformly mixed, the second mixed liquor is made；
Step 3 prepares cyanogen-less gold liquid: the second mixed liquor made from the first mixed liquor made from step 1 and step 2 is pressed
After certain volume ratio mixing, then after being diluted with water, the compounding cyanogen-less gold liquid is obtained.
5. a kind of preparation method for compounding cyanogen-less gold liquid according to claim 4, it is characterised in that: the step 1 system
In the step of standby first mixed liquor, the quality of the soft base class complexant, the non-soft base class complexant and the no cyanogen gold salt
The mass ratio of summation and the water is 2~4:6~8；
The step 2 was prepared in the step of the second mixed liquor, the reducing agent, the impurity screening agent, the additive and institute
The mass ratio of the quality summation and the water of stating pH buffer is 2~4:6~8；
The step 3 was prepared in the step of cyanogen-less gold liquid, by made from the first mixed liquor made from step 1 and step 2
After two mixed liquors are according to the volume ratio mixing of 1:2~4, then after being diluted with water 4~6 times, obtain the compounding cyanogen-less gold liquid.
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| CN107190251B (en) * | 2017-06-19 | 2018-11-16 | 广东东硕科技有限公司 | A kind of gold plating liquid and preparation method thereof |
| CN108220934A (en) * | 2018-01-22 | 2018-06-29 | 昆山成功环保科技有限公司 | A kind of no cyaniding gold leaching solution |
| ES2834877T3 (en) | 2018-01-26 | 2021-06-21 | Atotech Deutschland Gmbh | Electrolytic gold plating bath |
| CN109457239B (en) * | 2018-12-27 | 2021-08-17 | 吉安宏达秋科技有限公司 | Reduction type non-cyanide gold plating solution, gold plating method and gold plated product |
| CN114717618B (en) * | 2022-04-26 | 2023-01-31 | 深圳市联合蓝海黄金材料科技股份有限公司 | Cyanide-free gold electroplating bath and application thereof, semiconductor gold-plated part and preparation method thereof |
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