CN109207971A - A kind of chemistry quickly reduction gold plating liquid and its application - Google Patents
A kind of chemistry quickly reduction gold plating liquid and its application Download PDFInfo
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- CN109207971A CN109207971A CN201811126948.6A CN201811126948A CN109207971A CN 109207971 A CN109207971 A CN 109207971A CN 201811126948 A CN201811126948 A CN 201811126948A CN 109207971 A CN109207971 A CN 109207971A
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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
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Abstract
The invention belongs to chemical gilding technical fields, and in particular to a kind of chemistry quickly reduction gold plating liquid and its application.Including following density component: water-soluble gold compound (in terms of Au) 0.5~1.5g/L, 5~20g/L of sodium hypophosphite, 1~5g/L of hydroxyl sulfate, 25~55g/L of Triammonium citrate, 5~15g/L of disodium ethylene diamine tetraacetate, 0.1~3.0g/L of amino acid, mercapto-polyglycol 0.001~0.02g/L of-R, 0.001~0.02g/L of cetylpyridinium bromide, 0.001~0.005g/L of ligninsulfonate, 0.01~0.1g/L of dimethyamine borane, 0.01~0.3g/L of tartaric acid germanium.The gold plating liquid excellent in stability, deposition rate is fast, the Gold plated Layer surfacing of acquisition, uniform, bright and fine and close；And there is better corrosion resistance and tin plating reflux and beat gold thread performance.
Description
Technical field
The invention belongs to chemical gilding technical field, it is related to the chemical gilding technology of the surface treatment using printed circuit board
A kind of field, and in particular to chemistry quickly reduction gold plating liquid and its application.
Background technique
Carrier and chain junctor of the printed circuit board (PCB) as electronic component, are the main parts sizes of current electronic equipment,
It can be described as the carrying of information age.It the use of Copper substrate is in the pcb current optimal selection, good conductivity and price is relatively
It is low, but there are etching problems, and Cu oxide has lower solderability and unstable welding spot reliability.Fitting has light
Bright color and excellent electric conductivity pole, inoxidizability pole, ductility are very suitable for surface and apply (covering) coating.
Chemical gilding development is very swift and violent, and from nineteen fifty, the U.S. has delivered first chemical gilding patent, and after 10 years
It puts into production, becomes mature a research topic and production project by now.Earliest carried out directly in Copper base material it is gold-plated,
Then barrier layer is introduced in copper and gold, the function of layer gold is also changed in this process.The densification of PCB
(bonding area is smaller and smaller) development, signal high frequency or high-speed digitization need more complete coating；PCB production requirement simultaneously
It is continuously improved, shortens the production time, improve competitiveness, so possessing the better coating of property while how improving plating speed
It is a development trend.
Chemical gilding is chemically, to make the gold ion in gold plating liquid, obtains electronic deposition in plating layer surface, to obtain
Good coating is obtained, immersion gold plating can be divided into according to chemical reaction mechanism and is restored gold-plated.Immersion gold plating is using in plating layer
Metal and gold standard electric potential difference, the gold ion in immersion gold plating liquid, to form coating.But displacement reaction can be with
Gradually forming for Gold plated Layer and slow down, after completely covering layer gold, reaction terminating.So thicker Gold plated Layer cannot be formed,
And the generation of displacement reaction and the metal types of plating layer have great relevance, on some more active metal bases, such as
Copper (Cu2+/ Cu:0.314V), nickel (Ni2+/ Ni:-0.257V) etc. can be with gold (Au+/ Au:1.692V) displacement preferably occurs instead
It answers, and such as palladium (Pd2+/ Pd:0.915V), it is bad that the quality of coating for occurring or obtaining will be difficult.Simultaneously in replacement process, apply
Inevitably there is loss, and the more stabilization that will affect gold plating liquid of metal ion active present in plating solution in coating
Property, shorten its service life.
Restoring gold-plated is to form Gold plated Layer, again being restored the gold ion in gold plating liquid in plating layer surface with reducing agent
Matrix catalysis reduction and self catalyzed reduction can be divided into according to the catalysis oxidation type of reducing agent.Matrix catalysis is reducing agent in base
It is aoxidized under the catalysis of body metal, is restored to gold ion and electronics is provided, after basis material is capped, the catalysis oxidation of reducing agent becomes
Weak, the coating later period increasess slowly；Self-catalysis is that the metal for restoring metal ion by reducing agent, and being reduced can be catalyzed
Reduction reaction occurs for subsequent metal, which can obtain thicker coating.But standard electrode potential (the Au of gold+/ Au:
1.692V) very just, if in order to improve deposition rate and plated thickness, in the presence of using reducing agent, gold plating liquid
Stability will receive influence, be easy to turn over slot；And in order to safeguard the stability of gold plating liquid, it is forced using weak reductant, practical life
Production will limit deposition rate and deposition thickness.
Additionally, due to the presence of " Jia Fanni " effect, so that layer gold surface portion electronegativity is higher, so as to cause layer gold
Homogeneity question influences the corrosion resistance of pcb board in use.
At this stage in technology, chemical gold plating liquid described in the patent of invention just like Publication No. CN106399983A should
Gold-plated formula of liquid is with good stability, but present market demands are not achieved in plated thickness；For another example Publication No.
Chemical gold plating liquid described in the patent of invention of CN105745355A, the gold-plated formula of liquid can obtain smooth, uniform coating,
But the thickness of Gold plated Layer is not able to satisfy the present market demand；For another example described in the patent of invention of Publication No. CN105543816A
Chemical gold plating liquid, the thickness of coating which can obtain accords with the demands of the market, but which employs inferior sulfate radical conducts
The stability value of primary complexing agent, gold plating liquid must be discussed, and the stabilizer thiocarbamide being added will affect the solderability of layer gold.
Summary of the invention
For defect existing for existing chemical gilding technology, the purpose of the present invention is to provide a kind of complex reducing agent is fast
Speed reduction gold plating liquid, the excellent in stability of gold plating liquid, gold-plated rate is fast, and it is gold-plated to be capable of forming the bright and fine and close thickness of surfacing
Layer.
A kind of chemistry quickly reduction gold plating liquid, including following density component: water-soluble gold compound (in terms of Au) 0.5~
1.5g/L, 5~20g/L of sodium hypophosphite, 1~5g/L of hydroxyl sulfate, 25~55g/L of Triammonium citrate, ethylenediamine tetra-acetic acid two
5~15g/L of sodium, 0.1~3.0g/L of amino acid, mercapto-polyglycol 0.001~0.02g/L of-R, cetylpyridinium bromide 0.001
~0.02g/L, 0.001~0.005g/L of ligninsulfonate, 0.01~0.1g/L of dimethyamine borane, tartaric acid germanium 0.01~
0.3g/L。
Preferably, quickly golden liquid, including following density component: water-soluble gold compound are crossed in reduction to the chemistry (in terms of Au)
0.5~1.5g/L, 5~20g/L of sodium hypophosphite, 1~5g/L of hydroxyl sulfate, 30~50g/L of Triammonium citrate, ethylenediamine tetrem
5~15g/L of acid disodium, 0.5~1.5g/L of amino acid, mercapto-polyglycol 0.01~0.02g/L of-R, cetylpyridinium bromide
0.01~0.02g/L, 0.001~0.005g/L of ligninsulfonate, 0.01~0.1g/L of dimethyamine borane, tartaric acid germanium 0.02
~0.2g/L.
Preferably, the concentration of the sodium hypophosphite is 8~20g/L, and the concentration of the hydroxyl sulfate is 1.5~5g/L.
Preferably sodium hypophosphite and hydroxyl sulfate concentration, composite reduction effect can be formed, sodium hypophosphite is urged as matrix
Change reducing agent, can be in nickel and palladium surface reduction gold ion, while the corrosion of nickel being inhibited to be precipitated；Hydroxyl sulfate as self-catalysis also
Former agent can continue to restore gold ion after layer gold is formed, promote layer gold thickness.Simultaneously in gold plating process, sodium hypophosphite and
The synergistic effect of hydroxyl sulfate greatly promotes gold-plated rate, while improving the corrosion resistance of coating.
Preferably, the dimethyamine borane concentration is 0.01~0.06g/L.Preferably dimethyamine borane it is dense
Degree is added after each golden slot heats up, dimethyamine borane more than 70 DEG C at a temperature of, generation H atom can be decomposed, be adsorbed on
It is used as active site on matrix, promotes the initial rate of chemical gilding, and will not influence the stability of gold plating liquid.
Preferably, the concentration of the Triammonium citrate is 35~45g/L, and the concentration of disodium ethylene diamine tetraacetate is 5~8g/
L。
Wherein, above-mentioned chemistry is quickly in reduction gold plating liquid, the amino acids be in amino acid and its derivative at least
It is a kind of；Such as glycine, glutamic acid etc..
Preferably Triammonium citrate, disodium ethylene diamine tetraacetate and amino acid concentration, be added as complexant, can
Strong coordination is carried out with gold ion, improves the stability of gold plating liquid.
Wherein, above-mentioned chemistry quickly restores in gold plating liquid, and the mercapto-polyglycol-R, R can be amino, carboxyl and first
At least one of oxygroup.Institute preferably mercapto-polyglycol-R can with gold ion carry out coordination, and sulfydryl can with
The gold particle for being deposited on coating surface combines, and facilitates the enrichment of surface gold ion and orderly deposits, thus accelerate deposition rate,
And improve surface texture.
Wherein, it is above-mentioned chemistry quickly reduction gold plating liquid in, the cetylpyridinium bromide be selected from dodecylpyridinium bromide or
Person's cetyl pyridinium bromide.Preferably, the concentration of the cetyl pyridinium bromide is 0.004~0.01g/L.Institute is preferably
The concentration of cetyl pyridinium bromide can improve the surface shape between sedimentary and plating solution as cationic surfactant
State, it is easier to be adsorbed on the matrix surface in negative potential, inhibit " Jia Fanni " effect, promote the uniformity of layer gold.
Preferably, the concentration of wooden sulfonate is 0.001~0.003g/L, the wooden sulphur in the gold plating liquid
Hydrochlorate is selected from least one of wooden sodium sulfonate, wooden potassium sulfonate and wooden sulfoacid calcium etc..Wooden sulfonate is as dispersing agent, energy
Enough disperse the gold ion in plating solution, safeguards the stability of plating solution, disperse the gold ion of deposition surface, it is uniform to reach thickness of coating
Controllably.
Preferably, the concentration of tartaric acid germanium is 0.02~0.08g/L in the gold plating liquid.Tartaric acid germanium can mention
High suitable germanium ion, the underpotential deposition in the layer gold of deposition improve gold-plated deposition rate.
Wherein, above-mentioned chemistry quickly restores in gold plating liquid, and the pH range of the gold plating liquid is between 6.0~7.0；Preferably
6.3~6.8.
The present invention also provides quickly application of the reduction gold plating liquid in terms of printed circuit board surface processing of above-mentioned chemistry.
Preferably, in above-mentioned application, when being surface-treated to printed circuit board the plating temperature of gold plating liquid 82~
95℃；Preferably 83~86 DEG C.
The beneficial effects of the present invention are:
Complex reducing agent provided by the invention quickly restores in gold plating liquid (abbreviation gold plating liquid), passes through each group of the concentration
The coordinated effect for dividing substance, can greatly improve the properties of chemical gilding, safeguard the stability of gold plating liquid, improve gold-plated
Deposition velocity improves the surface nature of coating, makes that Gold plated Layer is brighter, smooth, fine and close and thickness is uniform.In addition, using institute
The chemistry stated quickly restores gold plating liquid, and gained thickness Gold plated Layer has better corrosion resistance, tin plating to flow back and beat gold thread performance,
It can be further improved the reliability and its service life of wiring board.
Detailed description of the invention
Fig. 1 is the influence diagram of hydroxyl sulfate, ascorbic acid and hydrazine hydrate to gold plating liquid degradation result.
Fig. 2 is embodiment 2 and the gold-plated deposition rate comparison diagram of comparative example 1.
Fig. 3 is printed circuit board Gold plated Layer SEM figure.
Specific embodiment
Following case study on implementation is intended to further illustrate the content of present invention, rather than limits the protection model of the claims in the present invention
It encloses, below with reference to specific example, the present invention is described in more detail.
Preparation example
Ni-Pd-Au layers are once obtained on printed circuit board, the specific steps are as shown below:
Alkali cleaning (50 DEG C, 5min) → washing (distilled water, room temperature, 2min) → acid etching cleaning agent (50 DEG C, 5min) → hot water
Wash (distilled water, 45 DEG C, 2min) → washing (distilled water, room temperature, 2min) → microetch (sodium peroxydisulfate 50g/L, sulfuric acid 40ml/L,
Room temperature, 3min) → pickling (sulfuric acid 100ml/L) → washing (distilled water, room temperature, 2min) → activation (activation palladium liquid, room temperature,
2min) → washing (distilled water, room temperature, 2min) → nickel plating (80~84 DEG C, 20min) → washing (distilled water, room temperature, 2min) →
Plate palladium (50 DEG C, 20min) → washing (distilled water, room temperature, 2min) → gold-plated (pH=6.3-6.8,86 DEG C, 20min) → washing
(distilled water, room temperature, 2min) → drying.
Gold plating liquid used is as shown in embodiment 1-6 and comparative example 1-10 when gold-plated.
Embodiment 1-6
Embodiment 1-6 gold plating liquid component is shown in Table 1.
1 embodiment 1-6 gold plating liquid component of table
Comparative example 1-10
Comparative example 1-10 gold plating liquid component is shown in Table 2.
2 comparative example 1-10 gold plating liquid component of table
Embodiment 7
It is measured using XRF calibrator coated coating thickness；The brightness of layer gold appearance can pass through magnifying glass and range estimation
It obtains, and binding force can be measured with tape method, brightness and binding force point are 5 grades from 1 to 5, and binding force and brightness are more excellent
Series is higher；The period of plating solution is judged by recycling plating, and (substrate plating gold carries out circulation experiment, is building bath gold concentration
In the case of the plating solution of 0.2g/L, the plating of gold analysis to the amount on substrate of 0.2g/L is become into 1MTO)；The uniformity of coating passes through
Scanning electron microscope assessment；Resistance to corrosion is measured by activation polarization, carries out the calculating of porosity.Embodiment 1-6 test
It the results are shown in Table 3, comparative example 1-10 test result is shown in Table 4.
3 embodiment 1-6 test result of table
4 comparative example 1-10 test result of table
Above embodiments 1,2,3,4,5,6 are centainly comparing in gold salt, reducing agent, complexant, organic additive and accelerator
When example, result of implementation is excellent.In conjunction with comparative example 1,2 as can be seen that when sodium hypophosphite is used alone, gold-plated rate is reduced；And
If improving the concentration of sodium hypophosphite, gold plating liquid stability is poor, thus improves the concentration of single reducing agent merely to improve deposition
Rate be it is insecure, the addition of hydroxyl sulfate is simultaneously in the composite reduction of sodium hypophosphite effect effective solution deposition rate
Fast and problem that plating solution is unstable；Comparative example 2,3 is as can be seen that gold salt, reducing agent and complexant concentration must keep certain
Proportion, when reductant concentration is excessively high, bath stability decline, deposition rate is accelerated, and it is unreliable to deposit, coating uniformity decline
And it is loose, porosity increases, corrosion resistance reduces；Comparative example 4,5,6 can be seen that must being used in combination for organic additive,
And certain proportion is kept with gold salt, when not using mercapto-polyglycol methoxyl group or cetyl pyridinium bromide, coating is equal
Even property decline, porosity increase, and corrosion resistance reduces, and when a kind of concentration of certain organic additive is excessive or too small, it is same to plate
Layer uniformity decline, porosity increase, and corrosion resistance reduces；Comparative example 7 can be seen that when not using accelerator, gold-plated speed
Rate slightly reduces.In comparative example 8,9,10, when component is more than gold plating liquid and Gold plated Layer quality described in claim in gold plating liquid
On declined, excellent result of implementation cannot be obtained.
8 gold plating liquid stability test of embodiment
Laser heating 10h, observation plating solution variation at 90 DEG C by gold plating liquid.Gold plating liquid forms substantially: water-soluble aurification is closed
Object (in terms of Au) 1.0g/L, sodium hypophosphite 15g/L, Triammonium citrate 40g/L, disodium ethylene diamine tetraacetate 10g/L, first sulphur ammonia
Sour 1.0g/L, mercapto-polyglycol hydroxyl 0.008g/L, cetyl pyridinium bromide 0.007g/L, ligninsulfonate 0.002g/
L, tartaric acid germanium 0.06g/L, dimethyamine borane 0.03g/L.It is separately added into hydroxyl sulfate, hydrazine hydrate and the Vitamin C of 1-5g/L
Acid carries out heat ageing test.Test results are shown in figure 1.
Comparison diagram 1 can be seen that the addition of ascorbic acid, so that the plating solution of above-mentioned composition, after degradation, plating solution is in
Yellow and have precipitating generate；The addition of hydrazine hydrate, so that the gold plating liquid of above-mentioned composition after senile experiment, generates black precipitate；
And the addition of hydroxyl sulfate, and have not been changed the stability of above-mentioned composition gold plating liquid.
The test of 9 deposition rate of embodiment
The difference of above-described embodiment 2 and comparative example 1 with unused hydroxyl sulfate, Fig. 2 be its deposition rate comparison diagram.From
In figure as can be seen that under complex reducing agent, after plating 1min, the deposition rate of complex reducing agent, which is significantly greater than, is used alone time Asia
Deposition rate under sodium phosphate, acceleration is obviously played in the addition of hydroxyl sulfate, and bath stability is good.
In conclusion gold plating liquid provided by the present invention, under the gold salt concentration and corresponding each component concentration,
Stability is good, and energy surface is uniform, bright, the excellent chemical plating layer gold of binding force, and the compound market demands of layer gold thickness, anti-corruption
Erosion is had excellent performance.
Claims (10)
1. a kind of chemistry quickly restores gold plating liquid, which is characterized in that the gold plating liquid includes following density component: water-soluble aurification is closed
Object (in terms of Au) 0.5~1.5g/L, 5~20g/L of sodium hypophosphite, 1~5g/L of hydroxyl sulfate, 25~55g/L of Triammonium citrate,
5~15g/L of disodium ethylene diamine tetraacetate, 0.1~3.0g/L of amino acid, mercapto-polyglycol 0.001~0.02g/L of-R, alkyl
0.001~0.02g/L of pyridinium bromide, 0.001~0.005g/L of ligninsulfonate, 0.01~0.1g/L of dimethyamine borane, wine
0.01~0.3g/L of stone acid germanium.
2. the quick reduction gold plating liquid of chemistry according to claim 1, which is characterized in that the concentration of the sodium hypophosphite is
8~20g/L, the concentration of the hydroxyl sulfate are 1.5~5g/L.
3. the quick reduction gold plating liquid of chemistry according to claim 1, which is characterized in that the dimethyamine borane concentration is
0.01~0.06g/L.
4. the quick reduction gold plating liquid of chemistry according to claim 1, which is characterized in that the concentration of the citric acid tri-amonia is
35~45g/L, the concentration of disodium ethylene diamine tetraacetate are 5~8g/L.
5. it is according to claim 1 chemistry quickly reduction gold plating liquid, which is characterized in that the amino acid be amino acid and its
At least one of derivative.
6. chemistry according to claim 1 quickly restores gold plating liquid, which is characterized in that in the mercapto-polyglycol-R
R is at least one of amino, carboxyl and methoxyl group.
7. chemistry according to claim 1 quickly restores gold plating liquid, which is characterized in that the cetylpyridinium bromide is selected from ten
Dialkyl group pyridinium bromide or cetyl pyridinium bromide.
8. the quick reduction gold plating liquid of chemistry according to claim 1, which is characterized in that the concentration of the wooden sulfonate is
0.001~0.003g/L, the wooden sulfonate in wooden sodium sulfonate, wooden potassium sulfonate and wooden sulfoacid calcium at least one
Kind.
9. chemistry according to claim 1 quickly restores gold plating liquid, which is characterized in that the pH range of the gold plating liquid exists
Between 6.0~7.0.
10. any one of claim 1~9 chemistry quickly restores gold plating liquid answering in terms of printed circuit board surface processing
With.
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| CN113046736A (en) * | 2021-03-02 | 2021-06-29 | 深圳市创智成功科技有限公司 | Cyanide-free chemical gold-precipitating solution for display panel field and process thereof |
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| CN114351129A (en) * | 2021-11-22 | 2022-04-15 | 赣州鑫冠科技股份有限公司 | Cyanide-free gold plating solution for loudspeaker frame |
| CN117987815A (en) * | 2024-01-31 | 2024-05-07 | 珠海斯美特电子材料有限公司 | High-stability reduction type electroless gold plating solution and application thereof |
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