CN112593220A - Cyanide-free chemical gold-deposition solution suitable for semiconductor and display panel - Google Patents
Cyanide-free chemical gold-deposition solution suitable for semiconductor and display panel Download PDFInfo
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- CN112593220A CN112593220A CN202011454923.6A CN202011454923A CN112593220A CN 112593220 A CN112593220 A CN 112593220A CN 202011454923 A CN202011454923 A CN 202011454923A CN 112593220 A CN112593220 A CN 112593220A
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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 discloses a cyanide-free chemical gold-precipitating solution suitable for semiconductors and display panels, which consists of the following components: the cyanide-free gold salt comprises, by content of Au ions, 4-5 g/L, 20-100 g/L of a complexing agent, 2-5g/L of a reducing agent, 0.05-0.2 g/L of a surfactant, 30-60g/L of a buffering agent and 0.2-5mg/L of a stabilizing agent, wherein the pH is adjusted to 7-9 by sulfuric acid or potassium hydroxide, the balance is water, and the operating temperature is 50-90 ℃. The gold plating layer obtained by the invention has good adhesiveness, uniform plating layer, high deposition rate and stable plating solution. Meanwhile, the cyanide-free chemical gold precipitation solution does not use potassium gold cyanide high-toxicity substances and does not contain cyanide, thereby reducing the health influence on operators and the potential safety hazard of the working environment and greatly reducing the burden and the influence of wastewater treatment.
Description
Technical Field
The invention relates to the technical field of semiconductor and display panel surface treatment, in particular to a cyanide-free chemical gold-plating solution suitable for a semiconductor and a display panel.
Background
In the production process of the printed circuit board, after the copper circuit is formed, other metals are required to be formed on the copper circuit to protect the copper circuit, so that oxidation is prevented, and in addition, the functions of routing, welding and the like can be realized, and the copper circuit and other components are interconnected and communicated. The traditional method is realized by chemical tin deposition, chemical silver deposition, chemical nickel gold and the like. The electroless nickel-gold process has the most extensive application because of the good functions of welding, routing and the like. In the electroless nickel-gold technique for copper substrates, electroless gold is mainly performed by means of displacement. The gold ions and the nickel layer formed in advance have a replacement reaction, and the gold ions form a gold plating layer to be deposited on the nickelA gold layer is formed on the surface. Most of the existing chemical gold precipitation adopts potassium gold cyanide (KAu (CN)2]The prepared gold leaching solution has the advantages of stable bath solution, low cost and good plating performance, and can be used for a long time. However, potassium aurocyanide is a highly toxic substance, and its highly toxic property brings great influence and hidden trouble to operators and factory management, and at the same time, makes waste liquid treatment more difficult, and brings great influence and burden to the environment. For cyanide-free chemical gold, some patents are published in China at present, but a certain distance is left from actual production. Patent CN 103993300B (CN 102212805A) discloses a cyanide-free electroless gold plating solution, which uses potassium gold citrate as gold salt, but the potassium gold citrate still contains cyanide, which is proved by authority departments, and is not true cyanide-free electroless gold.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides the cyanide-free chemical gold-precipitating solution suitable for the semiconductor and the display panel. Meanwhile, the cyanide-free chemical gold precipitation solution does not use potassium gold cyanide high-toxicity substances and does not contain cyanide, thereby reducing the health influence on operators and the potential safety hazard of the working environment and greatly reducing the burden and the influence of wastewater treatment.
In order to achieve the purpose, the invention provides a cyanide-free chemical gold-plating solution suitable for semiconductors and display panels, which comprises the following components in percentage by mass:
cyanide-free gold salt, which is 4-5 g/L calculated by the content of Au ions
20-100 g/L complexing agent
2-5g/L of reducing agent
0.05-0.2 g/L of surfactant
Buffer 30-60g/L
0.2-5mg/L stabilizer
The components are uniformly mixed according to the proportion, the pH is adjusted to 7-9 by using sulfuric acid or potassium hydroxide, the balance is water, and the operation temperature is 50-90 ℃.
The complexing agent comprises two of sodium sulfite and 1- (4-ethylphenyl) -2-thiourea, and the mass mixing ratio of the two is 0.3-3: 1.
Wherein the cyanide-free gold salt is sodium gold sulfite.
Wherein the buffer is one or two of ammonium chloride and ammonium citrate.
Wherein the reducing agent is one or more of vitamin C and sodium borohydride.
The surfactant is sodium methallylsulfonate.
Wherein the stabilizer is antimony potassium tartrate.
The invention has the beneficial effects that: compared with the prior art, the cyanide-free chemical gold-plating solution suitable for the semiconductor and the display panel,
1) by using sulfite and 1- (4-ethyl phenyl) -2-thiourea as a complexing agent of gold ions, the gold ions can be kept from being separated out and precipitated. In order to prevent the sulfite from being oxidized by air to cause a decrease in concentration, an excessive amount of sodium sulfite and 1- (4-ethylphenyl) -2-thiourea may be present in the solution as a complexing agent to maintain the stability of the plating solution. The single complexing agent has a narrow operation range, for example, when the pH value is lower than 7, sulfite has the risk of hydrolysis, 1- (4-ethylphenyl) -2-thiourea added can play a role in stabilizing gold ions in order to ensure the stability of the gold plating solution, but when the pH value is too high, the 1- (4-ethylphenyl) -2-thiourea is easily oxidized, and at the moment, the sulfite can ensure the stability of the solution.
2) The gold plating layer obtained by the invention has good adhesiveness, uniform plating layer, high deposition rate and stable plating solution. Meanwhile, the cyanide-free chemical gold precipitation solution does not use potassium gold cyanide high-toxicity substances and does not contain cyanide, thereby reducing the health influence on operators and the potential safety hazard of the working environment and greatly reducing the burden and the influence of wastewater treatment.
Drawings
FIG. 1 shows the cyanide-free chemical gold product obtained by the present invention;
FIG. 2 shows the circuit of the present invention with cyanide-free electroless gold coating.
Detailed Description
In order to more clearly describe the present invention, the present invention is further described below.
The invention provides a cyanide-free chemical gold-plating solution suitable for semiconductors and display panels, which comprises the following components in percentage by mass:
cyanide-free gold salt, which is 4-5 g/L calculated by the content of Au ions
20-100 g/L complexing agent
2-5g/L of reducing agent
0.05-0.2 g/L of surfactant
Buffer 30-60g/L
0.2-5mg/L stabilizer
The components are uniformly mixed according to the proportion, the pH is adjusted to 7-9 by using sulfuric acid or potassium hydroxide, the balance is water, and the operation temperature is 50-90 ℃.
In the embodiment, the complexing agent is sodium sulfite and 1- (4-ethylphenyl) -2-thiourea, and the mass mixing ratio of the sodium sulfite and the 1- (4-ethylphenyl) -2-thiourea is 0.3-3: 1.
In the invention, the gold sodium sulfite is used as a gold ion source and is cyanide-free gold salt, and in a cyanide-free system, the gold ions can be kept from being separated out and precipitated by using sulfite and 1- (4-ethylphenyl) -2-thiourea as a complexing agent of the gold ions. In order to prevent the sulfite from being oxidized by air to cause a decrease in concentration, an excessive amount of sodium sulfite and 1- (4-ethylphenyl) -2-thiourea may be present in the solution as a complexing agent to maintain the stability of the plating solution. The single complexing agent has a narrow operation range, for example, when the pH value is lower than 7, sulfite has the risk of hydrolysis, 1- (4-ethylphenyl) -2-thiourea added can play a role in stabilizing gold ions in order to ensure the stability of the gold plating solution, but when the pH value is too high, the 1- (4-ethylphenyl) -2-thiourea is easily oxidized, and at the moment, the sulfite can ensure the stability of the solution.
Because gold ions are easily complexed by sulfite and 1- (4-ethylphenyl) -2-thiourea, the oxidation potential of gold is greatly reduced, and the system belongs to a strong reduction system, but can still keep stable, namely, when the gold ions meet the sulfite, the oxidation-reduction reaction is not carried out, but the complexation reaction is carried out. Other strong reducing agents such as vitamin C and sodium borohydride in the invention have no complexing effect on gold, and during electroless gold plating, gold ions can oxidize the vitamin C or the sodium borohydride and deposit on the surface of a product to form a gold plating layer. In practical production, bubbles may adhere to some surfaces due to the shape limitation of the product, and thus, the product is isolated from the plating solution, resulting in that the gold layer cannot be deposited. In order to solve this problem, some surfactant is often added to the bath to lower the surface tension of the liquid, so that bubbles are easily released from the workpiece. However, conventional surfactants do not readily dissolve at high temperatures or in high solute solutions, resulting in turbid baths with a greatly compromised effect. In the invention, the sodium methallyl sulfonate is used as a surfactant, which can not cause tank liquor turbidity, and more importantly, the surfactant is a foamless surfactant, can not stimulate foam generation in the movement of liquid medicine, is easy to clean and is convenient to produce and maintain.
In order to obtain stable gold deposition rate, antimony potassium tartrate is added as a stabilizer for electroless gold plating, and the deposition rate can be more stable like a stabilizer in electroless nickel plating.
It is clear that cyanide-free electroless gold plating requires heating at too low a temperature, the oxidation potential of the gold ions is too low due to chelation by the complexing agent, and the deposition rate of gold is slow. In the invention, the deposition rate of gold is obviously improved when the temperature is above 50 ℃. However, when the temperature is too high, the water in the bath solution evaporates too fast, and the maintenance is relatively troublesome, so the proper temperature is 60-70 ℃.
In addition, because the gold salt is gold sodium sulfite, the stability of sulfite has high requirements on the pH value of the bath solution, the bath solution needs to be strictly controlled in a weakly alkaline environment, the pH value is optimal within 7-9, if the bath solution is weakly acidic, the sulfite is easy to hydrolyze to generate sulfur dioxide and water, and if the alkalinity is too strong, the reduction potential of a reducing agent and redundant sodium sulfite in the bath solution can be greatly reduced, so that the bath solution is easy to lose effectiveness due to air oxidation.
Therefore, in order to maintain the stability of the pH value of the bath solution, substances capable of stabilizing the pH value of the bath solution are required to be added into the bath solution, and ammonium chloride and ammonium citrate are used as buffering agents to maintain the stability of the pH value of the bath solution.
The chemical gold immersion solution system does not use gold potassium cyanide high-toxicity substances, does not contain cyanogen elements, reduces the health influence on operators and the potential safety hazard of working environment, also greatly reduces the burden and influence on the environment, and simultaneously has stable plating layer, good adhesiveness and uniform distribution of the gold plating layer.
In this embodiment, the cyanide-free gold salt is sodium gold sulfite. The buffer is one or two of ammonium chloride and ammonium citrate. The reducing agent is one or more of vitamin C and sodium borohydride. The surfactant is sodium methallylsulfonate. The stabilizer is antimony potassium tartrate.
Each liter of chemical immersion gold working solution comprises the following components:
the cyanide-free gold salt comprises the following components in percentage by content of Au ions: 4-5 g/L;
complexing agent: 20-100 g/L;
reducing agent: 2-5 g/L;
surfactant: 0.05-0.2 g/L;
buffering agent: 30-60 g/L;
adjusting the pH value to 7-9 by using sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: 50-90 ℃.
The following are several specific examples of the invention
Example 1
The cyanide-free chemical gold-plating solution comprises the following components by 1 liter:
the cyanide-free gold salt comprises the following components in percentage by content of Au ions: 4 g/L;
complexing agent: 20 g/L;
reducing agent: 2 g/L;
surfactant: 0.05 g/L;
antimony potassium tartrate: 2mg/L
Buffering agent: 30 g/L;
adjusting the pH to 7.2 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: at 50 ℃.
The cyanide-free gold salt is sodium gold sulfite, and the complexing agent is sodium sulfite, wherein the mass ratio of 1- (4-ethylphenyl) -2-thiourea is 1: 1, the reducing agent is sodium borohydride, the surfactant is sodium methallyl sulfonate, and the buffering agent is ammonium chloride.
Example 2
The cyanide-free chemical gold-plating solution comprises the following components by 1 liter:
the cyanide-free gold salt comprises the following components in percentage by content of Au ions: 4.2 g/L;
complexing agent: 100 g/L;
reducing agent: 5 g/L;
surfactant: 0.2 g/L;
antimony potassium tartrate: 0.2 mg/L;
buffering agent: 60 g/L;
adjusting the pH to 9.0 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: at 90 ℃.
The cyanide-free gold salt is sodium gold sulfite, and the complexing agent is sodium sulfite, wherein the mass ratio of 1- (4-ethylphenyl) -2-thiourea is 2: 1, the reducing agent is sodium borohydride, the surfactant is sodium methallyl sulfonate, and the buffering agent is ammonium chloride.
Example 3
The cyanide-free chemical gold-plating solution comprises the following components by 1 liter:
the cyanide-free gold salt comprises the following components in percentage by content of Au ions: 4.5 g/L;
complexing agent: 20 g/L;
reducing agent: 2 g/L;
surfactant: 0.05 g/L;
antimony potassium tartrate: 5 mg/L;
buffering agent: 30 g/L;
adjusting the pH to 7.2 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: at 50 ℃.
The cyanide-free gold salt is sodium gold sulfite, and the complexing agent is sodium sulfite, wherein the mass ratio of 1- (4-ethylphenyl) -2-thiourea is 1: 2, the reducing agent is vitamin C, the surfactant is sodium methallyl sulfonate, and the buffering agent is ammonium citrate.
Example 4
The cyanide-free gold salt comprises the following components in percentage by content of Au ions: 4.6 g/L;
complexing agent: 100 g/L;
reducing agent: 5 g/L;
surfactant: 0.2 g/L;
buffering agent: 60 g/L;
adjusting the pH to 8.0 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: 80 ℃.
The cyanide-free gold salt is sodium gold sulfite, the complexing agent is sodium sulfite, and the mass ratio of 1- (4-ethylphenyl) -2-thiourea is 2: 1, the reducing agent is vitamin C, the surfactant is sodium methallyl sulfonate, and the buffering agent is ammonium citrate.
Example 5
The cyanide-free gold salt comprises the following components in percentage by content of Au ions: 5 g/L;
complexing agent: 50 g/L;
reducing agent: 3 g/L;
surfactant: 0.1 g/L;
buffering agent: 45 g/L;
adjusting the pH to 8.1 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: 80 ℃.
The cyanide-free gold salt is sodium gold sulfite, the complexing agent is sodium sulfite, and the mass ratio of 1- (4-ethylphenyl) -2-thiourea is 1: 1, wherein the reducing agent is 1: 1, the surfactant is sodium methallylsulfonate, and the buffer is ammonium citrate and ammonium chloride 1: 1 of a mixture.
The cyanide-free chemical gold-deposition solution obtained in the embodiment of the invention is used for carrying out gold-deposition operation on a printed circuit board, the gold-deposition time is 10 minutes, the plating layer is smooth and clean and stable, the adhesiveness is good, the distribution is uniform, specifically, as shown in figure 1-2, a gold wire circuit is flat, has no fault, has uniform color and luster, and the photoresist has no abnormality such as damage, deformation, falling and the like, so that normal circuit conduction can be realized.
The above disclosure is only an example of the present invention, but the present invention is not limited thereto, and any variations that can be made by those skilled in the art should fall within the scope of the present invention.
Claims (7)
1. A cyanide-free chemical gold immersion solution suitable for semiconductors and display panels is characterized by comprising the following components in percentage by mass:
cyanide-free gold salt, which is 4-5 g/L calculated by the content of Au ions
20-100 g/L complexing agent
2-5g/L of reducing agent
0.05-0.2 g/L of surfactant
Buffer 30-60g/L
0.2-5mg/L stabilizer
The components are uniformly mixed according to the proportion, the pH is adjusted to 7-9 by using sulfuric acid or potassium hydroxide, the balance is water, and the operation temperature is 50-90 ℃.
2. The cyanide-free electroless gold plating solution suitable for semiconductors and display panels as claimed in claim 1, wherein the complexing agent is sodium sulfite or 1- (4-ethylphenyl) -2-thiourea, and the mass mixing ratio of the two is 0.3-3: 1.
3. The cyanide-free electroless gold plating solution for semiconductors and display panels as claimed in claim 1, wherein the cyanide-free gold salt is sodium gold sulfite.
4. The cyanide-free electroless gold plating solution for semiconductors and display panels as claimed in claim 1, wherein the buffer is one or both of ammonium chloride and ammonium citrate.
5. The cyanide-free electroless gold plating solution for semiconductors and display panels as claimed in claim 1, wherein the reducing agent is one or more of ascorbic acid and sodium borohydride.
6. The cyanide-free electroless gold plating solution for semiconductors and display panels as claimed in claim 1, wherein the surfactant is sodium methallylsulfonate.
7. The cyanide-free electroless gold plating solution for semiconductors and display panels as claimed in claim 1, wherein the stabilizer is antimony potassium tartrate.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111349917A (en) * | 2018-12-24 | 2020-06-30 | 天津环鑫科技发展有限公司 | Gold plating solution for semiconductor chip, gold plating method and nickel and gold plating method |
| CN114032529A (en) * | 2021-11-17 | 2022-02-11 | 江苏矽智半导体科技有限公司 | Chemical nickel plating solution and chemical nickel plating process for wafer-level packaging product |
| 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 |
| CN114481107A (en) * | 2022-02-18 | 2022-05-13 | 深圳市创智成功科技有限公司 | Gold-precipitating solution for cyanide-free chemical heavy gold precipitation and process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN114481107A (en) * | 2022-02-18 | 2022-05-13 | 深圳市创智成功科技有限公司 | Gold-precipitating solution for cyanide-free chemical heavy gold precipitation and process thereof |
| CN114481107B (en) * | 2022-02-18 | 2022-11-01 | 深圳市创智成功科技有限公司 | Gold-precipitating solution for cyanide-free chemical heavy gold precipitation and process thereof |
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