CN113026068B - Cyanide-free electroless gold plating solution applied to advanced wafer packaging field and gold plating process thereof - Google Patents
Cyanide-free electroless gold plating solution applied to advanced wafer packaging field and gold plating process thereof Download PDFInfo
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- CN113026068B CN113026068B CN202110231405.6A CN202110231405A CN113026068B CN 113026068 B CN113026068 B CN 113026068B CN 202110231405 A CN202110231405 A CN 202110231405A CN 113026068 B CN113026068 B CN 113026068B
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- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- C25D21/00—Processes for servicing or operating cells for electrolytic coating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
The invention discloses a cyanide-free chemical gold plating solution applied to the field of advanced wafer packaging and a gold plating process thereof, wherein the cyanide-free chemical gold plating solution comprises the following components: cyanide-free gold salt, wherein the content of Au ions is 6-10 g/L; 10-60g/L of complexing agent; 10-60g/L of conductive salt; 30-60g/L of buffer; 5-10g/L of anti-aging agent; 15-80mg/L of surfactant; 1-5mg/L of wetting agent; reaction accelerator 50-80 mg/L; 0.2-5mg/L stabilizer; the reaction accelerator is a compound of 2, 6-diaminopyridine and 3-pyridinemethanol, and the mass concentration ratio of the 2, 6-diaminopyridine to the 3-pyridinemethanol is 2: 1. The solution obtained by the invention not only ensures the stability of the plating solution, but also ensures that the plated part is easy to spread on the surface of the electrode to achieve the purpose of uniform plating, and further achieves the effect of filling the wafer packaging micropores without holes and gaps.
Description
Technical Field
The invention relates to the technical field of surface treatment, in particular to a cyanide-free chemical gold-plating solution applied to the field of advanced wafer packaging and a gold-plating process thereof.
Background
Wafer level packaging, which is generally oriented to perform most or all of the packaging test procedures directly on the wafer and then cut into individual components, has the advantages of smaller package size and better electrical performance, and is mainly used for various semiconductor products, and the requirements mainly come from the characteristic requirements of portable products for being light, thin, short and small.
In the production process of the wafer level packaging product, 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 wafer level packaging product 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.
The gold plating layer can meet various assembly requirements and has the performances of weldability, conductivity, high stability, oxidation resistance and the like. The first chemical gold plating all uses cyanide-containing gold salt as raw material, because cyanide plating solution contains extremely toxic cyanide, great unsafe factors can be generated in the actual production process and the relevant subsequent waste water, waste gas treatment and disposal, so that the development of the cyanide gold plating solution is limited, and with the improvement of environmental protection consciousness of people, cyanide-free gold plating technology is adopted more and more in the prior art, but the prior cyanide-free gold plating technology has the following defects:
1) during electroplating, the gold plating is easy to have defects such as voids, cracks and the like, so that perfect seamless electroplating filling cannot be achieved, and the effect of uniform plating cannot be achieved all the time.
2) The current efficiency and stability of the existing plating solution, the corrosion resistance of a plating layer and the brightness of the appearance have certain differences with a cyanide plating layer.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides a cyanide-free chemical gold-plating solution applied to the field of advanced wafer packaging and a gold-plating process thereof, wherein the solution achieves the effect of filling micropores of wafer packaging without holes and gaps; the process not only ensures the uniformity of electroplating, but also shortens the electroplating time.
In order to achieve the purpose, the invention provides a cyanide-free electroless gold plating solution applied to the field of advanced wafer packaging, which comprises the following components in mass concentration:
the reaction accelerator is a compound of 2, 6-diaminopyridine and 3-pyridinemethanol, and the mass concentration ratio of the 2, 6-diaminopyridine to the 3-pyridinemethanol is 2: 1;
after the components are uniformly mixed according to the proportion, the pH value is adjusted to 7-9 by using sulfuric acid or potassium hydroxide, the balance is water, and the cyanide-free electroless gold plating solution is formed after the operation temperature is 50-90 ℃.
Wherein the mass concentration ratio of the surfactant to the wetting agent in use is 15: 1.
Wherein the complexing agent is a 1, 2-ethanediamine compound; and the concentration sum of the conductive ions in the complexing agent and the conductive ions in the conductive salt is 10-15 mol/L.
Wherein the cyanide-free gold salt is tetrachloro-gold acid or gold hydroxide.
Wherein the buffer is one or two of ammonium chloride and ammonium citrate.
Wherein the surfactant is sodium methallyl sulfonate.
Wherein the stabilizer is antimony potassium tartrate.
In order to achieve the above object, the present invention further provides a cyanide-free electroless gold plating process applied to the field of advanced wafer packaging, comprising the following steps:
step 1, performing vacuum treatment on a plated part by using a pretreatment solution before chemical plating;
step 2, carrying out intermediate nickel plating treatment on the vacuumized plated piece to form a nickel plated layer;
step 3, putting the plated piece with the nickel plating layer into a gold plating solution tank filled with the cyanide-free electroless gold plating solution according to any one of claims 1 to 7 after carrying out ultrapure water treatment;
step 4, carrying out gold plating treatment on the plated part;
step 5, taking out the plated part after the gold plating is finished, and draining the used gold plating solution into a gold plating solution recovery tank;
and 6, concentrating the gold recovery liquid in the gold plating liquid recovery tank, calculating the gold content through specific gravity probe induction, controlling the concentration of the recovered gold plating liquid, and recovering the gold plating liquid into a gold plating liquid tank for recycling.
Wherein, the specific conditions of the gold plating treatment in the step 4 are as follows: the temperature of the plating solution is 50-70 ℃, and the stirring speed is between 100 and 200 r/min; the gold plating is carried out in two stages with different current densities: the current density of the first stage is 10-15A/dm2The current density of the second stage is 3-5A/dm2。
Wherein, nitrogen can be filled in the step 4.
The invention has the beneficial effects that: compared with the prior art, the cyanide-free electroless gold plating solution and the gold plating process thereof applied to the field of advanced wafer packaging have the following advantages:
1) adding a reaction accelerator into the cyanide-free electroless gold plating solution, wherein the reaction accelerator is a compound of 2, 6-diaminopyridine and 3-pyridinemethanol, and the mass concentration ratio of the 2, 6-diaminopyridine to the 3-pyridinemethanol is 2: 1; the accelerator adopts a composite mode, so that the phenomenon that the operation range of a single reaction accelerator is narrow is avoided; the setting of accurate concentration accelerates the activation reaction speed, reduces the activation time, and can quickly realize the void-free and seamless filling of the wafer packaging micropores;
2) in general, in order to ensure the stability of the plating solution, a wetting agent is not adopted, but the wetting agent is not adopted at all, so that the interfacial tension between an electrode and a plating solution interface is relatively large, and the plating solution is easy to have defects such as cavities, cracks and the like; in order to solve the problem, the mass concentration ratio of the surfactant to the wetting agent is 15:1 when the surfactant and the wetting agent are used, so that the surfactant and the wetting agent can achieve a compatible effect when the surfactant and the wetting agent are used, the stability of a plating solution is ensured, a plated part is easy to spread on the surface of an electrode to achieve the purpose of uniform plating, and the effect of filling the wafer packaging micropores without holes and gaps is further achieved;
3) the cyanide-free gold solution is recovered while electroplating in the gold plating process, so that the waste of the cyanide-free gold solution caused by the fact that the cyanide-free gold solution is collected to a certain degree and then recovered together in the past is avoided, and the cyanide-free gold solution is recovered synchronously to achieve the effect of immediate recycling;
4) because the reaction accelerator, the wetting agent and the surfactant with specific concentration ratio are added into the gold plating solution; the uniform plating effect is good, so that the gold plating process can be finished by adopting a current density higher than 10ASD when a piece is plated, and the electroplating can be finished more quickly on the premise of ensuring that the crystallization sizes of the plating layers are consistent and the electroplating is stable and ordered; when the electroplating is finished, the current density is reduced, so that the electroplating effect is further more perfect; the mode of different current densities in two stages in the process not only ensures the uniformity of electroplating, but also shortens the electroplating time.
Drawings
FIG. 1 is a coating morphology diagram of the cyanide-free chemical gold product obtained by the present invention.
Detailed Description
In order to make the invention more clear, the invention is further described below with reference to the text and the accompanying drawings.
The invention provides a cyanide-free chemical gold plating solution applied to the field of advanced wafer packaging and a gold plating process thereof, wherein the cyanide-free chemical gold plating solution comprises the following components in mass concentration:
the reaction accelerator is a compound of 2, 6-diaminopyridine and 3-pyridinemethanol, and the mass concentration ratio of the 2, 6-diaminopyridine to the 3-pyridinemethanol is 2: 1;
after the components are uniformly mixed according to the proportion, the pH value is adjusted to 7-9 by using sulfuric acid or potassium hydroxide, the balance is water, and the cyanide-free electroless gold plating solution is formed after the operation temperature is 50-90 ℃.
In this example, the mass concentration ratio of the surfactant to the wetting agent at the time of use was 15: 1.
In this embodiment, the complexing agent is a 1, 2-ethylenediamine compound; and the concentration sum of the conductive ions in the complexing agent and the conductive ions in the conductive salt is 10-15 mol/L. The complexing agent of the invention adopts 1, 2-ethanediamine compound, and the plating solution contains SO4 2-、Cl-The plasma conductive ions and the conductive salt also have conductive ions, so that the conductive effect of the plating solution can be greatly improved on the basis of ensuring the conductive performance.
In this embodiment, the cyanide-free gold salt is tetrachloro-auric acid or gold hydroxide. At present, gold sodium sulfite is generally adopted as cyanide-free gold salt because SO in plating solution3 2-Unstable and lead to SO by the action of oxygen in the air3 2-The concentration of the plating solution is reduced, so that the plating solution is decomposed, the physical property of the gold plating layer is unstable, and the crystallization of the plating layer is coarse, so that the effect of the gold plating layer is influenced; in order to solve the problem, the invention adopts tetrachloro-alloy acid or gold hydroxide, Au in the gold salt3+Can exist in the plating solution stably for a long time and is difficult to be changed, thereby ensuring the stability of the plating solution.
In this embodiment, the buffer is one or two of ammonium chloride and ammonium citrate. 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.
In this example, the surfactant is sodium methallylsulfonate.
In this example, the stabilizer is antimony potassium tartrate. 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.
In order to achieve the above object, the present invention further provides a cyanide-free electroless gold plating process applied to the field of advanced wafer packaging, comprising the following steps:
step 1, performing vacuum treatment on a plated part by using a pretreatment solution before chemical plating;
step 2, carrying out intermediate nickel plating treatment on the vacuumized plated piece to form a nickel plated layer;
step 3, putting the plated part with the nickel plating layer into a gold plating solution tank filled with the cyanide-free electroless gold plating solution after carrying out ultrapure water treatment;
step 4, carrying out gold plating treatment on the plated part;
step 5, taking out the plated part after the gold plating is finished, and draining the used gold plating solution into a gold plating solution recovery tank;
and 6, concentrating the gold recovery liquid in the gold plating liquid recovery tank, calculating the gold content through specific gravity probe induction, controlling the concentration of the recovered gold plating liquid, and recovering the gold plating liquid into a gold plating liquid tank for recycling. Because the cost of gold price is high, the gold is recycled after being immediately processed and recovered, and the gold plating cost is greatly reduced.
In this embodiment, the specific conditions of the gold plating process in step 4 are as follows: the temperature of the plating solution is 50-70 ℃, and the stirring speed is between 100 and 200 r/min; the gold plating time is divided into two stages with different current densities: the current density of the first stage is 10-15A/dm2The second stage current density is3-5A/dm2. Nitrogen may be purged in step 4. The addition of nitrogen ensures that the generation of oxygen is avoided in the gold plating process, and further ensures the stability of the plating solution. In the whole gold plating process, most of the thickness of the plated piece, namely about 3/4, is finished by adopting large density, and the rest 1/4 is reduced to low density when the thickness is about to be finished; the current density can be adjusted according to the electroplating condition of the plated part in the whole process, so that the thickness of the finally obtained gold-plated layer is suitable, and the gold layer has no holes or cracks; the surface is smooth and the weldability is good.
The invention has the beneficial effects that: compared with the prior art, the cyanide-free electroless gold plating solution and the gold plating process thereof applied to the field of advanced wafer packaging have the following advantages:
1) adding a reaction accelerator into the cyanide-free electroless gold plating solution, wherein the reaction accelerator is a compound of 2, 6-diaminopyridine and 3-pyridinemethanol, and the mass concentration ratio of the 2, 6-diaminopyridine to the 3-pyridinemethanol is 2: 1; the accelerator adopts a composite mode, so that the phenomenon that the operation range of a single reaction accelerator is narrow is avoided; the setting of accurate concentration accelerates the activation reaction speed, reduces the activation time, and can quickly realize the void-free and seamless filling of the wafer packaging micropores;
4) in general, in order to ensure the stability of the plating solution, a wetting agent is not adopted, but the wetting agent is not adopted at all, so that the interfacial tension between an electrode and a plating solution interface is relatively large, and the plating solution is easy to have defects such as cavities, cracks and the like; in order to solve the problem, the mass concentration ratio of the surfactant to the wetting agent is 15:1 when the surfactant and the wetting agent are used, so that the surfactant and the wetting agent can achieve a compatible effect when the surfactant and the wetting agent are used, the stability of a plating solution is ensured, a plated part is easy to spread on the surface of an electrode to achieve the purpose of uniform plating, and the effect of filling the wafer packaging micropores without holes and gaps is further achieved;
5) the cyanide-free gold solution is recovered while electroplating in the gold plating process, so that the waste of the cyanide-free gold solution caused by the fact that the cyanide-free gold solution is collected to a certain degree and then recovered together in the past is avoided, and the cyanide-free gold solution is recovered synchronously to achieve the effect of immediate recycling;
4) because the reaction accelerator, the wetting agent and the surfactant with specific concentration ratio are added into the gold plating solution; the uniform plating effect is good, so that the gold plating process can be finished by adopting a current density higher than 10ASD when a piece is plated, and the electroplating can be finished more quickly on the premise of ensuring that the crystallization sizes of the plating layers are consistent and the electroplating is stable and ordered; when the electroplating is finished, the current density is reduced, the stability of the solution and the concentration of gold are further ensured, and the electroplating effect is more perfect; the mode of different current densities in two stages in the process not only ensures the uniformity of electroplating, but also shortens the electroplating time.
5) 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.
The following are several specific examples of the invention
Example 1
A cyanide-free electroless gold plating solution comprising, for every 1 liter of the cyanide-free electroless gold plating solution:
adjusting the pH to 7.2 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: at 50 ℃.
The gold plating solution prepared by the components is adopted, and after cyanide-free gold plating is carried out on a wafer packaging product by the gold plating method, the finally obtained gold thickness is 0.3 micron; by adopting the solution and the gold plating process, the whole process only needs 20 minutes to complete; the obtained gold-plated layer has consistent crystal size and no cavity or crack; the surface is smooth.
Example 2
The cyanide-free chemical gold-plating solution comprises the following components by 1 liter:
adjusting the pH to 8 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: at 60 ℃.
The gold plating solution prepared by the components is adopted, and the gold thickness is 0.2 micron after cyanide-free gold plating is carried out on a wafer packaging product by the gold plating method; by adopting the solution and the gold plating process, the whole process only needs 12 minutes to complete; the obtained gold-plated layer has consistent crystal size and no cavity or crack; the surface is smooth.
Example 3
Adjusting the pH to 9 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: 80 ℃.
The gold plating solution prepared by the components is adopted, and the gold thickness is 0.05 microns after cyanide-free gold plating is carried out on a wafer packaging product by the gold plating method; by adopting the solution and the gold plating process, the whole process only needs 2 minutes to complete; the obtained gold-plated layer has consistent crystal size and no cavity or crack; the surface is smooth.
Comparative example
Adjusting the pH to 8 with sulfuric acid or potassium hydroxide;
the balance being water.
Operating temperature: at 60 ℃.
Reaction accelerator, conductive salt and wetting agent do not exist in the component; the gold plating solution prepared by the components is adopted to carry out cyanide-free gold plating on a wafer packaging product, and the gold thickness is 0.2 micron; the same gold plating conditions are adopted, the whole process needs 20 minutes to complete, although the rate is increased, the obtained gold plating layer has inconsistent crystallization and is slightly provided with holes and cracks; if the traditional gold plating process time and temperature are adopted, the crystal size of the surface of the plated part is consistent, but the whole process needs about 30 minutes.
As can be seen by comparing the three implementation examples and the comparative examples, the coating obtained by the invention not only achieves the effect of filling the wafer packaging micropores without holes and gaps; and the electroplating uniformity effect is good, and the electroplating efficiency is high. The gold plating layer obtained by adopting the cyanide-free gold plating solution and the gold plating process is shown in figure 1, and the gold plating layer is obviously uniform and compact in crystallization.
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 (6)
1. A cyanide-free electroless gold plating solution applied to the field of advanced wafer packaging is characterized by comprising the following components in mass concentration:
cyanide-free gold salt with the content of Au ions being 6-10g/L
10-60g/L complexing agent
10-60g/L of conductive salt
Buffer 30-60g/L
Anti-aging agent 5-10g/L
15-80mg/L of surfactant
Wetting agent 1-5mg/L
Reaction accelerator 50-80mg/L
0.2-5mg/L stabilizer
The reaction accelerator is a compound of 2, 6-diaminopyridine and 3-pyridinemethanol, and the mass concentration ratio of the 2, 6-diaminopyridine to the 3-pyridinemethanol is 2: 1;
uniformly mixing the components according to a ratio, adjusting the pH to 7-9 by using sulfuric acid or potassium hydroxide, and adjusting the balance of water to an operating temperature of 50-90 ℃ to form a cyanide-free electroless gold plating solution, wherein the mass concentration ratio of the surfactant to the wetting agent in use is 15:1;
the complexing agent is a 1, 2-ethanediamine compound; the concentration sum of the conductive ions in the complexing agent and the conductive ions in the conductive salt is 10-15mol/L;
the cyanide-free gold salt is tetrachloro-alloy acid or gold hydroxide;
the surfactant is sodium methallylsulfonate.
2. The cyanide-free electroless gold plating solution as claimed in claim 1, wherein the buffer is one or both of ammonium chloride and ammonium citrate.
3. The cyanide-free electroless gold plating solution applied to the field of advanced wafer packaging as claimed in claim 1, wherein the stabilizer is antimony potassium tartrate.
4. A cyanide-free electroless gold plating process applied to the field of advanced wafer packaging is characterized by comprising the following steps:
step 1, performing vacuum treatment on a plated part by using a pretreatment solution before chemical plating;
step 2, carrying out intermediate nickel plating treatment on the vacuumized plated piece to form a nickel plated layer;
step 3, putting the plated piece with the nickel plating layer into a gold plating solution tank filled with the cyanide-free electroless gold plating solution according to any one of the claims 1 to 3 after carrying out ultrapure water treatment;
step 4, carrying out gold plating treatment on the plated part;
step 5, taking out the plated part after the gold plating is finished, and draining the used gold plating solution into a gold plating solution recovery tank;
and 6, concentrating the gold recovery liquid in the gold plating liquid recovery tank, calculating the gold content through specific gravity probe induction, controlling the concentration of the recovered gold plating liquid, and recovering the gold plating liquid into a gold plating liquid tank for recycling.
5. The cyanide-free electroless gold plating process applied to the field of advanced wafer packaging as claimed in claim 4, wherein the specific conditions of the gold plating treatment in the step 4 are as follows: the temperature of the plating solution is 50-70 ℃, and the stirring speed is between 100 and 200 r/min; the gold plating is carried out in two stages with different current densities: the current density of the first stage is 10-15A/dm2The current density of the second stage is 1-1.5A/dm2。
6. The cyanide-free electroless gold plating process applied to the field of advanced wafer packaging as claimed in claim 5, wherein nitrogen gas can be filled in step 4.
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| CN113789553B (en) * | 2021-11-17 | 2022-02-08 | 深圳市创智成功科技有限公司 | Nickel plating solution applied to printed circuit board and nickel electroplating method thereof |
| CN114032529B (en) * | 2021-11-17 | 2022-08-19 | 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 |
| 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 |
| CN114232038A (en) * | 2022-02-25 | 2022-03-25 | 深圳市创智成功科技有限公司 | Cyanide-free electrogilding formula applied to wafer-level packaging and electrogilding process thereof |
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| US6565732B1 (en) * | 1999-10-07 | 2003-05-20 | Tanaka Kikinzoku Kogyo K.K. | Gold plating solution and plating process |
| CN103741180A (en) * | 2014-01-10 | 2014-04-23 | 哈尔滨工业大学 | Cyanide-free bright electrogilding additive and application thereof |
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| CN111705341A (en) * | 2020-06-12 | 2020-09-25 | 山东鲁蓝环保科技有限公司 | Cyanide-free gold plating electroplating solution and electroplating process thereof |
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| US6565732B1 (en) * | 1999-10-07 | 2003-05-20 | Tanaka Kikinzoku Kogyo K.K. | Gold plating solution and plating process |
| CN103741180A (en) * | 2014-01-10 | 2014-04-23 | 哈尔滨工业大学 | Cyanide-free bright electrogilding additive and application thereof |
| CN108754553A (en) * | 2018-06-26 | 2018-11-06 | 厦门大学 | Trivalent gold cyanogen-less gold plating solution based on the coordination of heterocycle Alkaloid and its application |
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