CN115449864A - Additive for thin film copper electroplating and electroplating process thereof - Google Patents

Additive for thin film copper electroplating and electroplating process thereof Download PDF

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CN115449864A
CN115449864A CN202211324250.1A CN202211324250A CN115449864A CN 115449864 A CN115449864 A CN 115449864A CN 202211324250 A CN202211324250 A CN 202211324250A CN 115449864 A CN115449864 A CN 115449864A
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copper
additive
electroplating
plating
solution
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CN115449864B (en
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姚玉
洪学平
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Shenzhen Chuangzhi Xinlian Technology Co ltd
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Shenzhen Chuangzhi Xinlian Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/38Electroplating: Baths therefor from solutions of copper
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/12Semiconductors
    • C25D7/123Semiconductors first coated with a seed layer or a conductive layer
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses an additive for thin film electro-coppering and an electro-coppering process thereof, wherein the additive for electro-coppering comprises the following components in percentage by mass: 60-90g/L of copper sulfate, 40-120mg/L of composite brightener, 30-90mg/L of composite leveler, 10-40mg/L of wetting agent, 20-60mg/L of anti-plating agent, 0.1-0.5g/L of electrolyte and 20-45mg/L of stabilizer. The solution of the invention belongs to neutral electro-coppering solution, the wastewater treatment is simple, the stability of the plating solution is excellent, the plating layer is uniform, bright and good in binding force, and the using current density range is 0.1-6.5A/dm 2

Description

Additive for thin film copper electroplating and electroplating process thereof
Technical Field
The invention relates to the technical field of copper electroplating, in particular to an additive applied to thin film copper electroplating and an electroplating process thereof.
Background
The copper electroplating technology for the semiconductor film is the electroplating technology which is most widely applied in the current market and has higher cost performance, and a layer of copper is electrodeposited on a semiconductor barrier layer and is used as a substrate for subsequent process production. Many techniques for copper electroplating on wafers have been developed and used, and a high copper electroplating solution is proposed in patent CN110541179A, but the solution has poor uniformity of copper layer; in addition, patent CN103290438A proposes a wafer copper electroplating solution, but the solution is too acidic, the waste solution treatment cost is high, and the solution does not conform to the current environmental protection trend.
Along with the increasing serious environmental protection pressure and the higher industrial wastewater treatment cost, great pressure is brought to a plurality of enterprises, and under the condition of meeting the market demand, the novel environment-friendly wastewater treatment device has the advantages of being excellent in performance, capable of reducing the wastewater treatment cost and achieving environmental protection, and is a necessary trend of the current development. Accordingly, the present invention is directed to a copper electroplating solution for a semiconductor thin film to solve the current problems.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides the additive for the film electro-coppering and the electro-coppering process thereof. The solution of the invention belongs to neutral copper electroplating solution, the wastewater treatment is simple, the stability of the plating solution is excellent, the plating layer is uniform, bright and good in binding force, and the range of the current density is wide.
In order to achieve the purpose, the invention provides an additive for thin film electrolytic copper plating, which comprises the following components in mass concentration:
the composition comprises the following components in mass concentration: 60-90g/L of copper sulfate, 40-120mg/L of composite brightener, 30-90mg/L of composite leveler, 10-40mg/L of wetting agent, 20-60mg/L of anti-plating agent, 0.1-0.5g/L of electrolyte, 20-45mg/L of stabilizer and pH value of 5.5-6.5
The operation temperature is 25-35 DEG C
The current density is 0.1-6.5A/dm 2
The composite leveling agent is a composition of tricyclazole and 2-propynyl-2-hydroxyalkyl ether, and the mass concentration ratio of the tricyclazole to the 2-propynyl-2-hydroxyalkyl ether is 1.
The composite brightening agent comprises pyridine propane sulfonic acid inner salt, N, N-diethyl propyne amine sulfate and sodium allylsulfonate, the mass concentration ratio of the pyridine propane sulfonic acid inner salt to the N, N-diethyl propyne amine sulfate to the sodium allylsulfonate is 1. The invention adopts the composite brightener to realize normal electroplating in a large current density range, does not generate copper nodules, and has great advantages compared with the electroplating copper solution on the market.
Wherein the electrolyte is potassium sulfate.
Wherein the stabilizer is sulfosalicylic acid. The service life of the bath solution can be prolonged, the electrolytic copper plating solution in the market has excessive impurities in the production process due to the prolonged service life, so that the electrolytic copper plating solution is unbalanced, and the stabilizer can greatly influence impurity ions such as zinc, iron and the like on the electrolytic copper plating solution.
Wherein the anti-bending agent is 3- [ [ (benzylthio) thiocarbonyl ] thio ] propionic acid; the wetting agent is 1-allyloxy-3- (4-nonylphenol) -2-propanol polyoxyethylene (10) ether ammonium sulfate.
In order to realize the aim, the invention also provides an electroplating process applied to the film copper electroplating additive, which comprises the following specific steps:
polishing a base material, washing the base material with pure water for three times, washing the base material with hydrofluoric acid, washing the base material with pure water for three times, removing oil for 1min in a neutral state, and then washing the base material with ultrasonic waves of 25kHz for 5min, activating ruthenium for 1min and washing the base material with pure water for one time;
secondly, carrying out chemical galvanizing, wherein the substrate subjected to ultrasonic cleaning enters a chemical galvanizing bath for chemical galvanizing to obtain a compact chemical zinc layer, and then cleaning for three times by pure water;
step three, electroless copper plating, wherein the base material enters an electroless copper plating tank after being washed by electroless zinc plating water, and is subjected to electroless copper plating to form a copper seed layer;
and fourthly, electroplating copper, wherein a cylinder dragging plate is used for pre-dragging for 2 hours before use to prevent copper nodules, the substrate subjected to electroless copper plating is washed for three times by pure water and then enters an electroplating copper tank, the used electroplating copper solution is the electroplating copper solution with any one of the copper additives, and after the electroplating copper is finished, the substrate is cleaned and dried.
Wherein the specific operation flow of the second step chemical galvanizing is as follows: the base material enters a chemical galvanizing bath after being activated, is directly subjected to reduction plating in a chemical galvanizing solution for 2min in a soaking mode, is washed once by pure water, is subjected to dezincification by a dezincification solution, is washed once by pure water, returns to a ruthenium activation bath, is washed once by pure water, and enters the galvanizing bath for 2min to obtain a compact zinc layer.
Wherein, the chemical galvanizing solution in the second step comprises the following components: 20-50g/L of zinc oxide, 50g/L of sodium hydroxide, 15g/L of potassium sodium tartrate, 5g/L of sodium succinate, 10 ml/L of OP-10, 60mg/L of ethoxylated butynediol, 30mg/L of lead acetate and 0.2-0.8g/L of DMAB; and the parameters of the chemical galvanizing are as follows: the temperature is 25-35 ℃, the thickness of the zinc coating is kept at 0.1-0.5 micron, the zinc stripping solution contains 30% volume concentration of nitric acid and 30-60mg/L of nicotinic acid, and the dezincification time is 30s. In order to improve the deposition of copper and realize the complete coverage of the seed layer when the copper seed layer is formed, the strong alkaline chemical galvanizing solution can improve the roughness of the barrier layer and simultaneously obtain a very thin compact zinc layer in advance.
Wherein the ruthenium activation solution for ruthenium activation in the first step comprises 15-25mg/L of ruthenium sulfate, 50-70mg/L of lauric acid random polyether LPE-1200, 30-60mg/L of terpolymer of 1-vinyl imidazole and 0.05-0.15g/L of 1,2, 4-triazole, and the parameters of ruthenium activation are as follows: the temperature is 35-45 ℃, the time is 0.5-2min, and the invention can improve the reduction activity of zinc and promote the rapid deposition of zinc by using the specially developed ruthenium activating solution.
Wherein, the concrete conditions of the fourth step are as follows: the operation temperature is 25-35 ℃, and the current density is 0.1-6.5A/dm 2 Electroplating copper under the protection of argon, wherein the pressure of argon is 1.5-2.5kg/cm 2, The purpose is to replace nitrogen to realize complete oxygen discharge.
The invention has the beneficial effects that: compared with the prior art, the additive for thin film copper electroplating and the electroplating process thereof provided by the invention have the following advantages:
1) The composite brightener provided by the invention is a pyridylpropane sulfonic acid inner salt, N, N-diethyl propyne amine sulfate and sodium allylsulfonate, the mass concentration ratio of the pyridylpropane sulfonic acid inner salt to the N, N-diethyl propyne amine sulfate to the sodium allylsulfonate is 1.
2) The invention adopts a sulfuric acid-free copper electroplating solution system, has low waste liquid treatment cost and has environmental protection compared with the traditional high-sulfuric acid copper electroplating solution.
3) The composite leveling agent is a composition of tricyclazole and 2-propynyl-2-hydroxyalkyl ether, the mass concentration ratio of the tricyclazole to the 2-propynyl-2-hydroxyalkyl ether is 1.
4) In order to improve the deposition of copper and realize the complete coverage of the seed layer when the copper seed layer is formed, the strong alkaline chemical zinc plating solution can improve the roughness of the barrier layer, and simultaneously obtain a very thin compact zinc layer in advance.
Drawings
FIG. 1 is a graph showing the judgment criteria of the test results of the examples and comparative examples of the present invention;
FIG. 2 is a graph showing the results of the tests conducted in the examples and comparative examples of the present invention.
Detailed Description
In order to more clearly describe the present invention, the present invention is further described below in terms of the text and the accompanying drawings.
The invention provides an additive for thin film copper electroplating, which comprises the following components in mass concentration:
60-90g/L of copper sulfate, 40-120mg/L of composite brightener, 30-90mg/L of composite leveler, 10-40mg/L of wetting agent, 20-60mg/L of anti-plating agent, 0.1-0.5g/L of electrolyte, 20-45mg/L of stabilizer and pH value of 5.5-6.5
The operation temperature is 25-35 DEG C
The current density is 0.1-6.5A/dm 2
The composite leveling agent is a composition of tricyclazole and 2-propynyl-2-hydroxyalkyl ether, and the mass concentration ratio of the tricyclazole to the 2-propynyl-2-hydroxyalkyl ether is 1.
In this embodiment, the composite brightener is a pyridylpropane sulfonic acid inner salt, N-diethyl propyne amine sulfate and sodium allylsulfonate, the mass concentration ratio of the pyridylpropane sulfonic acid inner salt to the N, N-diethyl propyne amine sulfate in use is 1-30 mg/L, the mass concentration ratio of the N, N-diethyl propyne amine sulfate to the sodium allylsulfonate is 10-30mg/L, and the mass concentration ratio of the sodium allylsulfonate is 20-60mg/L.
In this embodiment, the electrolyte is potassium sulfate.
In this example, the stabilizer is sulfosalicylic acid.
In this embodiment, the anti-plating agent is 3- [ [ (benzylthio) thiocarbonyl ] thio ] propanoic acid; the wetting agent is 1-allyloxy-3- (4-nonylphenol) -2-propanol polyoxyethylene (10) ether ammonium sulfate.
The invention also provides an electrolytic copper plating process containing the additive applied to the film electrolytic copper plating, which comprises the following specific steps:
the first step, polishing the substrate, washing with pure water for three times, washing with hydrofluoric acid, washing with pure water for three times, removing oil for 1min in a neutral state, washing with 25kHz ultrasonic waves for 5min, activating ruthenium for 1min, and washing with pure water for one time;
secondly, carrying out chemical galvanizing, wherein the substrate subjected to ultrasonic cleaning enters a chemical galvanizing bath for chemical galvanizing to obtain a compact chemical zinc layer, and then cleaning for three times by pure water;
step three, electroless copper plating, wherein the base material enters an electroless copper plating tank after being washed by electroless zinc plating water, and is subjected to electroless copper plating to form a copper seed layer;
and step four, electro-coppering, wherein pre-mopping is carried out for 2 hours by using a mopping cylinder plate before use so as to prevent copper nodules from generating, the substrate after electroless copper plating is washed for three times by pure water and then enters an electro-coppering tank, the electro-coppering solution is any one of the electro-coppering solutions, and after the electro-coppering is finished, the substrate is cleaned and dried.
In this embodiment, the specific operation flow of the second step of electroless zinc plating is as follows: the base material enters a chemical galvanizing bath after being activated, is directly subjected to reduction plating in a chemical galvanizing solution for 2min in a soaking mode, is washed once by pure water, is subjected to dezincification by a dezincification solution, is washed once by pure water, returns to a ruthenium activation bath, is washed once by pure water, and enters the galvanizing bath for 2min to obtain a compact zinc layer.
In this embodiment, the chemical galvanizing solution in the second step mainly comprises the following components and process parameters: the chemical galvanizing solution comprises 20-50g/L of zinc oxide, 50g/L of sodium hydroxide, 15g/L of sodium potassium tartrate, 5g/L of sodium succinate, 10 ml/L of OP, 60mg/L of ethoxylated butynediol, 30mg/L of lead acetate and 0.2-0.8g/L of DMAB, the temperature is 25-35 ℃, the thickness of a zinc coating is kept at 0.1-0.5 micron, the zinc stripping solution comprises 30% of nitric acid and 30-60mg/L of nicotinic acid by volume concentration, and the dezincification time is 30s.
In this embodiment, the main components and process parameters of the ruthenium activation in the first step are as follows: ruthenium sulfate 15-25mg/L, lauric acid random polyether LPE-1200-70 mg/L, terpolymer of 1-vinyl imidazole 30-60mg/L and 1,2, 4-triazole 0.05-0.15g/L, temperature 35-45 ℃ and time 0.5-2min.
In this embodiment, specific conditions of the fourth step are: the operation temperature is 25-35 ℃, and the current density is 0.1-6.5A/dm 2 Electroplating copper under the protection of argon, wherein the pressure of argon is 1.5-2.5kg/cm 2 The purpose is to replace nitrogen to realize complete oxygen discharge.
The invention has the beneficial effects that: compared with the prior art, the additive for thin film copper electroplating and the electroplating process thereof provided by the invention have the following advantages:
1) The composite brightener provided by the invention is a pyridine propane sulfonic acid inner salt, N, N-diethyl propyne amine sulfate and sodium allylsulfonate, the mass concentration ratio of the pyridine propane sulfonic acid inner salt to the N, N-diethyl propyne amine sulfate to the sodium allylsulfonate is 1.
2) The invention adopts a sulfuric acid-free copper electroplating solution system, has low waste liquid treatment cost and has environmental protection compared with the traditional high-sulfuric acid copper electroplating solution.
3) The composite leveling agent is a composition of tricyclazole and 2-propynyl-2-hydroxyalkyl ether, and the mass concentration ratio of the tricyclazole to the 2-propynyl-2-hydroxyalkyl ether is 1.
4) In order to improve the deposition of copper and realize the complete coverage of the seed layer when the copper seed layer is formed, the strong alkaline chemical zinc plating solution can improve the roughness of the barrier layer, and simultaneously obtain a very thin compact zinc layer in advance.
The following are several specific embodiments of the invention:
the judgment criteria of the test results of the examples and the comparative examples are shown in fig. 1, in which the uniformity test is performed using one substrate of the same type of plate for each set of experiments, and four sides and five middle points are respectively used as test objects.
Example 1
An additive for thin film electrolytic copper plating:
75g/L of copper sulfate, 10mg/L of pyridine propane sulfonic acid inner salt, 10mg/L of N, N-diethyl propyne amine sulfate, 20mg/L of sodium allyl sulfonate, 15mg/L of tricyclazole, 15mg/L of 2-propynyl-2-hydroxyalkyl ether, 10mg/L of 1-allyloxy-3- (4-nonylphenol) -2-propanol polyoxyethylene (10) ether ammonium sulfate, 20mg/L of 3- [ [ (benzylthio) thiocarbonyl ] thio ] propionic acid, 0.1g/L of potassium sulfate, 20mg/L of sulfosalicylic acid, pH =6, and the balance of pure water.
The operation temperature is 25 DEG C
The current density is 1.5A/dm 2
The time is 100min.
Example 2
An additive for thin film electrolytic copper plating:
75g/L of copper sulfate, 20mg/L of pyridine propane sulfonic acid inner salt, 20mg/L of N, N-diethyl propyne amine sulfate, 40mg/L of sodium allyl sulfonate, 30mg/L of tricyclazole, 30mg/L of 2-propynyl-2-hydroxyalkyl ether, 40mg/L of 1-allyloxy-3- (4-nonylphenol) -2-propanol polyoxyethylene (10) ether ammonium sulfate, 60mg/L of 3- [ [ (benzylthio) thiocarbonyl ] thio ] propionic acid, 0.5g/L of potassium sulfate, 45mg/L of sulfosalicylic acid, pH =6, and the balance of pure water.
The operation temperature is 25 DEG C
The current density is 2.5A/dm 2
The time is 65min.
Example 3
An additive for thin film electrolytic copper plating:
80g/L of copper sulfate, 30mg/L of pyridine propane sulfonic acid inner salt, 30mg/L of N, N-diethyl propyne amine sulfate, 60mg/L of sodium allylsulfonate, 40mg/L of tricyclazole, 40mg/L of 2-propynyl-2-hydroxyalkyl ether, 30mg/L of 1-allyloxy-3- (4-nonylphenol) -2-propanol polyoxyethylene (10) ether ammonium sulfate, 40mg/L of 3- [ [ (benzylthio) thiocarbonyl ] thio ] propionic acid, 0.3g/L of potassium sulfate, 30mg/L of sulfosalicylic acid, pH =6, and the balance of pure water.
The operation temperature is 25 DEG C
The current density is 5.5A/dm 2
The time is 30min.
Comparative example
An additive for thin film electrolytic copper plating:
75g/L of copper sulfate, 10-40mg/L of 1-allyloxy-3- (4-nonylphenol) -2-propanol polyoxyethylene (10) ether ammonium sulfate, 0.1-0.5g/L of potassium sulfate, pH of 5.5-6.5 and the balance of pure water.
The operation temperature is 25 DEG C
The current density is 5.5A/dm 2
The time is 30min.
Five panels were grouped for each example and the resulting test results are shown in FIG. 2, which is a comparison of examples 1-3 in FIG. 2 with the comparative example, and the conclusion is that: the plating solution obtained in the embodiments 1,2 and 3 has the advantages of excellent stability, brightness and smoothness, excellent folding plating phenomenon, excellent binding force and excellent uniformity. Compared with the embodiment, the comparative example lacks a composite brightener, a composite leveling agent, a stabilizer and an anti-bending plating agent, and the experimental results are that the plating solution has poor stability, poor brightness and smoothness, poor bending plating aberration, poor bonding force and poor uniformity. The experimental conditions are set in the experiment, and the specific production can be changed according to corresponding requirements.
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 (10)

1. The additive for thin film copper electroplating is characterized by comprising the following components in mass concentration: 60-90g/L of copper sulfate, 40-120mg/L of composite brightener, 30-90mg/L of composite leveler, 10-40mg/L of wetting agent, 20-60mg/L of anti-plating agent, 0.1-0.5g/L of electrolyte, 20-45mg/L of stabilizer and pH value of 5.5-6.5
The operation temperature is 25-35 DEG C
The current density is 0.1-6.5A/dm 2
The composite leveling agent is a composition of tricyclazole and 2-propynyl-2-hydroxyalkyl ether, and the mass concentration ratio of the tricyclazole to the 2-propynyl-2-hydroxyalkyl ether is 1.
2. The additive for thin film electrolytic copper plating according to claim 1, wherein the composite brightener comprises an inner salt of pyridine propane sulfonic acid, N, N-diethyl propyne amine sulfate and sodium allyl sulfonate, the mass concentration ratio of the inner salt of pyridine propane sulfonic acid to the sulfate is 1.
3. The additive for thin film electrolytic copper plating according to claim 1, wherein the electrolyte is potassium sulfate.
4. The additive for thin film electrolytic copper plating according to claim 1, wherein the stabilizer is sulfosalicylic acid.
5. The additive for thin film electrolytic copper plating according to claim 1, wherein the anti-deplating agent is 3- [ [ (benzylthio) thiocarbonyl ] thio ] propanoic acid; the wetting agent is 1-allyloxy-3- (4-nonylphenol) -2-propanol polyoxyethylene (10) ether ammonium sulfate.
6. An electroplating process applied to a film copper electroplating additive is characterized by comprising the following specific steps:
the first step, polishing the substrate, washing with pure water for three times, washing with hydrofluoric acid, washing with pure water for three times, removing oil for 1min in a neutral state, washing with 25kHz ultrasonic waves for 5min, activating ruthenium for 1min, and washing with pure water for one time;
secondly, carrying out chemical galvanizing, wherein the substrate subjected to ultrasonic cleaning enters a chemical galvanizing bath for chemical galvanizing to obtain a compact chemical zinc layer, and then cleaning for three times by pure water;
step three, electroless copper plating, wherein the base material enters an electroless copper plating tank after being washed by electroless zinc plating water, and is subjected to electroless copper plating to form a copper seed layer;
and a fourth step of electro-coppering, wherein pre-mopping is carried out for 2 hours by using a mopping cylinder plate before use so as to prevent generation of copper nodules, the substrate after electroless copper plating is washed for three times by pure water and then enters an electro-coppering tank, the electro-coppering solution is the electro-coppering solution with the copper additive disclosed by any one of claims 1-5, and after the electro-coppering is finished, the substrate is cleaned and dried.
7. An electroplating process applied to a thin film copper electroplating additive according to claim 6, wherein the specific operation flow of the second step of electroless zinc plating is as follows: the base material enters a chemical galvanizing bath after being activated, is directly subjected to reduction plating in a chemical galvanizing solution for 2min in a soaking mode, is washed once by pure water, is subjected to dezincification by a dezincification solution, is washed once by pure water, returns to a ruthenium activation bath, is washed once by pure water, and enters the galvanizing bath for 2min to obtain a compact zinc layer.
8. The electroplating process applied to the thin film copper electroplating additive according to claim 7, wherein the second-step chemical galvanizing solution comprises the following components: 20-50g/L of zinc oxide, 50g/L of sodium hydroxide, 15g/L of potassium sodium tartrate, 5g/L of sodium succinate, 10 ml/L of OP-10, 60mg/L of ethoxylated butynediol, 30mg/L of lead acetate and 0.2-0.8g/L of DMAB; and the parameters of the chemical galvanizing are as follows: the temperature is 25-35 ℃, the thickness of the zinc coating is kept at 0.1-0.5 micron, the zinc stripping solution contains 30% volume concentration of nitric acid and 30-60mg/L of nicotinic acid, and the dezincification time is 30s.
9. The electroplating process applied to the film copper electroplating additive according to claim 6, wherein the ruthenium activation solution adopted in the first step comprises 15-25mg/L of ruthenium sulfate, 50-70mg/L of random polyether of lauric acid LPE-1200, 30-60mg/L of terpolymer of 1-vinylimidazole and 0.05-0.15g/L of 1,2, 4-triazole, and the parameters of ruthenium activation are as follows: the temperature is 35-45 deg.C, and the time is 0.5-2min.
10. An electroplating process applied to a film copper electroplating additive according to claim 6, wherein the specific conditions of the fourth step are as follows: the operation temperature is 25-35 ℃, and the current density is 0.1-6.5A/dm 2 Electroplating copper under the protection of argon gas, wherein the pressure of argon gas is 1.5-2.5kg/cm 2
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Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004060017A (en) * 2002-07-30 2004-02-26 C Uyemura & Co Ltd Electroless zinc oxide plating method
CN104805421A (en) * 2015-03-30 2015-07-29 广东工业大学 Preparation method of shape-controllable nano zinc oxide film
CN105543908A (en) * 2016-02-29 2016-05-04 广州鸿葳科技股份有限公司 Solution and method for cyanide-free alkaline bright barrel copper plating
JP2017048414A (en) * 2015-08-31 2017-03-09 キヤノン・コンポーネンツ株式会社 Zinc oxide plating film-attached article, production method thereof, zinc oxide electroless plating solution, and zinc oxide electroless plating method
CN111945192A (en) * 2020-08-11 2020-11-17 深圳市创智成功科技有限公司 Blind hole filling electro-coppering solution for HDI (high Density interconnect) board and carrier board
CN112376094A (en) * 2020-11-06 2021-02-19 东莞市川富电子有限公司 Functional electroplating coating method for charging and discharging module block connecting terminal
CN113707854A (en) * 2021-08-13 2021-11-26 张家港智电芳华蓄电研究所有限公司 Preparation method of zinc powder coated with copper, tin, lead or alloy thereof
CN113737160A (en) * 2021-07-21 2021-12-03 深圳市信维通信股份有限公司 Chemical black nickel plating solution
CN114481106A (en) * 2022-02-20 2022-05-13 珠海市创智芯科技有限公司 Chemical nickel gold process applied to wafer aluminum copper substrate in field of IGBT power device
CN114672857A (en) * 2022-05-30 2022-06-28 深圳市创智成功科技有限公司 Preparation method of high-purity copper sulfate and copper electroplating process applied to copper interconnection
CN114875460A (en) * 2022-04-08 2022-08-09 广州市慧科高新材料科技有限公司 Synthetic method and application of ultrathin pore-filling copper plating leveling agent
CN114990647A (en) * 2022-08-01 2022-09-02 深圳市创智成功科技有限公司 Environment-friendly through hole filling pulse copper electroplating solution and electroplating method thereof

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004060017A (en) * 2002-07-30 2004-02-26 C Uyemura & Co Ltd Electroless zinc oxide plating method
CN104805421A (en) * 2015-03-30 2015-07-29 广东工业大学 Preparation method of shape-controllable nano zinc oxide film
JP2017048414A (en) * 2015-08-31 2017-03-09 キヤノン・コンポーネンツ株式会社 Zinc oxide plating film-attached article, production method thereof, zinc oxide electroless plating solution, and zinc oxide electroless plating method
CN105543908A (en) * 2016-02-29 2016-05-04 广州鸿葳科技股份有限公司 Solution and method for cyanide-free alkaline bright barrel copper plating
CN111945192A (en) * 2020-08-11 2020-11-17 深圳市创智成功科技有限公司 Blind hole filling electro-coppering solution for HDI (high Density interconnect) board and carrier board
CN112376094A (en) * 2020-11-06 2021-02-19 东莞市川富电子有限公司 Functional electroplating coating method for charging and discharging module block connecting terminal
CN113737160A (en) * 2021-07-21 2021-12-03 深圳市信维通信股份有限公司 Chemical black nickel plating solution
CN113707854A (en) * 2021-08-13 2021-11-26 张家港智电芳华蓄电研究所有限公司 Preparation method of zinc powder coated with copper, tin, lead or alloy thereof
CN114481106A (en) * 2022-02-20 2022-05-13 珠海市创智芯科技有限公司 Chemical nickel gold process applied to wafer aluminum copper substrate in field of IGBT power device
CN114875460A (en) * 2022-04-08 2022-08-09 广州市慧科高新材料科技有限公司 Synthetic method and application of ultrathin pore-filling copper plating leveling agent
CN114672857A (en) * 2022-05-30 2022-06-28 深圳市创智成功科技有限公司 Preparation method of high-purity copper sulfate and copper electroplating process applied to copper interconnection
CN114990647A (en) * 2022-08-01 2022-09-02 深圳市创智成功科技有限公司 Environment-friendly through hole filling pulse copper electroplating solution and electroplating method thereof

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