CN114959814A - Method for quickly electroplating high-conductivity and high-heat-conductivity copper layer - Google Patents
Method for quickly electroplating high-conductivity and high-heat-conductivity copper layer Download PDFInfo
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- CN114959814A CN114959814A CN202210650700.XA CN202210650700A CN114959814A CN 114959814 A CN114959814 A CN 114959814A CN 202210650700 A CN202210650700 A CN 202210650700A CN 114959814 A CN114959814 A CN 114959814A
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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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
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
- C25D7/123—Semiconductors first coated with a seed layer or a conductive layer
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a copper electroplating process, in particular to a method for quickly electroplating a copper layer with high electric conductivity and high heat conductivity, which is used for solving the defects of low copper layer preparation capacity and high cost caused by slow deposition rate in the existing pulse copper layer electroplating method. The method for rapidly electroplating the high-conductivity high-thermal-conductivity copper layer adopts bipolar pulse electroplating, and the electroplating process is divided into three stages, wherein the first stage and the second stage adopt an adhesion compact layer formed on the surface of a seed layer by low current density, and the third stage adopts a copper particle accumulation layer and a compact filling layer formed on the adhesion compact layer by high current density; the invention can realize the rapid deposition of the copper layer, and the electrical property of the deposited copper layer is close to that of pure copper, thereby improving the preparation capacity of the copper layer and reducing the production cost.
Description
Technical Field
The invention relates to a copper electroplating process, in particular to a method for quickly electroplating a high-conductivity and high-heat-conductivity copper layer.
Background
Electroplating a copper layer as a highly conductive and highly thermally conductive material, andand has high cost performance, and can be widely applied to semiconductor devices and photovoltaic products. A common method of electroplating copper layers is pulse electroplating, which is based on the principle of increasing the active polarization of the cathode and decreasing the concentration polarization of the cathode by relaxation of current (or voltage) pulses; when the current is turned on, metal ions near the cathode are sufficiently deposited; when the current is turned off, the discharge ions around the cathode are restored to the initial concentration; the continuous repeated pulse current with the period is mainly used for reducing metal ions, so that the physical and chemical properties of the coating are improved. In the electroplating process, the resistivity of the copper layer is rapidly reduced and then slowly increased along with the increase of the current density, because the copper is subjected to electric crystallization instant nucleation under low current density, the surface nucleation number is small, the grain size is large, the number of crystal nuclei is increased along with the increase of the current density, but the grain diameter is small and is not beneficial to interconnection, so that the current density adopted by the conventional pulse electroplating method is 2-4A/dm 2 However, the deposition rate of the copper layer is lower at the current density, which results in a lower throughput and higher cost of electroplating the copper layer.
Disclosure of Invention
The invention aims to solve the defects of low copper layer preparation productivity and high cost caused by low deposition rate of the existing pulse copper layer electroplating method, and provides a method for quickly electroplating a high-conductivity and high-heat-conductivity copper layer.
In order to solve the defects of the prior art, the invention provides the following technical solutions:
a method for quickly electroplating a copper layer with high electric conductivity and high thermal conductivity is characterized by comprising the following steps:
step 1, preparing a composite electroplating solution;
the composite electroplating solution comprises metal copper ions and metal copper particles, and the metal copper particles are uniformly suspended in the composite electroplating solution; the composite electroplating solution is acidic;
step 2, electroplating a copper layer;
adopting bipolar pulse electroplating to electrically connect the anode of a constant current power supply with metal copper, electrically connecting the cathode of the constant current power supply with a precursor to be plated, and plating a seed layer on the precursor to be plated; placing the metal copper and the precursor to be plated in the composite electroplating solution prepared in the step 1;
controlling the temperature of the composite electroplating solution to be 25-80 ℃, and stirring the composite electroplating solution;
setting constant current power supply parameters, and quickly electroplating a high-conductivity and high-heat-conductivity copper layer;
the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively as follows:
the current density of the first stage is 0.5-2A/dm 2 The duty ratio of the forward current pulse is 30-70%, the duty ratio of the reverse current pulse is 0-20%, and the electroplating time is 60 s;
the current density of the second stage is set to be 2-5A/dm 2 The duty ratio of the forward current pulse is 30-70%, the duty ratio of the reverse current pulse is 0-20%, and the electroplating time is 120 s;
the current density of the third stage is set to be 17-20A/dm 2 The duty ratio of the forward current pulse is 30-70%, the duty ratio of the reverse current pulse is 0-20%, and the electroplating time is 200-600 s.
Further, in the step 2, the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively:
the current density of the first stage is 2A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 0%, and the electroplating time is 60 s;
the current density in the second stage was set to 5A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the electroplating time is 120 s;
the current density of the third stage was set to 17.7A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the plating time is 200 s.
Further, in step 1, the composite plating solution includes copper sulfate pentahydrate (CuSO4 · 5H2O), and the mass ratio between the copper sulfate pentahydrate and the metallic copper particles is 5: 1.
Further, in the step 1, the diameter of the metal copper particles is 0.1-20 μm; the smaller diameter of the copper metal particles leads to higher cost, and the larger diameter of the copper metal particles weakens the adsorption force.
Further, in the step 1, the composite electroplating solution further comprises sodium hypophosphite, sodium citrate, disodium ethylene diamine tetraacetate and thiourea, and the pH value of the composite electroplating solution is 5.
Further, in the step 2, the seed layer is prepared by a physical vacuum method or a chemical plating method, the seed layer is a copper layer or a nickel layer or a chromium layer or a nickel-chromium alloy layer, and the thickness of the seed layer is 0.1-10 μm; the seed layer provides a conductive layer for electroplating.
Further, in step 2, the precursor to be plated is a heterojunction cell or a silicon substrate cell provided with a transparent conductive layer.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a method for quickly electroplating a high-conductivity and high-heat-conductivity copper layer, which adopts bipolar pulse electroplating and divides the electroplating process into three stages, wherein the first stage and the second stage adopt an adhesion compact layer formed on the surface of a seed layer by low current density, and the third stage adopts a copper particle accumulation layer and a compact filling layer formed on the adhesion compact layer by high current density; the invention can realize the rapid deposition of the copper layer, and the electrical property of the deposited copper layer is close to that of pure copper, thereby improving the preparation capacity of the copper layer and reducing the production cost.
Detailed Description
The invention will be further described with reference to exemplary embodiments.
Example 1
A method for quickly electroplating a high-conductivity high-thermal-conductivity copper layer comprises the following steps:
step 1, preparing a composite electroplating solution;
500g of copper sulfate pentahydrate (CuSO) is taken 4 ·5H 2 O), 50g of sodium hypophosphite, 50g of sodium citrate, 10g of disodium ethylene diamine tetraacetate and 25g of thiourea are sequentially added into deionized water and stirred to be dissolved; adding sulfuric acid to adjust the pH value to 5; then, 100g of metallic copper particles having an average diameter of 5 μm were added, and the mixture was stirred so that the weak acid solution would coat the copper powderRemoving impurities on the surface to obtain a composite electroplating solution;
step 2, electroplating a copper layer;
adopting bipolar pulse electroplating, electrically connecting the anode of a constant current power supply with metal copper, electrically connecting the cathode of the constant current power supply with a precursor to be plated, and plating a seed layer on the precursor to be plated, wherein the thickness of the seed layer is 0.1-10 mu m;
placing the metal copper and the precursor to be plated in the composite electroplating solution prepared in the step 1;
controlling the temperature of the composite electroplating solution to be 50 ℃;
the composite electroplating solution is internally provided with a stirring device, the rotating speed is set to 600r/min, so that the concentration of metal copper ions in the electrolyte of the cathode accessory in the electroplating process can be kept normal, the concentration polarization is reduced, the cathode current density is improved, and the deposition speed is accelerated;
setting constant current power supply parameters to quickly electroplate a high-conductivity and high-heat-conductivity copper layer;
the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively as follows:
the current density of the first stage is 2A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 0%, and the electroplating time is 60 s;
the current density in the second stage was set to 5A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the electroplating time is 120 s;
the current density of the third stage was set to 17.7A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the electroplating time is 200 s;
and obtaining a copper layer after the third stage is finished, wherein the copper layer comprises an adhesion compact layer formed by low current density adopted in the first stage and the second stage, a copper particle accumulation layer and a compact filling layer formed by high current density adopted in the third stage, the total thickness of the copper layer is 10.25 mu m, the sheet resistance is 0.00185 omega/□, and the bulk resistivity is 1.85 mu omega cm.
Example 2
In step 2 of this embodiment, the temperature of the composite electroplating solution is controlled to be 25 ℃;
the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively as follows:
the current density in the first stage is 1A/dm 2 The duty ratio of the forward current pulse is 40%, the duty ratio of the reverse current pulse is 10%, and the electroplating time is 60 s;
the current density in the second stage was set to 3A/dm 2 The duty ratio of the forward current pulse is 40%, the duty ratio of the reverse current pulse is 10%, and the electroplating time is 120 s;
the current density of the third stage was set to 18.5A/dm 2 The duty ratio of the forward current pulse is 40 percent, the duty ratio of the reverse current pulse is 10 percent, and the electroplating time is 300 s;
after the third stage, a copper layer was obtained, the total thickness of the copper layer was 15.74. mu.m, the sheet resistance was 0.00128. omega./□, and the bulk resistivity was 1.92. mu. omega. cm.
The rest of the setup of this example is the same as example 1.
Example 3
In step 2 of this embodiment, the temperature of the composite electroplating solution is controlled to 80 ℃;
the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively as follows:
the current density of the first stage is 2A/dm 2 The duty ratio of the forward current pulse is 50%, the duty ratio of the reverse current pulse is 15%, and the electroplating time is 60 s;
the current density in the second stage was set to 4A/dm 2 The duty ratio of the forward current pulse is 50%, the duty ratio of the reverse current pulse is 15%, and the electroplating time is 120 s;
the current density of the third stage is set to 18.8A/dm 2 The duty ratio of the forward current pulse is 50%, the duty ratio of the reverse current pulse is 15%, and the electroplating time is 400 s;
after the third stage, a copper layer was obtained, the total thickness of the copper layer was 20.63. mu.m, the sheet resistance was 0.00093. omega./□, and the bulk resistivity was 1.86. mu. omega. cm.
The rest of the setup of this example is the same as example 1.
Example 4
In step 2 of this embodiment, the temperature of the composite plating solution is controlled to 80 ℃;
the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively as follows:
the current density in the first stage is 0.5A/dm 2 The duty ratio of the forward current pulse is 30%, the duty ratio of the reverse current pulse is 0%, and the electroplating time is 60 s;
the current density in the second stage is set to 2A/dm 2 The duty ratio of the forward current pulse is 30%, the duty ratio of the reverse current pulse is 0%, and the electroplating time is 120 s;
the current density of the third stage was set to 19.1A/dm 2 The duty ratio of the forward current pulse is 30%, the duty ratio of the reverse current pulse is 0%, and the electroplating time is 500 s;
and obtaining a copper layer after the third stage, wherein the total thickness of the copper layer is 25.19 mu m, the sheet resistance is 0.000784 omega/□, and the volume resistivity is 1.96 mu omega cm.
The rest of the setup of this example was the same as example 1.
Example 5
In step 2 of this embodiment, the temperature of the composite electroplating solution is controlled to 80 ℃;
the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively as follows:
the current density of the first stage is 2A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the electroplating time is 60 s;
the current density in the second stage was set to 5A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the electroplating time is 120 s;
the current density of the third stage was set to 18.6A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the electroplating time is 600 s;
and obtaining a copper layer after the third stage, wherein the total thickness of the copper layer is 30.38 mu m, the sheet resistance is 0.000676 omega/□, and the bulk resistivity is 2.03 mu omega cm.
The rest of the setup of this example is the same as example 1.
Examples 1 to 5, the constant current source parameter settings for the third stage and the properties of the copper layers produced are shown in table 1:
TABLE 1
As can be seen from table 1, in the case of the same settings, the thickness of the plated layer increases linearly with the increase of the plating time in the third stage, and the bulk resistivity of the copper plated layer approaches that of pure copper (1.76 μ Ω · cm), from which it can be seen that the electrical properties of the copper layer prepared according to the present invention have those of pure copper.
The above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same, and it is obvious for a person skilled in the art to modify the specific technical solutions described in the foregoing embodiments or to substitute part of the technical features, and these modifications or substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions protected by the present invention.
Claims (7)
1. A method for quickly electroplating a high-conductivity high-thermal-conductivity copper layer is characterized by comprising the following steps:
step 1, preparing a composite electroplating solution;
the composite electroplating solution comprises metal copper ions and metal copper particles, and the metal copper particles are uniformly suspended in the composite electroplating solution; the composite electroplating solution is acidic;
step 2, electroplating a copper layer;
adopting bipolar pulse electroplating to electrically connect the anode of a constant current power supply with metal copper, electrically connecting the cathode of the constant current power supply with a precursor to be plated, and plating a seed layer on the precursor to be plated; placing the metal copper and the precursor to be plated in the composite electroplating solution prepared in the step 1;
controlling the temperature of the composite electroplating solution to be 25-80 ℃, and stirring the composite electroplating solution;
setting constant current power supply parameters, and quickly electroplating a high-conductivity and high-heat-conductivity copper layer;
the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively as follows:
the current density of the first stage is 0.5-2A/dm 2 The duty ratio of the forward current pulse is 30-70%, the duty ratio of the reverse current pulse is 0-20%, and the electroplating time is 60 s;
the current density of the second stage is set to be 2-5A/dm 2 The duty ratio of the forward current pulse is 30-70%, the duty ratio of the reverse current pulse is 0-20%, and the electroplating time is 120 s;
the current density of the third stage is set to be 17-20A/dm 2 The duty ratio of the forward current pulse is 30-70%, the duty ratio of the reverse current pulse is 0-20%, and the electroplating time is 200-600 s.
2. The method for rapidly electroplating the copper layer with high electric conductivity and high thermal conductivity according to claim 1, wherein the method comprises the following steps: in the step 2, the electroplating process is divided into three stages, and the parameters of the constant current power supply in the three stages are respectively as follows:
the current density of the first stage is 2A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 0%, and the electroplating time is 60 s;
the current density in the second stage was set to 5A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the electroplating time is 120 s;
the current density of the third stage was set to 17.7A/dm 2 The duty ratio of the forward current pulse is 70%, the duty ratio of the reverse current pulse is 20%, and the plating time is 200 s.
3. The method for rapidly electroplating the copper layer with high electric conductivity and high thermal conductivity according to claim 1 or 2, wherein: in the step 1, the composite plating solution comprises copper sulfate pentahydrate, and the mass ratio of the copper sulfate pentahydrate to the metal copper particles is 5: 1.
4. The method for rapidly electroplating the copper layer with high electric conductivity and high thermal conductivity according to claim 3, wherein the method comprises the following steps: in the step 1, the diameter of the metal copper particles is 0.1-20 μm.
5. The method for rapidly electroplating the copper layer with high electrical conductivity and high thermal conductivity according to claim 4, wherein the method comprises the following steps: in the step 1, the composite electroplating solution further comprises sodium hypophosphite, sodium citrate, disodium ethylene diamine tetraacetate and thiourea, and the pH value of the composite electroplating solution is 5.
6. The method for rapidly electroplating the copper layer with high electrical conductivity and high thermal conductivity according to claim 5, wherein: in the step 2, the seed layer is prepared by a physical vacuum method or a chemical plating method, the seed layer is a copper layer or a nickel layer or a chromium layer or a nickel-chromium alloy layer, and the thickness of the seed layer is 0.1-10 μm.
7. The method as claimed in claim 6, wherein the copper layer with high conductivity and high thermal conductivity is plated rapidly by the following steps: in the step 2, the precursor to be plated is a heterojunction cell or a silicon substrate cell provided with a transparent conducting layer.
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| CN202210650700.XA CN114959814A (en) | 2022-06-09 | 2022-06-09 | Method for quickly electroplating high-conductivity and high-heat-conductivity copper layer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117328113A (en) * | 2023-10-16 | 2024-01-02 | 广东省广新离子束科技有限公司 | Acid copper plating process for metallized film and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5972192A (en) * | 1997-07-23 | 1999-10-26 | Advanced Micro Devices, Inc. | Pulse electroplating copper or copper alloys |
| CN104120473A (en) * | 2013-04-24 | 2014-10-29 | 中芯国际集成电路制造(上海)有限公司 | Copper electroplating method |
| CN113881983A (en) * | 2021-10-19 | 2022-01-04 | 广州市慧科高新材料科技有限公司 | Through hole pulse electroplating liquid and through hole pulse electroplating coating method |
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2022
- 2022-06-09 CN CN202210650700.XA patent/CN114959814A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5972192A (en) * | 1997-07-23 | 1999-10-26 | Advanced Micro Devices, Inc. | Pulse electroplating copper or copper alloys |
| CN104120473A (en) * | 2013-04-24 | 2014-10-29 | 中芯国际集成电路制造(上海)有限公司 | Copper electroplating method |
| CN113881983A (en) * | 2021-10-19 | 2022-01-04 | 广州市慧科高新材料科技有限公司 | Through hole pulse electroplating liquid and through hole pulse electroplating coating method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117328113A (en) * | 2023-10-16 | 2024-01-02 | 广东省广新离子束科技有限公司 | Acid copper plating process for metallized film and application |
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