CN112779574B - Electroplating solution for enhancing conductivity of electronic copper foil, preparation method and electroplating process - Google Patents
Electroplating solution for enhancing conductivity of electronic copper foil, preparation method and electroplating process Download PDFInfo
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- CN112779574B CN112779574B CN202011466893.0A CN202011466893A CN112779574B CN 112779574 B CN112779574 B CN 112779574B CN 202011466893 A CN202011466893 A CN 202011466893A CN 112779574 B CN112779574 B CN 112779574B
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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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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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
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
Abstract
The invention discloses an electroplating solution for enhancing conductivity of an electronic copper foil, a preparation method and an electroplating process, wherein the electroplating solution comprises the following components: using a mixed solution of 100-150 parts of 1-ethyl-3-methylimidazole chloride (EMIMCl) and 63-95 parts of absolute ethyl Alcohol (AE) as a solvent, and carrying out anhydrous treatment on arsenic trichloride (AsCl) 3 ) 1 to 6 parts of anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of cosolvent, 10.3 to 20.8 parts of additive and 0.1 to 0.5 part of additive as solute. According to the invention, the electrical conductivity of the electronic copper foil is enhanced by electrodepositing a layer of NbAs alloy film on the electronic copper foil, and the prepared NbAs alloy film has the advantages of strong bonding capability with the electronic copper foil, high electrical conductivity and thermal conductivity, good chemical stability, simple process, no environmental pollution, low energy consumption and high repeatability.
Description
Technical Field
The invention relates to the field of copper foil manufacturing, in particular to an electroplating solution for enhancing the conductivity of an electronic copper foil, a preparation method and an electroplating process.
Background
The electronic copper foil is widely applied to a battery structure, can effectively improve the adhesive force of a positive electrode material and a collector of an aqueous system, but the traditional copper foil production process has the problems of low production efficiency, overlarge resistance, poor energy conversion effect, poor conductive performance of products, short service life, difficult removal after damage, environmental damage and the like, and restricts the further development of integrated circuit technologies such as chips and the like.
At present, a scholars utilize three elements of niobium chloride, arsenic and hydrogen to carry out chemical reaction together to prepare the niobium arsenide nanobelt, the surface of the niobium arsenide nanobelt has a surface state which can allow electrons to pass through rapidly, the conductivity is one hundred times of that of a copper film, the conductivity is one thousand times of that of graphene, and the fermi arc with the anti-sequence property causes the reduction of energy consumption. More importantly, the high-conductivity mechanism of niobium arsenide is still effective even at room temperature, unlike superconducting materials which can only be applied at ultralow temperature of tens of degrees below zero, the material has conductivity about three times that of copper at room temperature, and the discovery has great value in reducing the energy consumption of electronic devices and the like.
More research work is focused on the preparation of niobium arsenide films, and various technologies such as MBE, CVD, MOCVD, LPE, RF sputtering and the like are used for preparing niobium arsenide (NbAS) films, but most of the technologies have the defects of long production period, complex equipment, high energy consumption, high cost, environmental pollution and the like, and in the prior art, the application of electrodepositing the niobium arsenide films on copper foils to enhance the conductivity of electronic copper foils is not available.
Disclosure of Invention
The invention aims to provide an electroplating solution for enhancing the conductivity of an electronic copper foil, a preparation method and an electroplating process, so as to solve the problems in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
an electroplating solution for enhancing the conductivity of an electronic copper foil, which comprises the following components: using a mixed solution of 100-150 parts of 1-ethyl-3-methylimidazole chloride (EMIMCl) and 63-95 parts of absolute ethyl Alcohol (AE) as a solvent, and carrying out anhydrous treatment on arsenic trichloride (AsCl) 3 ) 1 to 6 parts of anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of cosolvent, 10.3 to 20.8 parts of additive and 0.1 to 0.5 part of additive as solute.
As a further scheme of the invention: the cosolvent is propylene carbonate and cationic cellulose, wherein the propylene carbonate is 0.3-0.8 part, and the cationic cellulose is 10-20 parts.
As a further scheme of the invention: the additive is 8-hydroxyquinoline.
As a further scheme of the invention: 100 to 150 parts of 1-ethyl-3-methylimidazole chloride (EMIMCl), 63 to 95 parts of absolute ethyl Alcohol (AE) and anhydrous arsenic trichloride (AsCl) 3 ) 1 to 6 parts of anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of propylene carbonate and 0.3 to 0.8 part of cationic cellulose, and 0.1 to 0.5 part of 8-hydroxyquinoline.
In an inert gas environment, a solution of 100 to 150 parts of EMIMCl and 63 to 95 parts of absolute ethyl alcohol is placed into an electrolytic tank, and anhydrous arsenic trichloride (AsCl) is added into the mixed solution 3 ) 1 to 6 parts of anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of propylene carbonate, 0.3 to 0.8 part of cationic cellulose, 10 to 20 parts of 8-hydroxyquinoline and 0.1 to 0.5 part of 8-hydroxyquinoline, and adding ultrasonic stirring for 4 to 12 hours to obtain the electroplating solution.
A plating process according to the above-described plating solution, comprising the steps of:
s1: adopting an electronic copper foil as a cathode, a platinum sheet or graphite as an anode, washing with acetone, activating with dilute hydrochloric acid, washing with deionized water, degreasing with acetone, and air-drying;
s2: preparing electroplating solution in an electrolytic tank in an inert gas environment;
s3: and (3) placing the pretreated cathode and anode into electroplating solution, keeping the polar distance at 1-3 cm, keeping the temperature at 70-150 ℃, controlling the stirring speed at 180-600 revolutions per minute, controlling the bath pressure at 15-30V, and carrying out constant current electroplating for 15-30 minutes to obtain the cathode alloy coating.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the electrical conductivity of the electronic copper foil is enhanced by electrodepositing a NbAs alloy film layer on the electronic copper foil. The invention adopts an electrodeposition method, and the electrodeposition is a simple, low-cost and small-pollution process, and is suitable for preparing III-V and II-VI compound semiconductor films. Nb and its alloys are electrodeposited from a high temperature molten salt solution, but relatively few substrates can be used due to the aggressive conditions of deposition; the most promising alternatives to these high temperature electrolytes are low temperature ionic liquids, and ionic liquids have electrochemical windows wide enough to allow electrodeposition of Nb and As elements, based on the above principle, the present invention utilizes a solution made of AsCl 3 ，NbCl 5 And EMIMCl, the method can obtain NbAS alloy film layer on the surface of the electronic copper foil without high-temperature post-treatment; the NbAs alloy film layer prepared by the invention has strong bonding capability with the electronic copper foil, high electric conductivity and thermal conductivity and good chemical stability, can be used for manufacturing novel electronic equipment, and has the advantages of simple process, no environmental pollution, low energy consumption and high repeatability.
Drawings
FIG. 1 is a surface topography of an NbAs alloy film layer of the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention aims to provide an electroplating solution, a preparation method and an electroplating process for enhancing the conductivity of an electronic copper foil, which are characterized in that the existing preparation of a niobium arsenide film has the defects of long production period, complex equipment, high energy consumption, high cost, environmental pollution and the like, and the existing technology for enhancing the conductivity of the electronic copper foil by depositing the niobium arsenide film on the electronic copper foil does not exist at present 3 ，NbCl 5 And EMIMCl, and can obtain NbAS alloy film layer on the surface of electronic copper foil. As element is added, the grain refinement is facilitated, so that the binding force between the alloy film and the electronic copper foil is enhanced; niobium arsenide has high conductivity and thermal conductivity because of its ultrahigh mobility with very high electron concentration; the NbAs alloy film layer prepared by the invention has strong bonding capability with the electronic copper foil, high electric conductivity and thermal conductivity and good chemical stability because of the NbAs three-dimensional framework structure and good stability in a wider acid-base range, and the invention has the advantages of simple process, no environmental pollution, less energy consumption and high repeatability.
An electroplating solution for enhancing the conductivity of an electronic copper foil, which comprises the following components: using a mixed solution of 100-150 parts of 1-ethyl-3-methylimidazole chloride (EMIMCl) and 63-95 parts of absolute ethyl Alcohol (AE) as a solvent, and carrying out anhydrous treatment on arsenic trichloride (AsCl) 3 ) 1 to 6 parts of anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of cosolvent, 10.3 to 20.8 parts of additive and 0.1 to 0.5 part of additive as solute.
100-150 parts of 1-ethyl-3-methylimidazole chloride (EMIMCl), 63-95 parts of absolute ethyl Alcohol (AE), and using the 1-ethyl-3-methylimidazole chloride (EMIMCl) and the absolute ethyl alcohol as anhydrous solvents, wherein the existence of the hydrogen evolution side reaction is prevented by adopting an aqueous solution, and the quality of a coating is influenced.
The anhydrous treated arsenic trichloride (AsCl) 3 ) 1 to 6 parts of the anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of anhydrous arsenic trichlorideAsCl 3 ) Anhydrous niobium pentachloride (NbCl) 5 ) Alloy raw materials required for electroplating are provided.
The cosolvent is propylene carbonate and cationic cellulose, wherein the propylene carbonate accounts for 0.3-0.8 part, the cationic cellulose accounts for 10-20 parts, and the propylene carbonate and the cationic cellulose accelerate dissolution of the inorganic electroplating raw materials.
The additive is 8-hydroxyquinoline, 0.1-0.5 part of 8-hydroxyquinoline is used as an electroplating additive, and the cathode polarization is increased, and alloy crystallization and nucleation are controlled.
In an inert gas environment, a solution of 100 to 150 parts of EMIMCl and 63 to 95 parts of absolute ethyl alcohol is placed into an electrolytic tank, and anhydrous arsenic trichloride (AsCl) is added into the mixed solution 3 ) 1 to 6 parts of anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of propylene carbonate, 0.3 to 0.8 part of cationic cellulose, 10 to 20 parts of 8-hydroxyquinoline and 0.1 to 0.5 part of 8-hydroxyquinoline, and adding ultrasonic stirring for 4 to 12 hours to obtain the electroplating solution.
A plating process according to the above-described plating solution, comprising the steps of:
s1: adopting an electronic copper foil as a cathode, a platinum sheet or graphite as an anode, washing with acetone, activating with dilute hydrochloric acid, washing with deionized water, degreasing with acetone, and air-drying;
s2: preparing electroplating solution in an electrolytic tank according to the parts and the preparation method in an inert gas environment;
s3: and (3) placing the pretreated cathode and anode into electroplating solution, keeping the polar distance at 1-3 cm, keeping the temperature at 70-150 ℃, controlling the stirring speed at 180-600 revolutions per minute, controlling the bath pressure at 15-30V, and carrying out constant current electroplating for 15-30 minutes to obtain the cathode alloy coating.
Example 1
The electroplating solution provided in this example comprises, by mass, 146 parts of EMIMCl, 94 parts of absolute ethyl alcohol, and 4 parts of absolute AsCl 3 6 parts of anhydrous NbCl 5 12.6 parts of cosolvent and 0.4 part of additive;
wherein the cosolvent is 12 parts of cationic cellulose and 0.6 part of propylene carbonate;
wherein the additive is 0.4 part of 8-hydroxyquinoline.
The electroplating solution is prepared according to the following steps: placing the mixed solution of EMIMCl and absolute ethyl alcohol into a self-made electrolytic tank, and then respectively adding absolute AsCl into the mixed solution 3 Anhydrous NbCl 5 And (3) mixing the cationic cellulose, 8-hydroxyquinoline and propylene carbonate for 10 hours by mechanical stirring and ultrasonic stirring to obtain the electroplating solution.
The electroplating process for electroplating by using the electroplating solution is carried out according to the following steps:
s1: adopting an electronic copper foil as a cathode, a platinum sheet or graphite as an anode, washing with acetone, activating with dilute hydrochloric acid, washing with deionized water, degreasing with acetone, and air-drying;
s2: preparing electroplating solution in an electrolytic tank in an inert gas environment;
s3: and (3) placing the pretreated cathode and anode into electroplating solution, keeping the polar distance at 2cm, keeping the temperature at 80 ℃, controlling the stirring speed at 400 revolutions per minute, controlling the bath pressure at 15V, and carrying out constant current electroplating for 15 minutes to obtain the cathode alloy plating layer.
Example 2
The electroplating solution preparation method and electroplating process steps adopted in this example are the same as those in example 1, except that the proportions of the components adopted in this example are different, and the electroplating solution provided in this example comprises, by mass, 100 parts of EMIMCl, 63 parts of absolute ethyl alcohol and 1 part of absolute AsCl 3 2 parts of anhydrous NbCl 5 10.3 parts of cosolvent and 0.1 part of additive;
wherein the cosolvent is 10 parts of cationic cellulose and 0.3 part of propylene carbonate;
wherein the additive is 0.1 part of 8-hydroxyquinoline.
The method for preparing the plating solution and the plating process of this example are the same as those of example 1.
Example 3
The electroplating solution preparation method and electroplating process steps adopted in this embodiment are the same as those in embodiment 1, except that the proportions of the components adopted in this embodiment are differentThe electroplating solution provided in the example comprises, by mass, 150 parts of EMIMCl, 95 parts of absolute ethyl alcohol and 6 parts of absolute AsCl 3 9 parts of anhydrous NbCl 5 20.8 parts of cosolvent and 0.5 part of additive;
wherein the cosolvent is 20 parts of cationic cellulose and 0.8 part of propylene carbonate;
wherein the additive is 0.5 part of 8-hydroxyquinoline.
The method for preparing the plating solution and the plating process of this example are the same as those of example 1.
Example 4
The electroplating solution preparation method and electroplating process steps adopted in this example are the same as those in example 1, except that the proportions of the components adopted in this example are different, and the electroplating solution provided in this example comprises, by mass, 125 parts of EMIMCl, 79 parts of absolute ethyl alcohol and 3 parts of absolute AsCl 3 5 parts of anhydrous NbCl 5 15.6 parts of cosolvent and 0.3 part of additive;
wherein the cosolvent is 15 parts of cationic cellulose and 0.6 part of propylene carbonate;
wherein the additive is 0.3 part of 8-hydroxyquinoline.
The method for preparing the plating solution and the plating process of this example are the same as those of example 1.
Comparative example 1
The comparative example is a traditional electronic copper foil, and the traditional electronic copper foil plating solution consists of the following components in parts by weight: niSO 4 ·6H 2 O60 parts, coSO 4 ·7H 2 O40 parts, cuSO 4 ·5H 2 O5 part, H 3 BO 3 1 part, na 2 SO 4 10 parts, C 6 H 5 Na 3 O 7 2 parts, C 12 H 25 SO 4 Na 0.2 parts, all analytically pure.
The components are mixed to prepare the traditional electronic copper foil electroplating solution.
The electroplating process for electroplating by using the electroplating solution is carried out according to the following steps:
s1: adopting an electronic copper foil as a cathode, a platinum sheet or graphite as an anode, washing with acetone, activating with dilute hydrochloric acid, washing with deionized water, degreasing with acetone, and air-drying;
s2: preparing electroplating solution in an electrolytic tank in an inert gas environment;
s3: placing the pretreated cathode and anode into electroplating solution, maintaining the temperature at 25deg.C, stirring at 400 rpm, pH value of 4.0, and plating time of 25min at current density of 3A/dm respectively 2 And obtaining the cathode alloy coating.
Comparative example 2
The plating solution preparation method and the plating process steps adopted in this comparative example are the same as those in example 1, except that the proportions of the components adopted in this comparative example are different, and the plating solution provided in this comparative example comprises, by mass, 160 parts of EMIMCl, 100 parts of absolute ethyl alcohol, and 7 g of absolute AsCl 3 10 g of anhydrous NbCl 5 24.2 parts of cosolvent and 0.7 part of additive;
wherein the cosolvent is 23 parts of cationic cellulose and 1.2 parts of propylene carbonate;
wherein the additive is 0.7 part of 8-hydroxyquinoline.
The preparation method and plating process of the plating solution of this comparative example were the same as those of example 1.
Effect example
The copper foils of examples 1 to 4 and comparative examples 1 to 2 were subjected to conductivity, average friction factor and bonding force test, and the surface contact resistance, bonding rate and average friction factor of the copper foils were measured as shown in table 1 below.
TABLE 1
| Contact resistance (/ mu omega) | Binding force (N) | Average moleFactor of wiping | |
| Example 1 | 4.1 | 25 | 0.88 |
| Example 2 | 11.2 | 23.5 | 0.81 |
| Example 3 | 10.5 | 23.74 | 0.83 |
| Example 4 | 11.6 | 23.61 | 0.85 |
| Comparative example 1 | 23.6 | 21.5 | 0.73 |
| Comparative example 2 | 25.7 | 12.55 | 0.74 |
As can be seen from the above Table 1, compared with comparative examples 1 and 2, the electroplating solution adopted in examples 1 to 4 provided by the invention has the advantages that the prepared NbAs alloy film layer has strong bonding capability with the electronic copper foil, the contact resistance is remarkably reduced, the electric conductivity and the heat conductivity are remarkably enhanced, and the chemical stability is good.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (5)
1. An electroplating solution for enhancing the conductivity of an electronic copper foil is characterized by comprising the following components: using a mixed solution of 100-150 parts of 1-ethyl-3-methylimidazole chloride (EMIMCl) and 63-95 parts of absolute ethyl alcohol as a solvent, and carrying out anhydrous treatment on arsenic trichloride (AsCl) 3 ) 1 to 6 parts of anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of cosolvent, 10.3 to 20.8 parts of additive and 0.1 to 0.5 part of additive as solute.
2. The plating solution for enhancing the conductivity of an electronic copper foil according to claim 1, wherein the cosolvent is propylene carbonate, and further comprising cationic cellulose, wherein the propylene carbonate is 0.3 to 0.8 parts, and the cationic cellulose is 10 to 20 parts.
3. The electroplating solution for enhancing the conductivity of an electronic copper foil according to claim 1, wherein the additive is 8-hydroxyquinoline.
4. A method for producing a plating solution according to any one of claims 1 to 3, wherein a solution of 100 to 150 parts of EMIMCl and 63 to 95 parts of absolute ethyl alcohol is placed in an electrolytic bath in an inert atmosphere, and anhydrous arsenic trichloride (AsCl) is added to the mixed solution 3 ) 1 to 6 parts of anhydrous niobium pentachloride (NbCl) 5 ) 2 to 9 parts of propylene carbonate, 0.3 to 0.8 part of cationic cellulose, 10 to 20 parts of 8-hydroxyquinoline and 0.1 to 0.5 part of 8-hydroxyquinoline, and adding ultrasonic stirring for 4 to 12 hours to obtain the electroplating solution.
5. A plating process of a plating solution according to any one of claims 1 to 3, comprising the steps of:
s1: adopting an electronic copper foil as a cathode, a platinum sheet or graphite as an anode, washing with acetone, activating with dilute hydrochloric acid, washing with deionized water, degreasing with acetone, and air-drying;
s2: preparing electroplating solution in an electrolytic tank in an inert gas environment;
s3: and (3) placing the pretreated cathode and anode into electroplating solution, keeping the polar distance at 1-3 cm, keeping the temperature at 70-150 ℃, controlling the stirring speed at 180-600 revolutions per minute, controlling the bath pressure at 15-30V, and carrying out constant current electroplating for 15-30 minutes to obtain the cathode alloy coating.
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| 张世超 等.铜箔表面粗化工艺的研究.《电镀与精饰》.2005,第27卷(第5期),第1-3页. * |
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