CN115305528B - Method and device for preparing prestressed electrolytic copper foil - Google Patents
Method and device for preparing prestressed electrolytic copper foil Download PDFInfo
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- CN115305528B CN115305528B CN202211032324.4A CN202211032324A CN115305528B CN 115305528 B CN115305528 B CN 115305528B CN 202211032324 A CN202211032324 A CN 202211032324A CN 115305528 B CN115305528 B CN 115305528B
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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
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a method and a device for preparing a prestressed electrolytic copper foil, which comprises the following steps: (1) preparing electrolyte; (2) cathode plate installation: one end of the driving mechanism can be fixed, and the other end is connected with the driving mechanism; or both ends are connected with the transmission mechanism; the transmission mechanism is used for applying single tensile stress, compressive stress or shear stress or a combination of the above stresses to the cathode plate; (3) debugging the transmission mechanism and observing the deformation of the cathode plate; finally filling electrolyte into the electrolytic tank; (4) preparing an initial electrodeposited layer; (5) preparing a second electrodeposited layer; (6) The steps (4) and (5) are repeated, and the electrolytic copper foil with certain gradient alternate distribution of internal stress with different properties in the thickness direction can be prepared; (7) The electrolytic copper foil is peeled off from the cathode plate and subjected to subsequent surface treatment. The invention can obviously improve the room temperature, high temperature tensile strength and elongation of the copper foil, and improve the high temperature resistance and service life of the copper foil.
Description
Technical Field
The invention relates to the technical field of electrolytic copper foil preparation, in particular to a method and a device for preparing a prestressed electrolytic copper foil.
Background
The electrolytic copper foil is an important material for manufacturing a printed circuit board, a copper-clad plate and a lithium ion battery negative current collector. With the rapid development of the electronic information technology in the current 5G age, on one hand, in the high-frequency and high-speed signal transmission process, a large amount of high-speed electronics 'skin-seeking' violent friction can lead the working environment temperature of a circuit to be locally higher than 100 ℃, so that heterogeneous interfaces in a substrate are inconsistent in thermal expansion and contraction, and further the circuit is peeled off, broken or deformed from the substrate; on the other hand, with miniaturization of electronic components and high integration of circuit boards, the heat dissipation space of the working environment is reduced, and the local working temperature of the transmission line is further increased. Therefore, the high-temperature mechanical properties of the electrolytic copper foil, particularly the high-temperature tensile strength and elongation, are key factors for determining the service performance of the copper foil.
In the process of developing the electrolytic copper foil towards the directions of flattening, flattening and thinning, the high-temperature mechanical property of the electrolytic copper foil is also weakened to a certain extent. The current common practice for meeting certain high-temperature mechanical properties of the ultrathin electrolytic copper foil is as follows: firstly, various additives are added to achieve grain refinement and homogenization, so that the mechanical property of the copper foil is improved; and secondly, carrying out surface treatment or heat treatment to improve the mechanical properties of the copper foil. The addition of additives and surface treatment can cause the doping of the electrolytic copper foil; the heat treatment is easy to oxidize for the ultrathin electrolytic copper foil, so that the environmental condition of the heat treatment is more demanding and the cost is high.
From the current market, the demand of ultra-thin high-temperature high-resistance high-elongation electrolytic copper foil still tends to rise. The preparation method of the ultrathin high-temperature high-resistance high-elongation electrolytic copper foil with high efficiency, simplicity, convenience and low cost is found to have great significance.
Disclosure of Invention
The invention aims to provide a method and a device for preparing a prestressed electrolytic copper foil, and provides a brand new and low-cost method for improving the mechanical property of the electrolytic copper foil, wherein a cathode plate (or a cathode roller, hereinafter collectively referred to as a cathode plate) is subjected to certain periodic change of elastic deformation (partial restoration) -restoration during working by certain mechanical transmission, so that the electrolytic copper foil with prestressing force is prepared: the internal stress with macroscopically different properties forms a gradient distribution in the thickness direction. The prestress with gradient distribution greatly improves the mechanical property of the electrolytic copper foil, and can well adapt to stress damage caused by expansion and contraction, load change, impact and the like of the external environment.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the invention provides a method for preparing a prestressed electrolytic copper foil, which comprises the following steps:
(1) Preparing electrolyte: the preparation method is configured according to the existing production process of various electrolytic copper foils.
(2) And (3) negative plate installation: one end of the driving mechanism can be fixed, and the other end is connected with the driving mechanism; or both ends are connected with the transmission mechanism.
Note that the type of transmission mechanism designed may vary, the load transferred may be tension, pressure, torque or bending moment, but eventually a single tensile, compressive or shear stress, or a combination of the above stresses, must be applied to the cathode plate, which will undergo a periodic variation of "elastic deformation-recovery (partial recovery)" over a range.
The following uses a transmission mechanism for transmitting a single tensile force and applying a single tensile force to the cathode plate as an example, but not limited to screw transmission, a multi-rod mechanism, a gear rack and the like.
(3) And the transmission mechanism is debugged, so that the working stability of the cathode plate is ensured, and the deformation of the cathode plate can be observed through the scale or the displacement sensor. And finally filling electrolyte into the electrolytic tank.
(4) An initial electrodeposited layer is prepared. Without applying a tensile load (f=0) to the cathode plate, an initial deposition layer of a certain thickness H was prepared first, and the electrodeposition time was calculated according to the following formula 1:
T＝7.544×10 -3 ηBLH/I equation 1
In equation 1: t is the electrodeposition time(s); η is the current efficiency (%); b is the width (mm) of the cathode plate; l is the length (mm) of the cathode plate; h is the thickness (mm) of the copper foil; i is the amperage (A).
(5) A second electrodeposited layer is prepared. At this time, a tensile load (f=f) is applied to the cathode plate 1 ) Preparing a certain thickness H 1 The electrodeposition time is still calculated according to equation 1. The tensile load F is calculated and controlled according to the following formula 2:
F≤Aσ e s formula 2
In equation 2: f is a tensile load (N); a is the cross-sectional area (mm) of the cathode plate 2 )；σ e Is the elastic limit or yield limit (N/mm) of the cathode plate material 2 ) The method comprises the steps of carrying out a first treatment on the surface of the S is a safety coefficient.
(6) And (3) repeating the steps (4) and (5) to prepare the electrolytic copper foil with the internal stress (tensile stress and compressive stress) with different properties alternately distributed in a certain gradient in the thickness direction.
Of course, the order of steps (4) and (5) may be interchanged.
Of course, the variation of the load F may be any periodic or aperiodic variation.
(7) After the deposition is completed, the electrolytic copper foil is stripped from the cathode plate and subjected to subsequent surface treatments such as oxidation prevention and the like.
Further, the thickness of the cathode plate should not exceed 1mm; the load F is preferably a pulsating periodic variation.
Further, the thickness H of the copper foil in the step (4) is controlled to be 2.5-6 μm.
Further, in the step (5), the safety coefficient S is controlled to be 1.1-1.6.
The invention also provides a device for preparing the prestressed electrolytic copper foil. The device comprises an electrolyte preparation tank, an electrolytic tank, a screw transmission mechanism, a power supply, a rack and accessories such as connection, support, sealing, insulation and the like.
The screw transmission mechanism comprises a motor, a coupler, a screw rod, a rolling bearing, an upper end nut pull head, a guide rod, a lower end bolt, a nut, a displacement sensor and a tension sensor.
The whole outer part of the lower end fixing bolt is coated or covered with insulating materials and is connected with a ground wire; the whole outside of the upper end nut pull head (or the contact part with the cathode plate) is coated or covered with insulating materials; the whole outside of the fixing pieces at the upper end and the lower end of the cathode plate is also coated or covered with insulating materials; the motor and the screw rod coupler are insulated couplers.
The whole screw transmission stretching process should consider displacement deformation (deformation of a non-cathode plate) caused by fixing, connecting and insulating parts, and the accumulated deformation errors should be deducted when calculating the actual deformation of the cathode plate.
A servo motor, a motor driver, a displacement sensor, a tension sensor and a PLC controller are selected for configuration interface design, so that communication between an upper computer and a lower computer is realized, and automatic and accurate control of the whole system can be realized.
The bottom in the electrolyte preparation tank is provided with a heating pipe, one side bottom of the electrolyte preparation tank is provided with a liquid inlet pipe, the other end of the liquid inlet pipe is communicated to the top of the electrolyte preparation tank, a circulating pump is arranged between the electrolyte preparation tank and the electrolyte preparation tank, the circulating pump and the electrolyte preparation tank are connected to one side bottom of the electrolyte preparation tank through a liquid outlet pipe, and the circulating pump and the electrolyte preparation tank are communicated to the top of the electrolyte preparation tank through the liquid outlet pipe.
The beneficial effects of the invention are as follows:
the invention can obviously improve the room temperature, high temperature tensile strength and elongation of the copper foil, and improve the high temperature resistance and service life of the copper foil. The introduction of the additive impurities is reduced, the heat treatment link is omitted, and the cost is low. Is suitable for manufacturing various electrolytic copper foils and has wide application range.
Drawings
The drawings are merely examples of embodiments of the present invention from which other embodiments of the present invention may be derived by those skilled in the art without undue effort.
FIG. 1 is a schematic view of electrodeposition of a pre-stressed electrolytic copper foil according to the present invention, (a) is a schematic view of gradient distribution of internal stress of the copper foil, and (b) is a certain variation law of tensile load F applied by a cathode plate;
FIG. 2 is a schematic view of an electrolytic copper foil production apparatus.
Illustration of: 1. a motor; 2. a coupling; 3. a screw rod; 4. a rolling bearing; 5. a frame; 6. an upper end nut pull head; 7. a cathode plate; 8. an anode plate; 9. a lower end fixing bolt; 10. an electrolytic cell; 11. a power supply; 12. a ground wire; 13. a nut; 14. a circulation pump; 15. a liquid outlet pipe; 16. a liquid inlet pipe; 17. heating pipes; 18. a liquid preparing tank; 19. And a guide rod.
Detailed Description
The invention will now be described in further detail with reference to the drawings and to specific examples, which are only preferred embodiments of the invention and are not limiting thereof.
The electrolyte mainly comprises 90g/L of copper ions, 120g/L of sulfuric acid, 35mg/L of chloride ions, 1.5mg/L of gelatin and 1mg/L of SP. Controlling the current density to be 65A/dm 2 The reaction temperature was 60 ℃. A TA1 pure titanium plate is adopted as a cathode, a red copper plate with the purity of 99.9 percent is adopted as an anode, and the sizes are 0.5 multiplied by 450 multiplied by 1000mm. Copper foil thickness was measured using ICP4562 method, and tensile strength and copper foil were measured using ICP-TM-6502.3.18 methodElongation.
The invention provides a method for preparing a prestressed electrolytic copper foil, which comprises the following steps:
(1) Preparing electrolyte: the preparation method is configured according to the existing production process of various electrolytic copper foils.
(2) And (3) negative plate installation: one end of the driving mechanism can be fixed, and the other end is connected with the driving mechanism; or both ends are connected with the transmission mechanism.
Note that the type of transmission mechanism designed may vary, the load transferred may be tension, pressure, torque or bending moment, but eventually a single tensile, compressive or shear stress, or a combination of the above stresses, must be applied to the cathode plate, which will undergo a periodic variation of "elastic deformation-recovery (partial recovery)" over a range.
The following uses a transmission mechanism for transmitting a single tensile force and applying a single tensile force to the cathode plate as an example, but not limited to screw transmission, a multi-rod mechanism, a gear rack and the like.
(3) And the transmission mechanism is debugged, so that the working stability of the cathode plate is ensured, and the deformation of the cathode plate can be observed through the scale or the displacement sensor. And finally filling electrolyte into the electrolytic tank.
(4) An initial electrodeposited layer is prepared. Without applying a tensile load (f=0) to the cathode plate, an initial deposition layer of a certain thickness H was prepared first, and the electrodeposition time was calculated according to the following formula 1:
T＝7.544×10 -3 ηBLH/I equation 1
In equation 1: t is the electrodeposition time(s); η is the current efficiency (%); b is the width (mm) of the cathode plate; l is the length (mm) of the cathode plate; h is the thickness (mm) of the copper foil; i is the amperage (A).
(5) A second electrodeposited layer is prepared. At this time, a tensile load (f=f) is applied to the cathode plate 1 ) Preparing a certain thickness H 1 The electrodeposition time is still calculated according to equation 1. The tensile load F is calculated and controlled according to the following formula 2:
F≤Aσ e s formula 2
In equation 2: f is a tensile load (N); a is the cross-sectional area (mm) of the cathode plate 2 )；σ e Is the elastic limit or yield limit (N/mm) of the cathode plate material 2 ) The method comprises the steps of carrying out a first treatment on the surface of the S is a safety coefficient.
(6) And (3) repeating the steps (4) and (5), so that the electrolytic copper foil with certain gradient alternate distribution of internal stress (tensile stress and compressive stress) with different properties in the thickness direction is prepared as shown in figure 1.
Of course, the order of steps (4) and (5) may be interchanged.
Of course, the variation of the load F is not limited to that shown in fig. 1 (b), and may be any periodic or aperiodic variation.
(7) After the deposition is completed, the electrolytic copper foil is stripped from the cathode plate and subjected to subsequent surface treatments such as oxidation prevention and the like.
Further, the thickness of the cathode plate should not exceed 1mm; the load F is preferably a pulsating periodic variation.
Further, the thickness H of the copper foil in the step (4) is controlled to be 2.5-6 μm.
Further, in the step (5), the safety coefficient S is controlled to be 1.1-1.6.
The invention also provides a device for preparing the prestressed electrolytic copper foil, which is shown in figure 2. The device comprises an electrolyte preparation tank 18, an electrolytic tank 10, a screw transmission mechanism, a power supply 11, a frame 5 and accessories such as connection, support, sealing, insulation and the like.
The screw transmission mechanism comprises a motor 1, a coupler 2, a screw rod 3, a rolling bearing 4, an upper end nut pull head 6, a guide rod 19, a lower end fixing bolt 9, a nut 13, a displacement sensor and a tension sensor.
The lower end fixing bolt 9 is entirely coated or covered with insulating material and is connected with the ground wire 12; the whole outer part of the upper end nut pull head 6 (or the contact part with the cathode plate 7) is coated or covered with insulating materials; the whole outside of the fixing pieces at the upper end and the lower end of the cathode plate 7 is also coated or covered with insulating materials; the motor and the screw rod coupler 2 are insulated couplers.
The whole screw transmission stretching process should consider displacement deformation (deformation of a non-cathode plate) caused by fixing, connecting and insulating parts, and the accumulated deformation errors should be deducted when calculating the actual deformation of the cathode plate 7.
A servo motor, a motor driver, a displacement sensor, a tension sensor and a PLC controller are selected for configuration interface design, so that communication between an upper computer and a lower computer is realized, and automatic and accurate control of the whole system can be realized.
The bottom in the electrolyte preparation tank 18 is provided with a heating pipe 17, one side bottom of the electrolyte preparation tank 18 is provided with a liquid inlet pipe 16, the other end of the liquid inlet pipe 16 is communicated to the top of the electrolyte preparation tank 10, a circulating pump 14 is arranged between the electrolyte preparation tank 18 and the electrolyte preparation tank 10, the circulating pump 14 and the electrolyte preparation tank 10 are connected to one side bottom of the electrolyte preparation tank 10 through a liquid outlet pipe 15, and the circulating pump 14 and the electrolyte preparation tank 18 are communicated to the top of the electrolyte preparation tank 18 through the liquid outlet pipe 15.
The anode plate 8 and the cathode plate 7 in the electrolytic tank 10 are respectively connected with the anode and the cathode of the power supply 11.
Example 1:
the thickness of the initial deposition layer is controlled to be 3 mu m, and no load is applied to the cathode plate; the second deposition layer is controlled at 3 mu m, and a tensile load of 15KN is applied to the cathode plate; the thickness of the third deposition layer is controlled to be 3 mu m, and no load is applied to the cathode plate; the fourth deposition layer is controlled at 3 mu m, and a tensile load of 15KN is applied to the cathode plate; the fifth deposition layer was controlled to be 3 μm thick, and no load was applied to the cathode plate. In the above order, the one-time electrodeposition is completed. After the deposition is completed, the copper foil is stripped from the cathode plate, subjected to surface oxidation prevention treatment and dried.
Example 2:
the thickness of the initial deposition layer is controlled to be 3 mu m, and a 20KN tensile load is applied to the cathode plate; the second deposition layer is controlled at 3 mu m, and no load is applied to the cathode plate; the thickness of the third deposition layer is controlled to be 3 mu m, and a 20KN tensile load is applied to the cathode plate; the fourth deposition layer is controlled at 3 mu m, and no load is applied to the cathode plate; the thickness of the fifth deposition layer was controlled to 3 μm, and a tensile load of 20KN was applied to the cathode plate. In the above order, the one-time electrodeposition is completed. After the deposition is completed, the copper foil is stripped from the cathode plate, subjected to surface oxidation prevention treatment and dried.
Comparative example 1:
the cathode plate is not loaded, the thickness is 15 mu m, and the one-time electrodeposition is completed. After the deposition is completed, the copper foil is stripped from the cathode plate, subjected to surface oxidation prevention treatment and dried.
The results of the mechanical property tests of the three groups of samples are shown in Table 1. It can be found that the tensile strength of the examples 1 and 2 is obviously improved compared with that of the comparative example 1, and the room temperature tensile strength is respectively improved by 28.0 percent and 35.1 percent; the high-temperature tensile strength is respectively improved by 52.4 percent and 56.4 percent. The elongations of the examples 1 and 2 are obviously improved compared with the elongation of the comparative example 1, and the room-temperature elongations are respectively improved by 40.4 percent and 50.0 percent; the high-temperature elongation rate is respectively improved by 57.8 percent and 84.4 percent.
Table 1 three sets of sample mechanical properties index
Claims (7)
1. A method for preparing a prestressed electrolytic copper foil, characterized by: the method comprises the following steps:
step 1, preparing electrolyte: the preparation method is configured according to the existing production process of various electrolytic copper foils;
step 2, cathode plate installation: one end of the driving mechanism is fixed, and the other end of the driving mechanism is connected with the driving mechanism; or both ends are connected with the transmission mechanism; the transmission mechanism is used for applying single tensile stress, compressive stress or shear stress or a combination of the above stresses to the cathode plate;
step 3, debugging a transmission mechanism to ensure the working stability of the transmission mechanism, and observing the deformation of the cathode plate through a displacement sensor; finally filling electrolyte into the electrolytic tank;
step 4, preparing an initial electrodeposited layer; without applying a stress load to the cathode plate, i.e., the stress load f=0, an initial deposition layer of a certain thickness H is first prepared, and the electrodeposition time is calculated according to the following formula 1:
T＝7.544×10 -3 ηBLH/I equation 1
In equation 1: t is electrodeposition time, s; η is current efficiency,%; b is the width of the cathode plate, mm; l is the length of the cathode plate, and mm; h is the thickness of the copper foil, and mm; i is current intensity, A;
step 5, preparing a second electrodeposited layer; at this time, stress load f=f is applied to the cathode plate 1 Preparing a certain thickness H 1 The electrodeposition time is still calculated according to formula 1; the stress load F is calculated and controlled according to the following formula 2:
F≤Aσ e s formula 2
In equation 2: f is stress load, N; a is the cross-sectional area of the cathode plate, mm 2 ；σ e N/mm being the elastic or yield limit of the cathode plate material 2 The method comprises the steps of carrying out a first treatment on the surface of the S is a safety coefficient;
step 6, repeating the step 4 and the step 5, so that the electrolytic copper foil with certain gradient alternate distribution of internal stress with different properties in the thickness direction can be prepared;
step 4 and step 5 are not sequenced;
and 7, after the deposition is completed, stripping the electrolytic copper foil from the cathode plate and carrying out subsequent surface treatment.
2. The method for preparing a pre-stress electrolytic copper foil according to claim 1, wherein: the thickness of the cathode plate is not more than 1mm.
3. The method for preparing a pre-stress electrolytic copper foil according to claim 1, wherein: in the step 4, the thickness of the copper foil is controlled to be 2.5-6 mu m.
4. The method for preparing a pre-stress electrolytic copper foil according to claim 1, wherein: and in the step 5, the safety coefficient S is controlled to be 1.1-1.6.
5. An apparatus for preparing a pre-stress electrolytic copper foil for realizing the method for preparing a pre-stress electrolytic copper foil according to any one of claims 1 to 4, characterized in that: the device comprises an electrolyte preparation tank (18), an electrolytic tank (10), a screw transmission mechanism, a power supply (11), a frame (5) and connecting, supporting, sealing and insulating accessories;
the screw transmission mechanism comprises a motor (1), a coupler (2), a screw rod (3), a rolling bearing (4), an upper end nut pull head (6), a guide rod (19), a lower end bolt (9), a nut (13), a displacement sensor and a tension sensor;
the whole outer part of the lower end fixing bolt (9) is coated or covered with insulating materials and is connected with a ground wire (12); the whole outside of the upper end nut pull head (6) or the contact part with the cathode plate is coated or covered with insulating materials; the whole outer parts of the fixing pieces at the upper end and the lower end of the cathode plate (7) are coated or covered with insulating materials; the coupling (2) between the motor and the screw rod adopts an insulating coupling.
6. The apparatus for preparing a pre-stress electrolytic copper foil according to claim 5, wherein: the device also comprises a servo motor, a motor driver and a PLC controller, wherein the servo motor, the motor driver, the displacement sensor, the tension sensor and the PLC controller are selected for configuration interface design, so that the communication of an upper computer and a lower computer is realized, and the automatic accurate control of the whole system is realized.
7. The apparatus for preparing a pre-stress electrolytic copper foil according to claim 5, wherein: the utility model discloses a solar cell, including electrolyte preparation groove (18), electrolyte preparation groove (18) and electrolyte preparation groove, be equipped with heating pipe (17) in bottom in electrolyte preparation groove (18), one side bottom of electrolyte preparation groove (18) is provided with feed liquor pipe (16), the other end of feed liquor pipe (16) switches on to the top of electrolysis groove (10), be provided with circulating pump (14) between electrolysis groove (10) and electrolyte preparation groove (18), circulating pump (14) are connected to one side bottom of electrolysis groove (10) through drain pipe (15) with electrolysis groove (10), circulating pump (14) are switched on to the top of electrolyte preparation groove (18) through drain pipe (15).
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2022
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| KR20040047264A (en) * | 2002-11-29 | 2004-06-05 | 엘지전선 주식회사 | Low Roughness Copper Foil Manufacturing Method And Electropolishing Device Thereof And Copper Foil Thereof |
| CN108677225A (en) * | 2018-08-14 | 2018-10-19 | 山东金宝电子股份有限公司 | A kind of processing method reducing electrolytic copper foil warpage |
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