Production method of ultrathin ultrahigh double-sided light-resistant lithium battery copper foil

文档序号:1827488 发布日期:2021-11-12 浏览:35次 中文

阅读说明:本技术 一种超薄超高抗双面光锂电铜箔的生产方法 (Production method of ultrathin ultrahigh double-sided light-resistant lithium battery copper foil ) 是由 曹露 黄国平 江明 张中明 李瑞强 于 2021-07-06 设计创作,主要内容包括:本发明公开了一种超薄超高抗双面光锂电铜箔的生产方法,包括以下步骤:配置电解液进行哈林槽打片,每次1.5L,根据多种添加剂体系要求,添加相应的添加剂,电解液参数按照要求进行,电解液浓度为1-20ppm;哈林槽加液1.5L,添加剂按照浓度添加,充分搅拌均匀,电流26.5A,通电50s,控制槽压4.5-5.5V,电镀结束后-用纯水冲洗,然后用吹风机吹干;将铜箔从阴极板剥下,检测光泽度、抗拉强度,添加剂实验每批次实验结束后换液。本发明采用上述一种超薄超高抗双面光锂电铜箔的生产方法,同时提升了铜箔的常温抗拉强度及延伸率,工艺简单,6μm高抗铜箔外观无差异。(The invention discloses a production method of an ultrathin ultrahigh double-sided light-resistant lithium battery copper foil, which comprises the following steps: preparing electrolyte for harlin groove flaking, wherein 1.5L of electrolyte is added each time according to the requirements of various additive systems, corresponding additives are added according to the requirements, the electrolyte parameters are carried out according to the requirements, and the electrolyte concentration is 1-20 ppm; adding 1.5L of liquid into a Harlin tank, adding additives according to the concentration, fully and uniformly stirring, controlling the tank pressure to be 4.5-5.5V and electrifying for 50s under the current of 26.5A, washing with pure water after the electroplating is finished, and drying by using a blower; and peeling the copper foil from the negative plate, detecting the glossiness and the tensile strength, and changing the liquid after the experiment of each batch of the additive experiment is finished. The production method of the ultrathin ultrahigh double-sided light-resistant lithium battery copper foil is adopted, the normal-temperature tensile strength and the elongation of the copper foil are improved, the process is simple, and the 6-micron high-resistant copper foil has no difference in appearance.)

1. The production method of the ultrathin ultrahigh double-sided light-resistant lithium battery copper foil is characterized by comprising the following steps of:

(1) preparing electrolyte for harlin groove flaking, wherein 1.5L of electrolyte is added each time according to the requirements of various additive systems, corresponding additives are added according to the requirements, the electrolyte parameters are carried out according to the requirements, and the electrolyte concentration is 1-20 ppm;

(2) adding 1.5L of liquid into a Harlin tank, adding additives according to the concentration, fully and uniformly stirring, controlling the tank pressure to be 4.5-5.5V and electrifying for 50s under the current of 26.5A, washing with pure water after the electroplating is finished, and drying by using a blower;

(3) and peeling the copper foil from the negative plate, detecting the glossiness and the tensile strength, and changing the liquid after the experiment of each batch of the additive experiment is finished.

2. The production method of the ultra-thin ultra-high anti-double-sided photo-lithium electro-copper foil according to claim 1, characterized in that: the electrolyte parameter in the step (1) is H2SO4Has a concentration of 100-2+Has a concentration of 90-95g/L and Cl-The concentration of the electrolyte is 20-30mg/L, and the temperature of the electrolyte is 46-50 ℃.

3. The production method of the ultra-thin ultra-high anti-double-sided photo-lithium electro-copper foil according to claim 1, characterized in that: the additive is a mixture of four types, namely a leveling agent (HC-1), a grain refiner (HC-2), a dispersant (HC-3) and a tensile agent (HC-4).

4. The production method of the ultra-thin ultra-high anti-double-sided photo-lithium electro-copper foil according to claim 3, characterized in that: the leveling agent is one or the combination of two of collagen and gelatin.

5. The production method of the ultra-thin ultra-high anti-double-sided photo-lithium electro-copper foil according to claim 3, characterized in that: the grain refiner is one or two of sodium thiolpropanate and N, N-dimethyl dithioformamide propane sulfonate.

6. The production method of the ultra-thin ultra-high anti-double-sided photo-lithium electro-copper foil according to claim 3, characterized in that: the dispersing agent is one or two of tetrahydroxypropyl ethylenediamine and alkyl glycoside.

7. The production method of the ultra-thin ultra-high anti-double-sided photo-lithium electro-copper foil according to claim 3, characterized in that: the tensile agent is one or two of ethylene thiourea and thiazolinyl dithio propane sodium sulfonate.

Technical Field

The invention relates to the technical field of new energy batteries, in particular to a production method of an ultrathin ultrahigh double-sided light-resistant lithium battery copper foil.

Background

With the development of new energy battery industry, in order to meet the development of power batteries and digital batteries, especially the demand of digital customers for ultrathin and ultrahigh-resistance products is gradually increased. The tensile strength of the conventional 6 μm copper foil is 30-40kgf/mm2The tensile strength of the copper foil is increased, and the elongation is reduced. Therefore, the tensile strength and the elongation of the copper foil are improved simultaneously, the battery is not easy to break in the thermal expansion process, and the capacity and the safety of the battery are improved.

Disclosure of Invention

The invention aims to provide a production method of an ultrathin ultrahigh double-sided photo-lithium battery copper foil, which improves the normal-temperature tensile strength and the elongation of the copper foil, is simple in process and has no difference in the appearance of a 6-micron high-resistance copper foil.

In order to achieve the purpose, the invention provides a production method of an ultrathin ultrahigh double-sided light-resistant lithium battery copper foil, which comprises the following steps:

(1) preparing electrolyte for harlin groove flaking, wherein 1.5L of electrolyte is added each time according to the requirements of various additive systems, corresponding additives are added according to the requirements, the electrolyte parameters are carried out according to the requirements, and the electrolyte concentration is 1-20 ppm;

(2) adding 1.5L of liquid into a Harlin tank, adding additives according to the concentration, fully and uniformly stirring, controlling the tank pressure to be 4.5-5.5V and electrifying for 50s under the current of 26.5A, washing with pure water after the electroplating is finished, and drying by using a blower;

(3) and peeling the copper foil from the negative plate, detecting the glossiness and the tensile strength, and changing the liquid after the experiment of each batch of the additive experiment is finished.

Preferably, the electrolyte parameter in the step (1) is H2SO4Has a concentration of 100-2+Has a concentration of 90-95g/L and Cl-The concentration of the electrolyte is 20-30mg/L, and the temperature of the electrolyte is 46-50 ℃.

Preferably, the additive is a mixture of four of leveling agent (HC-1), grain refiner (HC-2), dispersant (HC-3) and tensile agent (HC-4).

Preferably, the leveling agent is one or two of collagen and gelatin.

Preferably, the grain refiner is one or two of sodium thiolpropanate and sodium N, N-dimethyl-dithioformamide propane sulfonate.

Preferably, the dispersing agent is one or two of tetrahydroxypropyl ethylenediamine and alkyl glycoside.

Preferably, the tensile agent is one or two of ethylene thiourea and thiazolinyl dithio propane sodium sulfonate.

Therefore, the production method of the ultrathin ultrahigh double-sided light lithium battery copper foil is adopted, the normal-temperature tensile strength and the elongation of the copper foil are improved, the process is simple, and the 6-micron high-resistance copper foil has no difference in appearance.

The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.

Drawings

FIG. 1 is a single-value control diagram of the room-temperature tensile strength of the invention;

FIG. 2 is a single value control chart of the baking tensile strength of the present invention;

FIG. 3 is a single value control chart of the baking elongation of the present invention;

FIG. 4 is an optical microscope image of the production of a 6 μm high-resistance copper foil system of the present invention, wherein a is an optical microscope X100 (matte surface) and b is an optical microscope X400 (matte surface);

FIG. 5 is an optical microscope image of a 6 μm ordinary copper foil system according to the present invention, wherein a is an optical microscope X100 (matte surface) and b is an optical microscope X400 (matte surface);

FIG. 6 is a drawing of an optical microscope for manufacturing a 6 μm high-resistance copper foil system according to the present invention, wherein a is an optical microscope X100 (smooth surface) and b is an optical microscope X400 (smooth surface);

FIG. 7 is a drawing of an optical microscope for producing a 6 μm ordinary copper foil system of the present invention, wherein a is an optical microscope X100 (plain surface) and b is an optical microscope X400 (plain surface);

FIG. 8 is an SEM electron microscope photograph of a 6 μm high-resistance copper foil system of the present invention, wherein a is SEM (matte surface) and b is SEM (smooth surface).

Detailed Description

The invention provides a production method of an ultrathin ultrahigh double-sided light-resistant lithium battery copper foil, which comprises the following steps:

(1) preparing electrolyte for Harlin groove flaking with 1.5L each time, adding corresponding additives according to the requirements of various additive systems, wherein the additives are four mixtures of leveling agent (HC-1), grain refiner (HC-2), dispersant (HC-3) and tensile agent (HC-4), the electrolyte parameters are carried out according to the requirements, the concentration of the additives in the electrolyte is 1-20ppm, and the electrolyte parameter H is2SO4Has a concentration of 100-2+Has a concentration of 90-95g/L and Cl-The concentration of the copper foil is 20-30mg/L, the temperature of the electrolyte is 46-50 ℃, the concentration of sulfuric acid and copper ions is mainly used for keeping the stability in the production process, the appearance of the copper foil surface is influenced by insufficient content of the copper ions, the concentration is a relative value, the range can be changed up and down, and the adjustment of a matching process is needed. The chloride ions can perform a systematic action with other additives to enhance polarization, so that the copper foil is bright, and the internal structure and physical properties of the copper foil are affected by too high or too low of the copper foil. The increased temperature accelerates the migration of ions, the decreased temperature affects the moving speed of ions, the over-high temperature shortens the service life of the production pipeline, and the oxidation speed of the cathode is accelerated.

(2) Adding 1.5L of liquid into a Harlin tank, adding additives according to the concentration, fully and uniformly stirring, controlling the tank pressure to be 4.5-5.5V and electrifying for 50s under the current of 26.5A, washing with pure water after the electroplating is finished, and drying by using a blower;

(3) and peeling the copper foil from the negative plate, detecting the glossiness and the tensile strength, and changing the liquid after the experiment of each batch of the additive experiment is finished.

Further, the leveling agent is one or two of collagen and gelatin. The grain refiner is one or two of sodium thiolpropanate and N, N-dimethyl dithioformamide propane sulfonate. The dispersing agent is one or two of tetrahydroxypropyl ethylenediamine and alkyl glycoside. The tensile agent is one or two of ethylene thiourea and thiazolinyl dithio propane sodium sulfonate.

The reaction mechanism is as follows: the leveling agent, the grain refiner, the dispersant and the tensile agent are matched with each other, the grain refiner promotes the generation of copper foil crystal nucleus and the growth of crystal grain, the more the crystal nucleus is, the finer the crystal grain is in the production process; the dispersing agent promotes the uniform dispersion of copper ions, reduces the surface tension of the cathode and promotes the deposition; the leveling agent inhibits continuous production of copper foil in the copper deposition process, prevents continuous growth of crystal grains, enables the copper foil to be flat, and the tensile agent is used for enabling the leveling agent, the crystal grains and the crystal nucleus to be compatible, so that the crystal grains of the copper foil are fine, flat and mutually interwoven, the tensile strength is improved, and the elongation is increased.

The technical solution of the present invention is further illustrated by the accompanying drawings and examples.

Example 1

The additive system HC-1 selects collagen, the electrolyte concentration is 10 ppm; HC-2 adopts sodium thiolpropanate, and the concentration of the electrolyte is 3 ppm; HC-3 adopts tetrahydroxypropyl ethylenediamine, and the concentration of the electrolyte is 15 ppm; HC-4 adopts ethylene thiourea, and the concentration of the electrolyte is 2 ppm.

A sheet making test is carried out according to the additive system, and the physical properties of the copper foil are detected, wherein the specific properties are shown in Table 1:

TABLE 1

Example 2

The additive system HC-1 is gelatin, and the concentration of the electrolyte is 10 ppm; HC-2 adopts N, N-dimethyl dithio formamide propane sodium sulfonate, the concentration of electrolyte is 3 ppm; HC-3 is alkyl glycoside, the concentration of electrolyte is 1.5 ppm; HC-4 is thiazolinyl dithio propane sodium sulfonate, and electrolyte concentration is 20 ppm.

And (3) carrying out a flaking test according to the additive system, and detecting the physical properties of the copper foil, wherein the specific properties are shown in the table 2:

TABLE 2

Example 3

The additive system HC-1 adopts gelatin and collagen, the concentration ratio of the gelatin to the collagen is 1:1, and the concentration of the electrolyte is 10 ppm; HC-2 adopts N, N-dimethyl dithio formamide propane sodium sulfonate and alcohol sulfenyl propane sodium sulfonate, the concentration ratio of the two is 1:1, and the concentration of the electrolyte is 3 ppm; HC-3 adopts tetrahydroxypropyl ethylenediamine, and the concentration of the electrolyte is 15 ppm; HC-4 adopts ethylene thiourea and thiazolinyl dithio propane sodium sulfonate, the concentration ratio of the ethylene thiourea to the thiazolinyl dithio propane sodium sulfonate is 2:8, and the concentration of the electrolyte is 20 ppm.

According to the laboratory lab condition, the additive is determined to be compounded, the tensile strength and the elongation percentage of the copper foil are improved, the sheet making test is carried out according to the additive system, and the physical properties of the copper foil are detected, wherein the specific properties are shown in the table 3:

TABLE 3

Example 4

According to the results of the pilot plant, the additive system is determined and then the single regenerated foil system is used for production, and the electrolyte, the additive concentration and the production process parameters are shown in the table 4:

TABLE 4

The additive system HC-1 is gelatin and collagen with concentration ratio of 1:1 and electrolyte concentration of 5-10 ppm; HC-2 adopts N, N-dimethyl dithio formamide propane sodium sulfonate and alcohol sulfenyl propane sodium sulfonate, the concentration ratio of the two is 1:1, and the concentration of the electrolyte is 1-3 ppm; HC-3 adopts tetrahydroxypropyl ethylenediamine, and the concentration of the electrolyte is 10-15 ppm; HC-4 adopts ethylene thiourea and thiazolinyl dithio propane sodium sulfonate, the concentration ratio of the ethylene thiourea to the thiazolinyl dithio propane sodium sulfonate is 2:8, and the concentration of the electrolyte is 10-20 ppm.

The above test was carried out normally according to the above parameters, and the physical properties of the produced copper foil are shown in FIGS. 1 to 8 and Table 5:

TABLE 5

As can be seen from the figures 1-8, the surface condition of the copper foil is observed under an optical microscope and an SEM electron microscope, the microscopic grains of the copper foil with the copper foil grains are refined under the action of the additive system, the grains are obvious, the leveling effect of the thin surface is good, and no obvious bulge exists.

In summary, it can be seen from the above examples and test results that the tensile strength at room temperature of > 70kgf/mm is produced by the 6 μm high-resistance copper foil system adjusted by the additive process2Tensile strength at baking > 47kgf/mm2The baking elongation is more than 7 percent; the foil surface produced by the 6 mu m high-resistance copper foil is consistent with the existing copper foil, and the appearance of the copper foil is not different.

Therefore, the production method of the ultrathin ultrahigh double-sided light lithium battery copper foil is adopted, the normal-temperature tensile strength and the elongation of the copper foil are improved, the process is simple, and the 6-micron high-resistance copper foil has no difference in appearance.

Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.

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