阅读说明：本技术 反转铜箔生产工艺 (Production process of reverse copper foil ) 是由 万新领 高元亨 何宏杨 罗志艺 于 2020-05-15 设计创作，主要内容包括：本发明涉及一种反转铜箔生产工艺,属于电解铜箔技术领域,工艺过程包括电解生箔及表面处理,所述表面处理包括：微蚀→酸洗→粗化→水洗→固化→水洗→粗化→水洗→固化→水洗→表面合金化处理→水洗→表面抗氧化处理→水洗→钝化→在毛面上涂覆抗粘膜→硅烷化处理→干燥,所述涂覆抗粘膜中各组分的组成以及含量为,有机氯硅烷35.5～46wt％、机聚硅氧烷树脂27.8～33wt％、氨基硅烷12.7～20.1wt％、聚酯树脂10.2～12.2wt％、酸性白土催化剂2～8.2wt％,所述涂覆抗粘膜的厚度为3μm。采用本发明生产工艺。可以在减少铜箔表面的残铜率同时,保证铜箔表面与蚀刻阻剂的结合力,并且保证铜箔的延伸率。(The invention relates to a production process of a reverse copper foil, belonging to the technical field of electrolytic copper foil, wherein the process comprises electrolytic foil generation and surface treatment, and the surface treatment comprises the following steps: micro-etching → acid cleaning → coarsening → water cleaning → solidification → water cleaning → coarsening → water cleaning → surface alloying treatment → water cleaning → surface antioxidation treatment → water cleaning → passivation → coating anti-adhesive film on the hair surface → silanization treatment → drying, wherein the composition and content of each component in the coating anti-adhesive film are 35.5-46 wt% of organic chlorosilane, 27.8-33 wt% of organopolysiloxane resin, 12.7-20.1 wt% of amino silane, 10.2-12.2 wt% of polyester resin and 2-8.2 wt% of acid clay catalyst, and the thickness of the coating anti-adhesive film is 3 μm. The production process is adopted. The residual copper rate on the surface of the copper foil can be reduced, the binding force between the surface of the copper foil and the etching resistance agent is ensured, and the elongation of the copper foil is ensured.)

1. The production process of the reverse copper foil comprises electrolytic foil generation and surface treatment, and is characterized in that the surface treatment comprises the following steps: micro-etching → acid cleaning → coarsening → water cleaning → solidification → water cleaning → coarsening → water cleaning → surface alloying treatment → water cleaning → surface antioxidation treatment → water cleaning → passivation → coating anti-adhesive film on the hair surface → silanization treatment → drying, wherein the composition and content of each component in the coating anti-adhesive film are 35.5-46 wt% of organic chlorosilane, 27.8-33 wt% of organopolysiloxane resin, 12.7-20.1 wt% of amino silane, 10.2-12.2 wt% of polyester resin and 2-8.2 wt% of acid clay catalyst, and the thickness of the coating anti-adhesive film is 3 μm.

2. The process for producing an inverted copper foil according to claim 1, wherein in said anti-sticking film coating process, the smooth surface of the inverted copper foil is first adhered with an adhesive tape and covered over the entire surface thereof, and then H is used₂SO₄Pickling the matte side of the inverse copper foil, followed by the anti-adhesive coating, H₂SO₄The concentration of the acid is 70-90 g/L, and the concentration of the acid is 20-50 g/L H before the acid washing process₂SO₄Soaking the solution for 0.5h, and then keeping the solution for 0.5h under the condition that the humidity is 35-45% RH.

3. The process for producing an inverted copper foil according to claim 2, wherein the coated inverted copper foil is left at 20 ℃ and 60% RH for 0.5 hour, and after attaching a rubber film having a thickness of 0.4mm to the matte side coated with the anti-adhesion film, the coated side is made to face up, and then the inverted copper foil is pressed with a circular roller and held at a high temperature of 60 ℃ for 0.5 hour, and then at 20 ℃ for 0.5 hour, and then the rubber film is removed.

4. The process for producing a reversed copper foil according to claim 3, wherein the load of the round drum is 15g/cm²And the thickness of the cylinder wall of the circular roller is 0.2 mm.

5. The process for producing an inverse copper foil according to claim 4, wherein the roughening is carried out under Cu condition²⁺10～23g/L，H₂SO₄100～130g/L，Mg²⁺1.5～3g/L，Cl^-10×10^-6，Mg²⁺Current density D of 1.5-3 g/L_k30 to 50A/dm2, the electroplating time t 5 to 10s, and the additive is L u₂O₃7～10g/L，NiSO₄1-5 g/L, and carrying out anti-oxidation treatment, wherein the technological condition of curing is that Cu²⁺20～30g/L，H₂SO₄50～70g/L，Cl^-10×10^-6(ii) a Current density D_k10 to 20A/dm2, and the electroplating time t 5 to 10 s.

6. The process for producing a reverse copper foil according to claim 5, wherein the surface alloying treatment is performed by electroplating with an electrogalvanizing nickel-cobalt alloy under a condition of NiSO₄·6H₂O 13～20g/L，ZnSO₄·7H₂O 10～14g/L，CoSO₄·7H₂O5-7 g/L, complexing agent 100-120 g/L and additive L u₂O₃7～10g/L，NiSO₄1-5 g/L, electroplating temperature of 50-60 ℃, pH of 7-11, and current density D_k5～6A/dm²The electroplating time is t 5-10 s, and the passivation process condition is Cr³⁺3 to 5 g/L10 to 20 g/L2 to 4 g/L, and a current density D_k2～5A/dm²And the electroplating time is t 5-10 s.

7. The process for producing an inverse copper foil according to claim 6, wherein the drying temperature is 100 to 150 ℃.

Technical Field

The invention belongs to the technical field of electrolytic copper foil, and particularly relates to a production process of a reverse copper foil.

Background

The electrolytic copper foil is a new copper processing product, and the electrolytic copper foil is more and more important in the electronic material industry in the high-speed development of the current electronic information industry, the electrolytic copper foil is called a 'neural network' for signal and power transmission and communication of electronic products, the electrolytic copper foil is convenient to be adhered to the surfaces of other materials besides the high conductivity, high thermal conductivity, certain mechanical strength and beautiful metallic luster of the copper foil produced by other methods.

However, some problems of the product are gradually highlighted in the production and processing process, some reversed copper foil plates are rough in surface, residual glue is easy to remain after dry film development, residual copper is easy to generate after etching, and the problem of residual copper is a common problem in the plate processing process.

Disclosure of Invention

In view of the above, the present application provides a process for producing an inverse copper foil, which can reduce the residual copper rate on the surface of the copper foil, ensure the adhesion between the surface of the copper foil and the etching resist, and ensure the elongation of the copper foil by coating an anti-sticking film on the rough surface of the inverse copper foil.

In order to achieve the purpose, the invention provides the following technical scheme:

the invention relates to a production process of a reverse copper foil, which comprises electrolytic foil generation and surface treatment, wherein the surface treatment comprises the following steps: micro-etching → acid cleaning → coarsening → water cleaning → solidification → water cleaning → coarsening → water cleaning → surface alloying treatment → water cleaning → surface antioxidation treatment → water cleaning → passivation → coating anti-adhesive film on the hair surface → silanization treatment → drying, wherein the composition and content of each component in the coating anti-adhesive film are 35.5-46 wt% of organic chlorosilane, 27.8-33 wt% of organopolysiloxane resin, 12.7-20.1 wt% of amino silane, 10.2-12.2 wt% of polyester resin and 2-8.2 wt% of acid clay catalyst, and the thickness of the coating anti-adhesive film is 3 μm.

Further, in the anti-adhesive film coating process, the smooth surface of the reversed copper foil is first attached with an adhesive tape and covered over the entire surface thereof, and then H is used₂SO₄Pickling the matte side of the inverse copper foil, followed by the anti-adhesive coating, H₂SO₄The concentration of the acid is 70-90 g/L, and the concentration of the acid is 20-50 g/L H before the acid washing process₂SO₄Soaking the solution for 0.5h, and then keeping the solution for 0.5h under the condition that the humidity is 35-45% RH.

Further, the coated reversed copper foil was placed at 20 ℃ and 60% RH for 0.5 hour, attached to the matte side coated with the anti-adhesive film with a rubber film of 0.4mm thickness such that the coated side was facing upward, and then pressed with a circular roller at a high temperature of 60 ℃ for 0.5 hour, further at 20 ℃ for 0.5 hour, and then removed.

Further, the load of the round roller is 15g/cm²And the thickness of the cylinder wall of the circular roller is 0.2 mm.

Further, the coarsening process condition is that Cu²⁺10～23g/L，H₂SO₄100～130g/L，Mg²⁺1.5～3g/L，Cl^-10×10^-6，Mg²⁺Current density D of 1.5-3 g/L_k30 to 50A/dm2, the electroplating time t 5 to 10s, and the additive is L u₂O₃7～10g/L，NiSO₄1-5 g/L, and carrying out anti-oxidation treatment, wherein the technological condition of curing is that Cu²⁺20～30g/L，H₂SO₄50～70g/L，Cl^-10×10^-6(ii) a Current density D_k10 to 20A/dm2, and the electroplating time t 5 to 10 s.

Further, the surface alloying treatment adopts the electrogalvanizing nickel-cobalt alloy, and the process condition of the electrogalvanizing nickel-cobalt alloy is that NiSO₄·6H₂O 13～20g/L，ZnSO₄·7H₂O 10～14g/L，CoSO₄·7H₂O5-7 g/L, complexing agent 100-120 g/L and additive L u₂O₃7～10g/L，NiSO₄1-5 g/L, electroplating temperature of 50-60 ℃, pH of 7-11, and current density D_k5～6A/dm²The electroplating time is t 5-10 s, and the passivation process condition is Cr³⁺3 to 5 g/L10 to 20 g/L2 to 4 g/L, and a current density D_k2～5A/dm²And the electroplating time is t 5-10 s.

Further, the drying temperature is 100-150 ℃.

The invention has the beneficial effects that: according to the invention, the anti-adhesive film is coated on the rough surface of the reversed copper foil, so that the ridges on the rough surface can be reduced, the line width and the line distance can be reduced, but the ridges on the rough surface cannot be completely removed, and the bonding force between the surface of the copper foil and the etching resistance agent cannot be changed greatly. According to the production process, the anti-adhesive film is coated, so that the combination of the rough surface and the etching resisting agent is changed into the combination of the anti-adhesive film and the etching resisting agent, the combination force is more stable compared with the direct combination of the rough surface, the residual copper rate on the surface of the copper foil can be reduced, the combination force between the surface of the copper foil and the etching resisting agent is ensured, and the elongation of the copper foil is ensured.

The process method of the invention increases the copper foil size by oxidizing and then coating, and after the copper foil is oxidized, the rough surface of the copper foil forms tiny copper oxide micro crystalsThe surface area is increased, so that the bonding strength between the anti-adhesive film and the copper foil is higher, and the risk of falling off of the anti-adhesive film is reduced, by adding L u₂O₃And NiSO₄And the additives are co-precipitated with copper ions in the deposition process to form more active particles and inhibit the formation of dendritic crystals, so that an ideal deposition layer is obtained, and the bonding strength between crystal grains is improved. The coarsening process is carried out under the condition of relatively large current, the second coarsening treatment is to form a fine coarsening layer on the closed surface, the coarsening layer is firmly combined with the closed layer to obtain relatively ideal combination force, and the structural surface of the structure becomes more stable through curing treatment.

Drawings

For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:

FIG. 1 is a process flow diagram of example 2 of the present invention.

Detailed Description

The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and examples may be combined with each other without conflict.

Wherein the showings are for the purpose of illustrating the invention only and not for the purpose of limiting the same, and in which there is shown by way of illustration only and not in the drawings in which there is no intention to limit the invention thereto; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.

The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by terms such as "upper", "lower", "left", "right", "front", "rear", etc., based on the orientation or positional relationship shown in the drawings, it is only for convenience of description and simplification of description, but it is not an indication or suggestion that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes, and are not to be construed as limiting the present invention, and the specific meaning of the terms may be understood by those skilled in the art according to specific situations.