CN112921371A - Surface roughening and curing treatment method of RTF copper foil for high-frequency copper-clad plate - Google Patents
Surface roughening and curing treatment method of RTF copper foil for high-frequency copper-clad plate Download PDFInfo
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- CN112921371A CN112921371A CN202110081063.4A CN202110081063A CN112921371A CN 112921371 A CN112921371 A CN 112921371A CN 202110081063 A CN202110081063 A CN 202110081063A CN 112921371 A CN112921371 A CN 112921371A
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/16—Electroplating with layers of varying thickness
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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
- C25D7/0692—Regulating the thickness of the coating
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Abstract
The invention relates to a surface roughening and curing treatment method of an RTF copper foil for a high-frequency copper-clad plate, which comprises the following steps: step A, acid washing pretreatment; step B, primary coarsening electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 1: 2-5: 1, and the current density is ensured to be 20A-100A/dm2(ii) a Step C, primary weak solidification electroplating; step D, repeating B, C steps for 2-5 times; step E, primary curing electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 3: 1-10: 1, and the current density is ensured to be 20A-50A/dm2. The crystal grains of the plating layer are refined, the surface is fine,the oxidation resistance and the corrosion resistance of the copper foil are improved.
Description
Technical Field
The invention relates to the technical field of electrolytic copper foil production, in particular to a surface roughening and curing treatment method of an RTF copper foil for a high-frequency copper-clad plate.
Background
At present, the surface treatment process of copper foil adopted by various copper foil production enterprises at home and abroad can be generally summarized as follows: raw foil-pretreatment-coarsening treatment-solidification (heat-resistant barrier layer) treatment-anti-oxidation treatment-surface treatment.
The coarsening and curing treatment is a process of plating a thin layer of copper and oxide on the surface of the copper foil, and a layer of copper crystal is formed on the surface of copper grains formed by coarsening the surface of the copper foil under the control of different copper ion concentrations and different direct current densities, so that the peel strength of the copper foil on a base material can be enhanced.
As shown in fig. 1, the copper foil is subjected to 2000 × electron microscope scanning after the conventional roughening and curing treatment.
When domestic enterprises carry out surface treatment on the electrolytic copper foil, the coarsening layer mainly adopts a direct copper electroplating method. By adopting a common surface roughening copper plating process, the environment is affected by adding the additive, and the bonding force between the copper foil without the additive and the base material is insufficient, so that the problem of circuit breaking of the subsequent PCB is caused. The copper foil adopts the traditional roughening and curing treatment process, and the obtained surface electron microscope scanning image of the copper foil is shown as figure 1, and the plating layer of the copper foil is rough and the crystal grains are roughened.
In addition, in order to improve the peeling strength, the current is increased in the conventional arsenic-free roughening process, so that copper powder is easy to fall off during process control to cause short circuit of a PCB (printed Circuit Board), and therefore, the research on the surface roughening treatment process of the electrolytic copper foil is of great significance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method overcomes the defects of the prior art, provides a surface roughening and curing treatment method of the RTF copper foil for the high-frequency copper-clad plate, and solves the problems of insufficient surface bonding force and weak peeling strength of the copper foil caused by the adoption of the existing electroplating method.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the surface roughening and curing treatment method of the RTF copper foil for the high-frequency copper-clad plate comprises the following steps:
step A, acid washing pretreatment: washing an oxide layer on the surface of the original foil of the electrolytic copper foil to be treated by a pickling tank;
step B, primary coarsening electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 1: 2-5: 1, and the current density is ensured to be 20A-100A/dm2；
Step C, primary weak solidification electroplating: the current density of the original foil electroplated in the electrolytic bath is 20A-50A/dm2；
Step D, repeating B, C steps for 2-5 times;
step E, primary curing electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 3: 1-10: 1, and the current density is ensured to be 20A-50A/dm2。
Furthermore, the thickness of the original foil of the electrolytic copper foil is 0.012-0.070 mm.
Furthermore, Rz of the original foil of the electrolytic copper foil is less than or equal to 5 mu m, and Ra of the smooth surface is less than or equal to 0.4 mu m.
Further, in the step B and the step E, when pulse copper electroplating is carried out, the pulse width and the pulse interval of the pulse are 2-10 ms, the temperature is 25-45 ℃, and the voltage is 5-20V.
Further, in the step B, the roughening plating liquid used comprises: cu2+：10～20g/L，H2SO4: 100-200 g/L and 0.1-1 g/L of coarsening additive;
in step E, the curing of the plating bath composition comprises: cu2+：40～60g/L，H2SO4：100～200g/L，Cl-：5～20mg/L。
Furthermore, when pulse electrolytic copper plating is carried out, the anode plate is covered by a filter screen.
The invention has the beneficial effects that:
the invention provides a surface roughening and curing treatment method of an RTF copper foil, which utilizes pulse plating to periodically transmit power in a forward direction and a reverse direction, forms a roughened surface on the surface of the copper foil, but the roughness is still lower, and ensures good bonding force between the copper foil and a high-speed high-frequency copper-clad plate substrate while pursuing the surface roughness to be reduced as much as possible. Compared with common electroplating, the method has the advantages of smooth and compact plating layer, good adhesiveness, high current efficiency, good environmental protection performance and the like, and creates conditions for the continuous development of the industry. The invention is only improved on the aspects of direct current power supply equipment and an anode plate, is convenient and feasible for the reconstruction of the prior old process, does not need to add an additional process, and does not need to carry out any large process route reconstruction.
The method meets the current environmental protection requirements (no toxicity, harmlessness and sustainable development), finds a method for electroplating by a pulse power supply, refines the crystal grains of a plating layer by adjusting the forward-reverse time ratio, has a delicate surface, improves the oxidation resistance and corrosion resistance of the copper foil, can clean copper powder attached to a conductive roller during reverse electroplating, reduces the surface defects of the copper foil, improves the surface quality of a product, improves the labor efficiency, and creates conditions for the continuous development of the industry.
The invention only modifies equipment such as a rectification power supply, is convenient and feasible for modifying the prior old process, does not need to add an additional process, and does not need to modify any large process route.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a 2000X scanning electron microscope image of a copper foil after a conventional roughening and curing treatment;
FIG. 2 is a 2000X electron microscope scanning image of the copper foil after roughening and curing treatment in case I;
FIG. 3 is a 2000X electron microscope scanning image of the copper foil after roughening and curing treatment in case II;
FIG. 4 is a 1000X scanning electron microscope image of the copper foil after roughening and curing treatment in case III;
Detailed Description
The invention will now be further described with reference to specific examples. These drawings are simplified schematic diagrams only illustrating the basic structure of the present invention in a schematic manner, and thus show only the constitution related to the present invention.
A surface roughening and curing treatment method of RTF copper foil for a high-frequency copper-clad plate comprises the following steps:
step A, acid washing pretreatment: washing an oxide layer on the surface of the original foil of the electrolytic copper foil to be treated by a pickling tank;
step B, primary coarsening electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 1: 2-5: 1, and the current density is ensured to be 20A-100A/dm2；
Step C, primary weak solidification electroplating: the current density of the original foil electroplated in the electrolytic bath is 20A-50A/dm2；
Step D, repeating B, C steps for 2-5 times;
step E, primary curing electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 3: 1-10: 1, and the current density is ensured to be 20A-50A/dm2。
Specifically, in the embodiment, the thickness of the original foil of the electrolytic copper foil is 0.012-0.070 mm.
Specifically, in this embodiment, Rz of the raw electrolytic copper foil is not more than 5 μm, and Ra of the polished surface is not more than 0.4 μm.
In the embodiment, in the step B and the step E, when the pulse copper electroplating is performed, the pulse width and the pulse interval of the pulse are 2 to 10ms, the temperature is 25 to 45 ℃, and the voltage is 5 to 20V.
Specifically, in this example, the roughening plating liquid used in step B includes: cu2+：10～20g/L，H2SO4: 100-200 g/L and coarsening additive; the coarsening additive may be tungstate or carbonate.
In step E, the curing of the plating bath composition comprises: cu2+：40～60g/L，H2SO4：100～200g/L，Cl-：5～20mg/L。
Specifically, in this embodiment, the anode plate is covered with a filter screen during the pulse copper electroplating.
The surface roughening and curing treatment method of the RTF copper foil for the high-frequency copper-clad plate, disclosed by the invention, has the advantages that the crystal grains of the plating layer are refined and the surface is fine by adjusting the forward-reverse time ratio, and the oxidation resistance and the corrosion resistance of the copper foil are improved.
The following three cases are listed for comparison with the copper foil prepared by the conventional method
Case one
A surface roughening and curing treatment method of RTF copper foil for a high-frequency copper-clad plate comprises the following steps:
step A, acid washing pretreatment;
step B, primary coarsening electroplating: electroplating by pulse electroplating with forward/reverse time ratio of 1:2 and current density of 20A/dm2；
Step C, primary weak solidification electroplating: the current density of the original foil electroplated in the electrolytic bath is 30A/dm2；
Step D, B, C is repeated for 2 times;
step E, primary curing electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 3:1, and the current density is ensured to be 50A/dm2。
In the step B and the step E, when pulse copper electroplating is carried out, the pulse width and the pulse interval of the pulse are 10ms, the temperature is 35 ℃, and the voltage is 5V;
in step B, the roughening plating solution used comprises: cu2+：10g/L，H2SO4: 100g/L and coarsening additive 0.1 g/L; the coarsening additive may be selected from tungstate or molybdate.
In step E, the curing of the plating bath composition comprises: cu2+：40g/L，H2SO4：100g/L，Cl-：5mg/L。
The copper foil treated by the surface roughening and curing treatment method of the first case is shown in fig. 2, and is opposite to fig. 1, so that the copper foil is flat and compact in plating layer, fine in grain and fine in surface through the roughening and curing treatment method of the first case.
Case two
A surface roughening and curing treatment method of RTF copper foil for a high-frequency copper-clad plate comprises the following steps:
step A, acid washing pretreatment;
step B, primary coarsening electroplating: use ofElectroplating by pulse electroplating method with forward/reverse time ratio of 2:1 and current density of 50A/dm2；
Step C, primary weak solidification electroplating: electroplating the original foil in an electrolytic bath at 20A/dm2；
Step D, repeating B, C step 3 times;
step E, primary curing electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 5:1, and the current density is ensured to be 20A/dm2。
In the step B and the step E, when pulse copper electroplating is carried out, the pulse width and the pulse interval of the pulse are 5ms, the temperature is 45 ℃, and the voltage is 10V;
in step B, the roughening plating solution used comprises: cu2+：15g/L，H2SO4: 150g/L and coarsening additive 0.5 g/L; the coarsening additive may be selected from tungstate or molybdate.
In step E, the curing of the plating bath composition comprises: cu2+：50g/L，H2SO4：150g/L，Cl-：10mg/L。
The copper foil treated by the surface roughening and curing treatment method of case two is shown in fig. 3, and is opposite to fig. 1, and it can be seen that the plating layer of the copper foil is flat and compact, the crystal grains are refined, and the surface is fine by the roughening and curing treatment method of case two.
Case three
A surface roughening and curing treatment method of RTF copper foil for a high-frequency copper-clad plate comprises the following steps:
step A, acid washing pretreatment;
step B, primary coarsening electroplating: electroplating by pulse electroplating with forward/reverse time ratio of 5:1 and current density of 100A/dm2；
Step C, primary weak solidification electroplating: electroplating the raw foil in an electrolytic bath at 50A/dm2；
Step D, repeating B, C step 3 times;
step E, primary curing electroplating: the original foil is arranged onIn the coarsening electrolytic tank, electroplating is carried out by using a pulse electroplating method, the forward-reverse time ratio of the pulse electroplating is 10:1, and the current density is ensured to be 40A/dm2。
In the step B and the step E, when pulse copper electroplating is carried out, the pulse width and the pulse interval of the pulse are 2ms, the temperature is 25 ℃, and the voltage is 10V;
in step B, the roughening plating solution used comprises: cu2+：20g/L，H2SO4: 200g/L and coarsening additive 1 g/L; the coarsening additive may be selected from tungstate or molybdate.
In step E, the curing of the plating bath composition comprises: cu2+：60g/L，H2SO4：200g/L，Cl-：20mg/L。
The copper foil treated by the surface roughening and curing treatment method of case three is shown in fig. 4, and is opposite to fig. 1, so that the plating layer of the copper foil is flat and compact, the crystal grains are refined, and the surface is fine through the roughening and curing treatment method of case three.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (6)
1. A surface roughening and curing treatment method of RTF copper foil for a high-frequency copper-clad plate is characterized by comprising the following steps:
step A, acid washing pretreatment: washing an oxide layer on the surface of the original foil of the electrolytic copper foil to be treated by a pickling tank;
step B, primary coarsening electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 1: 2-5: 1, and the current density is ensured to be 20A-100A/dm2；
Step C, primary weak solidification electroplating: the current density of the original foil electroplated in the electrolytic bath is 20A-50A/dm2；
Step D, repeating B, C steps for 2-5 times;
step E, primary curing electroplating: electroplating the original foil in a coarsening electrolytic tank by using a pulse electroplating method, wherein the forward-reverse time ratio of the pulse electroplating is 3: 1-10: 1, and the current density is ensured to be 20A-50A/dm2。
2. The surface roughening and curing treatment method of RTF copper foil for high-frequency copper clad laminate according to claim 1,
the thickness of the original foil of the electrolytic copper foil is 0.012-0.070 mm.
3. The surface roughening and curing treatment method of RTF copper foil for high-frequency copper clad laminate according to claim 1,
the Rz of the original foil of the electrolytic copper foil is less than or equal to 5 mu m, and the Ra of the polished surface is less than or equal to 0.4 mu m.
4. The surface roughening and curing treatment method of RTF copper foil for high-frequency copper clad laminate according to claim 1,
in the step B and the step E, when pulse copper electroplating is carried out, the pulse width and the pulse interval of the pulse are 2-10 ms, the temperature is 25-45 ℃, and the voltage is 5-20V.
5. The method for roughening and curing the surface of the RTF copper foil for the high-frequency copper-clad plate according to claim 1, wherein the roughening plating solution used in the step B comprises: cu2+：10～20g/L，H2SO4: 100-200 g/L and 0.1-1 g/L of coarsening additive;
in step E, the curing of the plating bath composition comprises: cu2+：40～60g/L，H2SO4：100～200g/L，Cl-：5～20mg/L。
6. The surface roughening and curing treatment method of RTF copper foil for high-frequency copper-clad plate according to claim 1, wherein the anode plate is covered with a filter screen during the pulse copper electroplating.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114622253A (en) * | 2022-03-25 | 2022-06-14 | 电子科技大学 | Method for rapidly preparing copper foil for high-frequency substrate by double pulses |
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