CN106480479A - The preparation method of flexible additive for electrolytic copper foil, product and its application - Google Patents
The preparation method of flexible additive for electrolytic copper foil, product and its application Download PDFInfo
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- CN106480479A CN106480479A CN201610888713.5A CN201610888713A CN106480479A CN 106480479 A CN106480479 A CN 106480479A CN 201610888713 A CN201610888713 A CN 201610888713A CN 106480479 A CN106480479 A CN 106480479A
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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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- 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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Abstract
The invention discloses the preparation method of additive for electrolytic copper foil, product and its application, which includes the raw material components of following weight ratio：3 mercaptopropanesulfonic acid sodium；Sodium polydithio-dipropyl sulfonate；Ethylene thiourea；2 mercaptothiazolines；Sodium hydroxymethane sulfonate；Polyethylene glycol；Aliphatic amine polyoxyethylene ether；Hydroxyethyl cellulose.Which is used for preparing 6 to 12um electrolytic copper foil, when electrolytic copper foil is prepared, adds additive for electrolytic copper foil in electrolyte electrolytic process, and its additive flow is 100 300mL/Min, and electrolyte is：80 120g/L of content of copper ion, 90 130g/L of sulfate radical content, work 45 60 °C of liquid temp.By the electrolytic copper foil surface crystal grain of Additive Production of the present invention is smooth, profile is low, tensile strength, high-elongation, while having and the preferable sticking effect of polyimide base film and characteristic, can be used for high-end flexibility coat copper plate（FCCL）Circuit board matrix material.Additive low cost of the present invention, technique scope of application width, it is easy to technology controlling and process, it is ensured that product quality and benefit.
Description
Technical field
The present invention relates to field manufactured by electrolytic copper foil, and in particular to for preparing the high property of high ductibility of 6 to 12um
Additive of the flexible electrolytic copper foil of energy and preparation method thereof.
Background technology
With flexibility coat copper plate（FCCL）It is widely used in aerospace equipment, navigator, aircraft instrument, military guidance system
With electronic products such as mobile phone, digital camera, DV, vehicle satellite direction positioning device, LCD TV, notebook computers
In.Fast development due to electronic technology so that the stable yield of flexibility coat copper plate increases, production scale constantly expands, especially
It is the high performance flexibility coat copper plate with Kapton as base material, its demand and growth trend are more projected.FCCL is removed
Outside with thin, light and flexual advantage, with the FCCL of polyimide base film, also there is electrical property, hot property, heat resistance excellent
Good feature.Its relatively low-k（Dk）Property so that electric signal is quickly transmitted.Good hot property, can cause
Component is easy to cooling.Higher vitrification point（Tg）Component can be caused well to run at higher temperatures.As FCCL is big
Continuously to become web-like form to be supplied to user, therefore partial product, be, produce printed circuit board using FCCL, beneficial to realization
The automatic continuous production of FPC and carry out on FPC components and parts successional surface install.
The conductor material of flexibility coat copper plate, the overwhelming majority is to adopt Copper Foil, has electrolytic copper foil（ED）And rolled copper foil
（RA）, its own feature comprehensive, as main conductive transport vehicle Copper Foil must have high temperature resistant, high-transmission, high ductibility,
The performances such as high antistripping, only even property low profile, high-tensile, high-elongation, height put close, and the strong cathode copper of stickup property
Foil can meet simultaneously.
Content of the invention
For the problems referred to above, it is an object of the invention to, a kind of preparation method of flexibility additive for electrolytic copper foil is provided,
Its step is easy, and condition is easily controllable, low cost.
The present invention also aims to, a kind of flexible additive for electrolytic copper foil of employing said method preparation is provided, its
It is applied to and ultrathin electrolytic copper foil is prepared, in particular for produces 6 to 12um electrolytic copper foil.
For achieving the above object, the technical solution used in the present invention is：
A kind of preparation method of flexibility additive for electrolytic copper foil, comprises the following steps：
（1）Prepare the raw material components of following weight ratio：
3- mercaptopropanesulfonic acid 30～200mg/L of sodium；
20～120mg/L of sodium polydithio-dipropyl sulfonate；
30～180mg/L of ethylene thiourea；
40～250mg/L of 2-mercaptothiazoline；
35～250mg/L of sodium hydroxymethane sulfonate；
PEG20000 # 75～300mg/L；
30～180mg/L of aliphatic amine polyoxyethylene ether；
170～420mg/L of hydroxyethyl cellulose；
It is 1.5 according to weight： 1： 1.5 ：2： 2： 2.5：1.5：3.5 weigh 3- mercaptopropanesulfonic acid sodium respectively,
Sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, sodium hydroxymethane sulfonate, PEG20000 #, fatty amine gather
Oxygen vinethene, hydroxyethyl cellulose；
（2）By 3- mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, methylol sulfonic acid
Sodium, PEG20000 #, aliphatic amine polyoxyethylene ether, hydroxyethyl cellulose are each dissolved in 250mL deionization pure water, respectively
Obtain solution A, solution B, solution C, solution D, solution E, solution F, solution G, Solution H；
（3）By step（2）In solution A, solution B, solution C, solution D, solution E, solution F, that solution G, Solution H are poured into 5L is permanent
In temperature stirring cup, add deionized water 2L to spend under environment in constant temperature 55 to 60 and stir 30 minutes, obtain mixed liquor；
（4）By step（3）In mixed liquor deionized water be quantitatively diluted to 10L, complete additive package preparation.
Using flexible additive for electrolytic copper foil obtained in above-mentioned preparation method, which includes the raw material group of following weight ratio
Point：
3- mercaptopropanesulfonic acid 30～200mg/L of sodium；
20～120mg/L of sodium polydithio-dipropyl sulfonate；
30～180mg/L of ethylene thiourea；
40～250mg/L of 2-mercaptothiazoline；
35～250mg/L of sodium hydroxymethane sulfonate；
PEG20000 # 75～300mg/L；
30～180mg/L of aliphatic amine polyoxyethylene ether；
170～420mg/L of hydroxyethyl cellulose.
The application of above-mentioned flexibility additive for electrolytic copper foil, which is used for preparing 6 to 12um electrolytic copper foil.
The application of above-mentioned flexibility additive for electrolytic copper foil, which comprises the steps：When electrolytic copper foil is prepared, in electrolysis
Liquid electrolytic process adds described additive for electrolytic copper foil, and its additive flow is 100-300mL/Min.
The application of above-mentioned flexibility additive for electrolytic copper foil, electrolyte is：Content of copper ion 80-120g/L, sulfate radical contain
Amount 90-130g/L, work 45-60 °C of liquid temp.
Have the advantage that compared with prior art：
The present invention adds this additive package using electrolysis electrodeposition technology, the net liquid of copper sulphate；In the presence of electric field, following
Metallic copper is deposited on the titanium cathode roller that ring is rotated, after being peeled off by the stripper roll of unit, wind after anti-oxidation process.Wherein institute
State in electrolytic process, content of copper ion 80-120g/L, sulfate radical content 90-130g/L in electrolyte composition, work liquid temp
45-60 °C, add this additive package in electrolyte, flow of electrolyte is 60-90m3/H, current density 4500-12000A/
DC electrodeposition is carried out under M2, CL ion 50-100mg/L process environments；The electrolytic copper foil produced by the present invention, is enhanced
Tensile strength and peel strength, improve the reliability of fitting with base materials such as polyimide base film, are directly used in flexibility coat copper plate
Make.
By the electrolytic copper foil surface crystal grain of Additive Production of the present invention is smooth, profile is low, tensile strength, high-elongation,
While having and the preferable sticking effect of polyimide base film and characteristic, can be used for high-end flexibility coat copper plate（FCCL）Circuit board base
Body material.Additive low cost of the present invention, technique scope of application width, it is easy to technology controlling and process, it is ensured that product quality and benefit.
Specific embodiment
Embodiment 1：
The preparation method of the flexible additive for electrolytic copper foil that the present embodiment is provided, comprises the following steps：
（1）Prepare the raw material components of following weight ratio：
3- mercaptopropanesulfonic acid 30～200mg/L of sodium；
20～120mg/L of sodium polydithio-dipropyl sulfonate；
30～180mg/L of ethylene thiourea；
40～250mg/L of 2-mercaptothiazoline；
35～250mg/L of sodium hydroxymethane sulfonate；
PEG20000 # 75～300mg/L；
30～180mg/L of aliphatic amine polyoxyethylene ether；
170～420mg/L of hydroxyethyl cellulose；
It is 1.5 according to weight： 1： 1.5 ：2： 2： 2.5：1.5：3.5 weigh 3- mercaptopropanesulfonic acid sodium respectively,
Sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, sodium hydroxymethane sulfonate, PEG20000 #, fatty amine gather
Oxygen vinethene, hydroxyethyl cellulose；
（2）By 3- mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, methylol sulfonic acid
Sodium, PEG20000 #, aliphatic amine polyoxyethylene ether, hydroxyethyl cellulose are each dissolved in 250mL deionization pure water, respectively
Obtain solution A, solution B, solution C, solution D, solution E, solution F, solution G, Solution H；
（3）By step（2）In solution A, solution B, solution C, solution D, solution E, solution F, that solution G, Solution H are poured into 5L is permanent
In temperature stirring cup, add deionized water 2L to spend under environment in constant temperature 55 to 60 and stir 30 minutes, obtain mixed liquor；
（4）By step（3）In mixed liquor deionized water be quantitatively diluted to 10L, complete additive package preparation.
Using flexible additive for electrolytic copper foil obtained in above-mentioned preparation method, which includes the raw material group of following weight ratio
Point：
3- mercaptopropanesulfonic acid 30～200mg/L of sodium；
20～120mg/L of sodium polydithio-dipropyl sulfonate；
30～180mg/L of ethylene thiourea；
40～250mg/L of 2-mercaptothiazoline；
35～250mg/L of sodium hydroxymethane sulfonate；
PEG20000 # 75～300mg/L；
30～180mg/L of aliphatic amine polyoxyethylene ether；
170～420mg/L of hydroxyethyl cellulose.
The application of above-mentioned flexibility additive for electrolytic copper foil, which is used for preparing 6 to 12um electrolytic copper foil.
The application of above-mentioned flexibility additive for electrolytic copper foil, which comprises the steps：When electrolytic copper foil is prepared, in electrolysis
Liquid electrolytic process adds described additive for electrolytic copper foil, and its additive flow is 100-300mL/Min.
The application of above-mentioned flexibility additive for electrolytic copper foil, electrolyte is：Content of copper ion 80-120g/L, sulfate radical contain
Amount 90-130g/L, work 45-60 °C of liquid temp.
Embodiment 2：The preparation method of the flexible additive for electrolytic copper foil that the present embodiment is provided, its raw material components and step
All substantially the same manner as Example 1, its difference is：
（1）Prepare the raw material components of following weight ratio：
3- mercaptopropanesulfonic acid sodium 150mg/L；
Sodium polydithio-dipropyl sulfonate 100mg/L；
Ethylene thiourea 150mg/L；
2-mercaptothiazoline 200mg/L；
Sodium hydroxymethane sulfonate 200mg/L；
PEG20000 # 250mg/L；
Aliphatic amine polyoxyethylene ether 150mg/L；
Hydroxyethyl cellulose 350mg/L；
（2）By 3- mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, methylol sulfonic acid
Sodium, PEG20000 #, aliphatic amine polyoxyethylene ether, hydroxyethyl cellulose are each individually dissolved in 250mL deionization pure water,
Respectively obtain solution A, solution B, solution C, solution D, solution E, solution F, solution G, Solution H；
（3）By step（2）In solution A, solution B, solution C, solution D, solution E, solution F, that solution G, Solution H are poured into 5L is permanent
In temperature stirring cup, add deionized water 2L to spend under environment in constant temperature 55 to 60 and stir 30 minutes, obtain mixed liquor；
（4）By step（3）In mixed liquor deionized water be quantitatively diluted to 10L, complete additive package preparation.
Embodiment 3：The preparation method of the flexible additive for electrolytic copper foil that the present embodiment is provided, its raw material components and step
All essentially identical with embodiment 1,2, its difference is：
（1）Prepare the raw material components of following weight ratio：
3- mercaptopropanesulfonic acid sodium 100mg/L；
Sodium polydithio-dipropyl sulfonate 50mg/L；
Ethylene thiourea 100mg/L；
2-mercaptothiazoline 150mg/L；
Sodium hydroxymethane sulfonate 150mg/L；
PEG20000 # 200mg/L；
Aliphatic amine polyoxyethylene ether 100mg/L；
Hydroxyethyl cellulose 300mg/L；
（2）By 3- mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, methylol sulfonic acid
Sodium, PEG20000 #, aliphatic amine polyoxyethylene ether, hydroxyethyl cellulose are each individually dissolved in 250mL deionization pure water,
Respectively obtain solution A, solution B, solution C, solution D, solution E, solution F, solution G, Solution H；
（3）By step（2）In solution A, solution B, solution C, solution D, solution E, solution F, that solution G, Solution H are poured into 5L is permanent
In temperature stirring cup, add deionized water 2L to spend under environment in constant temperature 55 to 60 and stir 30 minutes, obtain mixed liquor；
（4）By step（3）In mixed liquor deionized water be quantitatively diluted to 10L, complete additive package preparation.
Embodiment 4：The preparation method of the flexible additive for electrolytic copper foil that the present embodiment is provided, its raw material components and step
All all essentially identical with one of embodiment 1,2,3, its difference is：
（1）Prepare the raw material components of following weight ratio：
3- mercaptopropanesulfonic acid sodium 80mg/L；
Sodium polydithio-dipropyl sulfonate 30mg/L；
Ethylene thiourea 80mg/L；
2-mercaptothiazoline 130mg/L；
Sodium hydroxymethane sulfonate 130mg/L；
PEG20000 # 180mg/L；
Aliphatic amine polyoxyethylene ether 80mg/L；
Hydroxyethyl cellulose 280mg/L；
（2）Respectively by 3- mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, methylol
Sodium sulfonate, PEG20000 #, aliphatic amine polyoxyethylene ether, it is pure that hydroxyethyl cellulose is each individually dissolved in 250mL deionization
In water, solution A, solution B, solution C, solution D, solution E, solution F, solution G, Solution H is respectively obtained；
（3）By step（2）In solution A, solution B, solution C, solution D, solution E, solution F, that solution G, Solution H are poured into 5L is permanent
In temperature stirring cup, add deionized water 2L to spend under environment in constant temperature 55 to 60 and stir 30 minutes, obtain mixed liquor；
（4）By step（3）In mixed liquor deionized water be quantitatively diluted to 10L, complete additive package preparation.
Advantages of the present invention：Using electrolysis electrodeposition technology, the net liquid of copper sulphate adds this additive package；By electric field
Under effect, on the titanium cathode roller of cycle rotation, metallic copper is deposited, after being peeled off by the stripper roll of unit, after anti-oxidation process
Winding.In wherein described electrolytic process, content of copper ion 80-120g/L, sulfate radical content 90-130g/L in electrolyte composition,
45-60 °C of liquid temp of work, adds this additive package in electrolyte, and flow of electrolyte is 60-90m3/H, current density
DC electrodeposition is carried out under 4500-12000A/M2, CL ion 50-100mg/L process environments；The electrolysis produced by the present invention
Copper Foil, enhances tensile strength and peel strength, improves the reliability of fitting with base materials such as polyimide base film, is directly used in
Flexibility coat copper plate makes.
By the electrolytic copper foil surface crystal grain of Additive Production of the present invention is smooth, profile is low, tensile strength, high-elongation,
While having and the preferable sticking effect of polyimide base film and characteristic, can be used for high-end flexibility coat copper plate（FCCL）Circuit board base
Body material.Additive low cost of the present invention, technique scope of application width, it is easy to technology controlling and process, it is ensured that product quality and benefit.
After testing, prepared electrolytic copper foil hair side roughness is 2 μm of Rz ＜, and light surface roughness is Ra ＜ 0.35
μm, thickness is 6 ~ 12 μm, and surface density is 57-100 ± 1.5g/m 2, hydrophily ＞ 35, room temperature tensile strength ＞ 30kg/
Mm 2, bending performance are more than 100,000 times, normal temperature elongation percentage 5.5%.
The present invention is not limited to above-described embodiment, all using same as the previously described embodiments or similar technical scheme, reaches
To other schemes of the object of the invention, all within the scope of the present invention.
Claims (5)
1. a kind of flexibility additive for electrolytic copper foil preparation method, it is characterised in that comprise the following steps：
（1）Prepare the raw material components of following weight ratio：
3- mercaptopropanesulfonic acid 30～200mg/L of sodium；
20～120mg/L of sodium polydithio-dipropyl sulfonate；
30～180mg/L of ethylene thiourea；
40～250mg/L of 2-mercaptothiazoline；
35～250mg/L of sodium hydroxymethane sulfonate；
PEG20000 # 75～300mg/L；
30～180mg/L of aliphatic amine polyoxyethylene ether；
170～420mg/L of hydroxyethyl cellulose；
It is 1.5 according to weight： 1： 1.5 ：2： 2： 2.5：1.5：3.5 weigh 3- mercaptopropanesulfonic acid sodium respectively,
Sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, sodium hydroxymethane sulfonate, PEG20000 #, fatty amine gather
Oxygen vinethene, hydroxyethyl cellulose；
（2）By 3- mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, ethylene thiourea, 2-mercaptothiazoline, methylol sulfonic acid
Sodium, PEG20000 #, aliphatic amine polyoxyethylene ether, hydroxyethyl cellulose are each dissolved in 250mL deionization pure water, respectively
Obtain solution A, solution B, solution C, solution D, solution E, solution F, solution G, Solution H；
（3）By step（2）In solution A, solution B, solution C, solution D, solution E, solution F, that solution G, Solution H are poured into 5L is permanent
In temperature stirring cup, add deionized water 2L to spend under environment in constant temperature 55 to 60 and stir 30 minutes, obtain mixed liquor；
（4）By step（3）In mixed liquor deionized water be quantitatively diluted to 10L, complete additive package preparation.
2. one kind flexible additive for electrolytic copper foil obtained in method according to claim 1, it is characterised in that it include with
The raw material components of lower weight ratio：
3- mercaptopropanesulfonic acid 30～200mg/L of sodium；
20～120mg/L of sodium polydithio-dipropyl sulfonate；
30～180mg/L of ethylene thiourea；
40～250mg/L of 2-mercaptothiazoline；
35～250mg/L of sodium hydroxymethane sulfonate；
PEG20000 # 75～300mg/L；
30～180mg/L of aliphatic amine polyoxyethylene ether；
170～420mg/L of hydroxyethyl cellulose.
3. a kind of application of flexible according to claim 2 additive for electrolytic copper foil, it is characterised in which is used for preparing 6
To 12um electrolytic copper foil.
4. the application of flexible additive for electrolytic copper foil according to claim 3, it is characterised in which comprises the steps：
When electrolytic copper foil is prepared, gradually add described additive for electrolytic copper foil, its additive flow in electrolyte electrolytic process
For 100 300mL/Min.
5. the application of flexible additive for electrolytic copper foil according to claim 4, it is characterised in that the electrolyte is：Copper
Ion concentration 80-120g/L, sulfate radical content 90-130g/L, work 45-60 °C of liquid temp.
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Effective date of registration: 20221122 Address after: No. 118, Rixin Road, Xuancheng economic and Technological Development Zone, Xuancheng City, Anhui Province Patentee after: ANHUI HUAWEI COPPER FOIL TECHNOLOGY CO.,LTD. Address before: 523000 No.2 Industrial Zone, matigang village, Dalingshan Town, Dongguan City, Guangdong Province Patentee before: DONGGUAN WAHWEI COPPER FOIL TECHNOLOGY Co.,Ltd. |