CN102234823B - Copper material used for producing electrolytic copper foil, and method for producing electrolytic copper foil - Google Patents
Copper material used for producing electrolytic copper foil, and method for producing electrolytic copper foil Download PDFInfo
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- CN102234823B CN102234823B CN 201010171504 CN201010171504A CN102234823B CN 102234823 B CN102234823 B CN 102234823B CN 201010171504 CN201010171504 CN 201010171504 CN 201010171504 A CN201010171504 A CN 201010171504A CN 102234823 B CN102234823 B CN 102234823B
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Abstract
The invention relates to a copper material used for producing electrolytic copper foil, and a method for producing electrolytic copper foil. The copper material used for producing electrolytic copper foils is a corrugated copper strip, wherein the corrugated copper strip is produced from a copper plate through processes of punching, cutting, and the like. The corrugations of the copper strip have certain dimension scales. During an electrolytic copper foil producing process, the copper strips are stacked in a dissolving tank. When a large amount of copper strips are stacked, large contact areas are maintained between the copper materials and the sulfuric acid electrolyte. Therefore, the copper materials are dissolved quickly, and are oxidized into copper ions. The copper material provided by the invention can be quickly dissolved in sulfuric acid electrolyte, and copper ions are formed. The copper material is used as a supplement source of copper ions during an electrolytic copper foil producing process. With the material, integral production efficiency can be improved, and productivity can be improved.
Description
Technical field
The present invention is about a kind of manufacture method of making the raw material of electrolytic copper foil and using this raw material, especially in regard to a kind of method that has the electrolytic copper foil raw material of specific dimensions ratio and use this raw material.
Background technology
Copper-clad laminate in printed circuit board (PCB) is to be formed by electrolytic copper foil and resol or epoxy resin pressing.In the electrolytic copper foil production process, the electrolytic solution that mainly utilizes copper sulfate, sulfuric acid and other added ingredients to form through electrochemical reaction, is reduced into metal copper foil with the cupric ion in electrolytic solution.In above-mentioned reaction, after the cupric ion in copper sulfate electrolyte was reduced into metal copper foil, copper ion concentration descended gradually, in order to ensure the Copper Foil quality, the copper ion concentration in electrolytic solution must be controlled within the specific limits.
Generally speaking, in the electrolytic copper foil production process, except forming the electrolyzer of metal copper foil in order to carry out electrochemical reaction, separately be provided with dissolving tank.The purposes of this dissolving tank is to utilize sulfuric acid that copper material dissolved oxygen is cupric ion, forms copper-bath, then it is imported in electrolyzer, to keep the copper ion concentration in electrolyzer, guarantees the quality of electrolytic copper foil.In order to stablize the copper ion concentration in electrolyzer, the copper raw metal in dissolving tank must continue and rapidly in vitriolization solution.In other words, the copper material is continued and dissolving rapidly, become the considerable factor of electrolytic copper foil production efficiency that improves.
In the past, used copper coin as the copper material in the electrolytic copper foil production process, directly copper coin be placed in the dissolving tank that contains sulphuric acid soln, make copper coin slowly dissolved oxygen change into cupric ion.But because the dissolution rate of copper coin is too slow, existing multiple modification method.For example, reel off raw silk from cocoons into the copper cash of diameter below 10 millimeters after copper coin is melted, or directly copper coin is cut into copper billet or copper bar, to increase the contact area of copper material and sulphuric acid soln, improve dissolution rate.Yet the melting copper coin reels off raw silk from cocoons smelting furnace need to be set, and increases equipment cost.Copper coin is cut into copper billet or copper bar, though can increase the contact area of copper material and sulphuric acid soln, the specific surface area of copper billet and copper bar is still not enough, and the speed of dissolving is still quite slow.
Therefore, in the electrolytic copper foil production process, still need a kind of can continuing and the copper material of vitriolization electrolytic solution rapidly.
Summary of the invention
The object of the invention is to provide a kind of copper material for the manufacture of electrolytic copper foil, and it can continue and vitriolization electrolytic solution rapidly.
Another purpose of the present invention is to provide a kind of method of making electrolytic copper foil, and it can make the copper material continue and vitriolization electrolytic solution rapidly.
For reaching above-mentioned and other purpose, the invention provides a kind of copper material for the manufacture of electrolytic copper foil, this copper material is the copper bar that is wavy and has the specific dimensions ratio, the adjacent peaks of this wavy copper bar and the horizontal throw of trough are between 20 to 140 millimeters, and the vertical drop of crest and trough is between 1 to 80 millimeter.When copper material of the present invention is stacked in the electrolytic copper foil production process applied dissolving tank, under the condition of a large amount of storehouses, still can keep sizable contact area between copper material and sulfuric acid electrolyte, make the copper material can dissolve fast and be oxidized to cupric ion.Copper material of the present invention, vitriolization electrolytic solution and form cupric ion fast is applied in the electrolytic copper foil production process to help to improve integral production efficient as the additional source of cupric ion, increases production capacity.
The present invention also provides a kind of method of electrolytic copper foil, comprises that copper bar this is wavy and that have a specific dimensions ratio is placed in the dissolving tank that contains sulfuric acid electrolyte, as the copper material of making electrolytic copper foil; This copper bar dissolved and be oxidized to cupric ion, replenishing the source as the cupric ion in the electrolytic copper foil production process; And the electrolytic solution that will contain cupric ion sends into and carries out electrochemical reaction in electrolyzer, makes this cupric ion be reduced into the Copper Foil metal.
Description of drawings
Figure 1A to Fig. 1 D show to form the specific examples of the copper material for the manufacture of electrolytic copper foil of the present invention.
Wherein, description of reference numerals is as follows:
110 copper coins
120 wavy copper coins
130 wavy copper bars
L length
The LW horizontal throw
The SW difference of altitude
T thickness
The W face width
Embodiment
Below by specific specific examples explanation embodiment of the present invention, those skilled in the art can understand advantage of the present invention and effect easily by content disclosed in the present specification.The present invention can also other different mode be implemented, and, under not departing from disclosed category, can give different modifications and change that is.
Figure 1A to Fig. 1 D show to form the specific examples of the copper material for the manufacture of electrolytic copper foil of the present invention.In this specific examples, use copper coin to carry out punching press, the procedure of processing such as cut and form the wavy copper bar with specific dimensions, as the copper material of making electrolytic copper foil.There is no particular restriction in order to the copper coin processed, generally can be used in the electrolytic copper foil production process, all can use as the copper coin of cupric ion supplementary source.At first, utilize the directed punching press copper coin of decompressor 110 surfaces of copper coin cutting machine, make copper coin present wave-like, form wavy copper coin 120, as shown in Figure 1A, Figure 1B.Then, utilize cutting machine should wavy copper coin 120 to cut and be divided into several wavy copper bars 130, as shown in Fig. 1 C, obtain the copper material for the manufacture of electrolytic copper foil of the present invention.
Generally speaking, keep the wave-like of specific dimensions in order to make formed copper material, and increase the contact area of copper material and sulfuric acid electrolyte, the thickness of the copper coin that uses is to be no more than 15 millimeters as good.If the copper plate thickness that uses is too thick, the procedure of processing such as not only be unfavorable for punching press, cut also is unfavorable for increasing the contact area of copper material and sulfuric acid electrolyte.As shown in Fig. 1 D, in order to take into account the processing convenience of copper coin, and keep the specific wave-like of copper bar, increase this wavy copper bar can with the contact area of sulfuric acid electrolyte, the thickness T of wavy copper bar of the present invention is preferably between 3 to 20 millimeters, more preferably between 6 to 10 millimeters; The face width W of this wavy copper bar is preferably between 1 to 25 millimeter, more preferably between 2 to 20 millimeters.
Wavy copper bar of the present invention is mainly used in the electrolytic copper foil production process, is placed in the dissolving tank that contains sulfuric acid electrolyte and originates as the cupric ion of electrolytic copper foil production process is additional.In order to increase the copper stockpile stack quantity in applied dissolving tank in this electrolytic copper foil production process, and keep appropriate gap between each copper material of institute's storehouse, increase the contact area of copper material and sulfuric acid electrolyte, make the copper material dissolve fast and to be oxidized to cupric ion, the shape of the wavy copper bar of the present invention has specific dimension scale.As shown in Fig. 1 C, the wavy copper bar as copper material in the electrolytic copper foil production process of the present invention, the horizontal throw LW of its adjacent peaks and trough is preferably between 20 to 140 millimeters, more preferably between 60 to 100 millimeters; And the vertical drop SW of the crest of this wavy copper bar and trough, preferably between 1 to 80 millimeter, more preferably between 5 to 50 millimeters.On the other hand, there is no particular restriction for the length of this wavy copper bar, can put into the applied dissolving tank of electrolytic copper foil production process and get final product.Usually, the length L of this wavy copper bar is between 30 to 3000 millimeters, preferably between 100 to 1500 millimeters.
Generally speaking, in the electrolytic copper foil production process of Copper Foil factory, mainly utilize sulphuric acid soln to corrode, dissolve the copper material, the copper material is dissolved and be oxidized to cupric ion, form copper-bath, and this copper-bath is imported in electrolyzer as electrolytic solution, carry out electrochemical reaction, make the cupric ion in copper-bath be reduced into the Copper Foil metal.On the other hand, in this electrolytic copper foil production process, along with the cupric ion in electrolyzer is reduced into the Copper Foil metal, the copper ion concentration in this electrolyzer can descend gradually.Therefore, need constantly supplementation with copper ion, to keep the copper ion concentration in electrolyzer.
Electrolytic copper foil method of the present invention is used has the wavy copper bar of specific dimensions ratio as the copper material in the electrolytic copper foil production process, this copper material is placed in the dissolving tank that contains sulphuric acid soln, the copper material is dissolved and be oxidized to cupric ion, form copper sulfate electrolyte, again this copper sulfate electrolyte is imported in electrolyzer, keep the copper ion concentration in electrolyzer, then via electrochemical reaction, make the cupric ion in electrolyzer be reduced into the Copper Foil metal.
Electrolytic copper foil method of the present invention uses the wavy copper bar with specific dimensions ratio as the copper material of making electrolytic copper foil, because the wavy copper bar of this kind can be stacked in the dissolving tank that contains sulphuric acid soln in large quantities, process in dissolving, still can keep suitable gap between the copper bar of each storehouse, make and keep sizable contact area between copper material and sulfuric acid electrolyte.Therefore, the copper material can dissolve and be oxidized to cupric ion rapidly, forms copper-bath, makes electrolyzer keep stable copper ion concentration, helps to improve integral production efficient, increases production capacity.
Embodiment
Embodiment 1
Get 8 millimeters of thickness, each copper coin of 400 millimeters of length and width carries out punching press, cuts the wavy copper bar sample 1 of formation, 12.55 kilograms of gross weights.As listed in table 1, the adjacent peaks of this wavy copper bar sample 1 and trough horizontal throw LW are 80 millimeters, and crest and trough vertical drop SW are 25 millimeters, and face width W is 7 millimeters.
Under 60 ℃ of conditions, carry out the dissolution rate test of wavy copper bar sample.This wavy copper bar sample 1 is placed in the sulphuric acid soln (concentration 100 grams per liters) of 125.5 liters, after 24 hours, measures the gross weight after wavy copper bar sample 1 dissolves, calculate meltage and dissolution rate, and result is embedded in table 1.
Embodiment 2
Get 8 millimeters of thickness, each copper coin of 400 millimeters of length and width carries out punching press, cuts the wavy copper bar sample 2 of formation, 11.48 kilograms of gross weights.As listed in table 1, the adjacent peaks of this wavy copper bar sample 2 and trough horizontal throw LW are 80 millimeters, and crest and trough vertical drop SW are 25 millimeters, and face width W is 5 millimeters.
Under 60 ℃ of conditions, carry out the dissolution rate test of wavy copper bar sample.This wavy copper bar sample 2 is placed in the sulphuric acid soln (concentration 100 grams per liters) of 114.8 liters, after 24 hours, measures the gross weight after wavy copper bar sample 2 dissolves, calculate meltage and dissolution rate, and result is embedded in table 1.
Embodiment 3
Get 8 millimeters of thickness, each copper coin of 400 millimeters of length and width carries out punching press, cuts the wavy copper bar sample 3 of formation, 12.76 kilograms of gross weights.As listed in table 1, the adjacent peaks of this wavy copper bar sample 3 and trough horizontal throw LW are 80 millimeters, and crest and trough vertical drop SW are 15 millimeters, and face width W is 5 millimeters.
Under 60 ℃ of conditions, carry out the dissolution rate test of wavy copper bar sample.This wavy copper bar sample 3 is placed in the sulphuric acid soln (concentration 100 grams per liters) of 127.6 liters, after 24 hours, measures the gross weight after wavy copper bar sample 3 dissolves, calculate meltage and dissolution rate, and result is embedded in table 1.
Comparative example 1
Get 8 millimeters of thickness, each copper coin of 400 millimeters of length and width carries out punching press, cuts the wavy copper bar comparative sample 1 of formation, 12.89 kilograms of gross weights.As listed in table 1, the adjacent peaks of comparative sample 1 and trough horizontal throw LW are 200 millimeters, and crest and trough vertical drop SW are 15 millimeters, and face width W is 5 millimeters.
Under 60 ℃ of conditions, carry out the dissolution rate test of wavy copper bar sample.Comparative sample 1 is placed in the sulphuric acid soln (concentration 100 grams per liters) of 128.9 liters, after 24 hours, measures the gross weight after comparative sample 1 dissolves, calculate meltage and dissolution rate, and result is embedded in table 1.
Comparative example 2
Get 8 millimeters of thickness, each copper coin of 400 millimeters of length and width cuts and forms copper bar comparative sample 2,13.33 kilograms of gross weights.As listed in table 1, the face width W of comparative sample 2 is 5 millimeters.
Under 60 ℃ of conditions, carry out the dissolution rate test of copper bar sample.Comparative sample 2 is placed in the sulphuric acid soln (concentration 100 grams per liters) of 133.3 liters, after 24 hours, measures the gross weight after comparative sample 2 dissolves, calculate meltage and dissolution rate, and result is embedded in table 1.
Comparative example 3
Get 8 millimeters of thickness, each copper coin of 400 millimeters of length and width is cut into the copper ingot sample 3 as a comparison of 20 millimeters * 20 millimeters, 12.10 kilograms of gross weights.
Under 60 ℃ of conditions, carry out the dissolution rate test of copper coin sample.Comparative sample 3 is placed in the sulphuric acid soln (concentration 100 grams per liters) of 121.0 liters, after 24 hours, measures the gross weight after comparative sample 3 dissolves, calculate meltage and dissolution rate, and result is embedded in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | ||
| Thickness T | 8 | 8 | 8 | 8 | 8 | 8 | |
| Width W | 7 | 5 | 5 | 5 | 5 | - | |
| Horizontal throw LW | 80 | 80 | 80 | 200 | - | - | |
| Difference of altitude SW | 25 | 25 | 15 | 15 | - | - | |
| Gross weight (kilogram) before dissolving | 12.55 | 11.48 | 12.76 | 12.89 | 13.33 | 12.10 | |
| Gross weight (kilogram) after dissolving | 11.98 | 10.94 | 12.23 | 12.55 | 13.09 | 11.95 | |
| Meltage (kilogram) | 0.57 | 0.54 | 0.53 | 0.34 | 0.24 | 0.15 | |
| Dissolution rate (%) | 4.54 | 4.70 | 4.15 | 2.64 | 1.80 | 1.24 |
Show according to table 1 result, use the copper coin (comparative example 3) that does not cut as the copper material, because its surface-area is limited, the dissolution rate in sulphuric acid soln only approximately 1.2%.If the copper coin material is cut to copper bar (comparative example 2) as the copper material, although surface-area increases, during a large amount of storehouse, can't keep the gap between each storehouse copper bar, therefore the contact area of copper material and sulphuric acid soln limited still, dissolution rate only is increased to 1.8%.
On the other hand, the present invention first strikes out copper coin wavy, cut into again have specific dimensions wavy copper bar (embodiment 1,2,3) as the copper material, owing to keeping suitable gap between the wavy copper bar of each storehouse, make and keep larger contact area between copper material and sulfuric acid electrolyte, can make dissolution rate be promoted to 4%, even more than 4.5%.In comparison, if wavy copper bar (comparative example 1) does not have specific dimensions of the present invention, can't effectively keep the gap between the wavy copper bar of each storehouse, its dissolution rate only is promoted to approximately 2.5%, and effect is limited still.
Claims (7)
1. copper material for the manufacture of electrolytic copper foil, this copper material is to be wavy copper bar, and the adjacent peaks of this wavy copper bar and the horizontal throw of trough are between 20 to 140 millimeters, and the vertical drop of crest and trough is between 1 to 80 millimeter, wherein, the face width of this wavy copper bar is between 1 to 7 millimeter, and the thickness of this wavy copper bar is between 3 to 20 millimeters.
2. copper material as claimed in claim 1, wherein, the adjacent peaks of this wavy copper bar and the horizontal throw of trough are between 60 to 100 millimeters.
3. copper material as claimed in claim 1, wherein, the adjacent peaks of this wavy copper bar and the vertical drop of trough are between 5 to 50 millimeters.
4. copper material as claimed in claim 1, wherein, the thickness of this wavy copper bar is between 6 to 10 millimeters.
5. copper material as claimed in claim 1, wherein, the length of this wavy copper bar is between 30 to 3000 millimeters.
6. copper material as claimed in claim 1, be to be formed by the copper coin machining, comprises the following steps:
Utilize directed punching press to make copper coin present wave-like; And
Utilize cutting machine to cut into a plurality of wavy copper bars by wavy copper coin.
7. the method for an electrolytic copper foil comprises:
(a) copper material as claimed in claim 1 is placed in the dissolving tank that contains sulfuric acid electrolyte as the copper material of making electrolytic copper foil;
(b) this copper bar dissolved and be oxidized to cupric ion, replenishing the source as the cupric ion in the electrolytic copper foil production process; And
The electrolytic solution that (c) will contain cupric ion is sent into and is carried out electrochemical reaction in electrolyzer, makes this cupric ion be reduced into the Copper Foil metal.
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| CN109137019B (en) * | 2018-08-14 | 2019-12-31 | 歌尔股份有限公司 | Continuous plating method |
| US10581081B1 (en) | 2019-02-01 | 2020-03-03 | Chang Chun Petrochemical Co., Ltd. | Copper foil for negative electrode current collector of lithium ion secondary battery |
| CN110295380A (en) * | 2019-06-19 | 2019-10-01 | 九江德福科技股份有限公司 | A kind of copper foil pot for smelted copper copper material method for arranging |
| CN112323102A (en) * | 2020-11-04 | 2021-02-05 | 湖南龙智新材料科技有限公司 | Electrolytic copper foil for FPC and preparation method thereof |
| CN113089035B (en) * | 2021-04-14 | 2021-10-15 | 广东嘉元科技股份有限公司 | Copper dissolving method for electrolytic copper foil production and copper dissolving device adopting same |
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