CN109056009B - A kind of copper foil for printed circuit board and preparation method thereof - Google Patents
A kind of copper foil for printed circuit board and preparation method thereof Download PDFInfo
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- CN109056009B CN109056009B CN201810944963.5A CN201810944963A CN109056009B CN 109056009 B CN109056009 B CN 109056009B CN 201810944963 A CN201810944963 A CN 201810944963A CN 109056009 B CN109056009 B CN 109056009B
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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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/58—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- Parts Printed On Printed Circuit Boards (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The present invention relates to a kind of copper foil for printed circuit board, the one side that copper foil is engaged with resin substrate is the copper alloy layer of Cu-Ti-Nb-Mo, other three kinds of alloying element Ti-Nb-Mo add up to institute's accounting to be 0.0005-2%wt in copper alloy layer, Ti:Nb:Mo=10:1:39 in copper alloy layer, using include the following steps: following preparation method by untreated copper foil carry out plating, plating solution is conventional sulfuric acid copper electrolyte, wherein contain Ti, Nb, the compound of Mo, it adds up to 0.01-5g/L, the peel strength of prepared copper foil is 2.0-2.5kg/cm, current density is 25-35A/dm2, electroplating time is 4-8 seconds, with a thickness of 0.25-2.0 μm, roughened layer is preferably realized without picking phenomenon , peel strength is high, and electrical characteristic is good.
Description
Technical field
The present invention relates to printed circuit board (PCB), more particularly to a kind of improved copper foil for printed circuit board and its system
Preparation Method.
Background technique
Electronic circuit board plays relaying in the connection for being used between electronic component be formed predetermining circuit in electronic component
The effect of transmission is the critical electronic interconnection piece of electronic product.And the copper foil as wiring board is major components, the prior art
The copper foil of preparation will also meet specific electrical characteristic, heat resistance and can lose to improve the binding force with resin substrate
Quarter property generally will carry out roughening treatment to copper foil.Electrolyzing and coarsening is one of processing method.
The copper foil of existing copper foil production technology production, due to the crystalline structure of hair side deposition in surface treatment coarsening process
Structure is very loose, easily forms more copper powder, and more copper powder or copper powder diameter are more than 50 μm, in production printed circuit board
The risk for occurring short circuit in the process is very high, when copper foil hair side copper powder quantity is more, will lead to copper foil after the client of downstream
Circuit is punctured or short-circuited in process, seriously affects the quality of product.
With the fast development of printed circuit board industry, the miniaturization of electronic component and printed circuit board it is fine
Change, short circuit risk caused by more hair side copper powder is higher and higher.
Existing technical solution can not effectively solve the problems, such as that hair side copper powder is more, generally use adjusting roughening, solidification electricity
Stream reduces copper powder and generates.Copper powder can only be inhibited to generate to a certain extent, effect is unobvious, fundamentally cannot effectively solve
Hair side copper powder.
In addition, for the roughening treatment of copper foil surface, it is known that there are also the formation of cobalt-nickel alloy coating, still, with
Past formation has the copper foil of cobalt-nickel alloy coating, the roughening grain obtained by copper-cobalt-nickel alloy plating being formed on its surface
The shape of son is dendroid, and the top of the branch or root are peeled off, commonly referred to as powder falling phenomenon.
103397342 A of Chinese invention patent application CN discloses a kind of high heat resistance electrolytic copper foil and preparation method thereof,
Be characterized in that: high heat resistance electrolytic copper foil of the invention is suitable for the high-speed high frequency of LOW DK/Df, high heat resistance CCL and pcb board material
The electrolytic copper foil of demand, its hair side crystal grain are in laminated crystalline.The preparation method is that being using DC electrodeposition technique
After electrolytic copper foil is made, different electrolyte combination and electro-deposition process parameter are taken in electrolysis installation by multiple stages
Cooperation processing carries out pickling processes, low roughening treatment, curing process, Darkening process, washing, oxygen to the surface of electrolytic copper foil
Change processing, hot water wash, silane treatment and baking process.However the processing method roughness is different, granular size is different.
103590077 A of Chinese invention patent application CN is disclosed for printed circuit board and lithium ion secondary battery
The manufacturing method of electrolytic copper foil, comprising the following steps: prepare additive solution, include polydithio-dipropyl sulphur in additive solution
Sour sodium, polyethylene glycol, hydrochloric acid, 3-sulfydryl-1-propane sulfonic acid sodium；Copper sulfate electrolyte is taken, copper sulfate electrolyte is heated to 45
Additive solution is added in copper sulfate electrolyte after~60 DEG C, the electrolyte formed after uniform stirring enters electrolytic cell,
Current density of the electrolyte in electrolytic cell is 40~80A/dm2, is electrochemically reacted；It is 0.1~5g/L and pH with concentration
It is worth the chromatedsolution less than 6.0 and surface passivation is carried out to copper foil；After surface passivation, carry out apply silane coupling agent processing to get
To the electrolytic copper foil for printed circuit board and lithium ion secondary battery.The patent application is detailed there is no carrying out for roughening
Discussing it still can unavoidably generate dendrite, and peel strength is low.
Chinese invention patent application CN201410083759.0 discloses a kind of flexible circuit board electrolytic copper foil additive,
It is characterized in that, in every L additive solution, the solute component of included following quality: 10~20mg of cellulose；Titanium sulfate 1~
3mg；3~7mg of sodium tungstate；5~15mg of polypropylene glycol.Invention additionally discloses the addictive preparation method and its applications.This flexibility
Circuit board electrolytic copper foil additive can lower electrolytic copper foil hair side roughness, increase the crystal density of crystal grain and increase tension strong
Degree, peel strength.By rationally adding this additive, the copper foil quality of preparation is reachable: weight per unit area: 107 grams/m2,
Room temperature tensile strength >=30kg/mm2, peel strength >=0.8kg/cm, room temperature elongation percentage >=25%, surface roughness: Ra
≤ 2.0 microns, standard bending: > 150,000 times, it is much better than existing additive.Although it is the improvement for electrolyte,
It is that its peel strength is very low, only 0.8kg/cm, and also electrolyte composition is complicated, and technique is unstable.
It is to be used in high-frequency circuit board can also inhibit to pass well that Chinese invention patent application CN104125711A, which is provided,
Defeated loss and the high-frequency circuit copper foil that copper foil surface generation powder falling can be inhibited well.High-frequency circuit copper of the invention
Foil is 3 formd on the primary particle layer after the primary particle layer that the surface of copper foil forms copper comprising copper, cobalt and nickel
Member is the copper foil of the offspring layer of alloy, the three-dimensional table of the certain area in roughening treatment face obtained based on laser microscope
Area is 2.0 more than and less than 2.2 relative to bivariate table area ratio.Although it solves powder falling phenomenon to a certain extent,
But its normality peel strength is lower.Performance is to be improved.
Chinese invention patent application CN104451796A provides a kind of high frequency printing board surface treatment process, including following
Step: (1) alkalescent oil removal treatment: rolled copper foil is placed in alkalescent mixing degreasing fluid；(2) roughening treatments:
Rolled copper foil by above-mentioned pickling is placed in an electroplate liquid；(3) secondary roughening treatment: by treated calendering
Copper foil is again placed in second time electroplating liquid；(4) barrier layer coating is handled: the above-mentioned rolled copper foil after roughening treatment is passed through again
Zinc-nickel alloy coating processing；(5) it anti-oxidation processing: will be handled again through coating by above-mentioned processed rolled copper foil；By the pressure
Prolong copper foil to be placed in four electroplate liquids；The present invention, which has, goes that speed oil is fast, effect is good, corrosion is small and to rolled copper foil clean surface
Preferable advantage；And the corrosion resistance of rolled copper foil is also improved, and can also improve the binding force of itself and printed board.It should
Application does not have recognized the need at all solves the problems, such as that roughening ion is fallen.And its treatment process effect is general.
Chinese invention patent application CN104928740A discloses a kind of processing method for reducing copper foil hair side copper powder, will give birth to
The hair foil of foil plating passes sequentially through the 1st roughening process, the 2nd roughening process, the 1st curing process, the 2nd curing process, galvanizer
Sequence, anti-oxidation process, coupling agent painting process, baking process processing.Treatment process through the invention, largely reduces copper powder
It generates, copper foil 10cm2Copper powder quantity is no more than 10 in sample, and maximum copper powder diameter is no more than 30 μm, significantly reduces it
Lead to the risk of short circuit for making printed circuit board in the process, solves the problems, such as powder although proposing, what is passed through consolidates
The problems such as change complex procedures, process flow is long.
Summary of the invention
For above-mentioned technical problem present in the prior art, the technical problems to be solved by the present invention are: preventing from being electrolysed
The removing easily of roughening of copper foil layer copper particle causes picking phenomenon.
On the basis of existing technology, discovery forms the ultra-thin copper alloy layer comprising Cu-Ti-Nb-Mo to the present inventor
Copper foil can not only solve picking phenomenon, additionally it is possible to provide preferable peel strength and etching characteristic.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme:
A kind of copper foil for printed circuit board, the one side that copper foil is engaged with resin substrate are the copper alloy layer of Cu-Ti-Nb-Mo.
It is preferred that: other three kinds of alloying element Ti-Nb-Mo add up to institute's accounting to be 0.0005-2%wt in copper alloy layer.
It is preferred that: other three kinds of alloying element Ti-Nb-Mo add up to institute's accounting to be 0.0005-0.1%wt in copper alloy layer.
It is preferred that other three kinds of alloying element Ti-Nb-Mo add up to institute's accounting to be 0.005-0.05%wt in copper alloy layer.
It is preferred that Ti:Nb:Mo=10-30:1-2:39-100 in copper alloy layer, more preferable 10:1:39.
It is preferred that, it is characterised in that include the following steps: to carry out untreated copper foil into plating, plating solution is conventional sulfuric acid copper electricity
Solve liquid, wherein in the compound containing Ti, Nb, Mo, add up to 0.01-5g/L.
It is preferred that the titanium source is titanyl sulfate, butyl titanate, metatitanic acid, titanium tetrachloride, titanium trichloride, preferably tetrachloro
Change titanium and titanyl sulfate；For molybdenum from molybdic acid, sodium molybdate, potassium molybdate, ammonium molybdate etc., the source Nb is niobium oxalate.
It is preferred that: further include on the alloy-layer copper coating or nickel coating or zinc coating or in which the knot of any one
It closes.
It is preferred that: the peel strength of prepared copper foil is 2.0-2.5kg/cm.
It is preferred that: the concentration that electrodeposit liquid contains copper sulphate is 70-80g/L, sulfuric acid concentration 110-150g/L, current density
For 25-35A/dm2, electroplating time is 4-8 seconds, with a thickness of 0.25-2.0 μm, preferably 0.5-1.0 μm.
The present invention has the following obvious advantages compared with prior art:
1, what the prior art used roughened layer particle is all subsequent curing process, and is not carried out to roughened layer particle itself
It improves, and the binding force of roughened layer particle itself improves to be only and effectively solves picking phenomenon, although subsequent cure is to a certain degree
On can improve, effect is limited after all.The application is creative to be proposed using new roughened layer particle multicomponent alloy electrolysis slightly
Change mode, effective solution electrolytic copper foil lose powder phenomenon.
Although 2, the prior art is related to preventing the roughening electrolyte improved technology of picking once in a while, especially with regard to Cu-Co-Ni
The improvement of ternary alloy three-partalloy, but its whole peel strength is lower, is unfavorable for subsequent handling processing.
3, new alloy element Ti, Nb, Mo effectively inhibit the growth of dendrite, and roughening ion is more uniform, in conjunction with
Power is secured, especially the introducing of the niobium of ultramicron, due to outermost two layers of its outer shell structure in it is unstable it is abnormal (12,1 or
11,2), it is possible to when it being caused to be co-deposited with Cu it is micro in conjunction with and refine crystal grain, dendrite inhibition.
4, what traditional electro-deposition of niobium was more is in fused salt or ionic liquid, and its object is to obtain more niobium analysis
Out, the application acts in a diametrically opposite way, the content of niobium ultramicron in order to improve roughening ion, and needed for it, use solubility compared with
The water solution system deposition that small and electro-deposition is less susceptible to, it is lucky to realize technical effect, and other electro-deposition have been cooperateed with, make
Mutual cooperation, overcome technology prejudice, broken conventional thought.
5, simultaneously in order to obtain stable metal co-deposition, using the hydride systems and compounding chelated by force
Sodium potassium tartrate tetrahydrate system enables the quaternary alloy layer to be smoothly precipitated, and each component is obtained than meeting expection.
6, other three kinds of alloying element Ti-Nb-Mo add up to institute's accounting to be 0.005-0.05%wt in copper alloy layer, are lower than
Preferable inhibition picking phenomenon cannot be generated when 0.005%, effect increases not significant when being higher than 0.05%, increases urgency instead
Acute cost payout, reduces the competitiveness of product.
Specific embodiment
Embodiment 1:
Plating will be carried out with a thickness of Rz=3.8 μm of roughness of untreated copper foil of 15 microns, face to be processed, plating solution is
Conventional sulfuric acid copper electrolyte, the concentration of copper sulphate are 70g/L, sulfuric acid concentration 110g/L, titanium tetrachloride 1.0g/L, niobium oxalate
0.2g/L, ammonium molybdate 3.5g/L, Cymag 15g/L, sodium potassium tartrate tetrahydrate 8g/L, current density 25A/dm2, electroplating time 8
Second, temperature of electroplating solution is 40 DEG C, with a thickness of 0.5 μm.
Embodiment 2:
Plating will be carried out with a thickness of Rz=3.8 μm of roughness of untreated copper foil of 15 microns, face to be processed, plating solution is
Conventional sulfuric acid copper electrolyte, the concentration of copper sulphate are 80g/L, sulfuric acid concentration 150g/L, titanium tetrachloride 0.6g/L, niobium oxalate
0.12g/L, sodium molybdate 1.8g/L, Cymag 25g/L, sodium potassium tartrate tetrahydrate 12g/L, current density 35A/dm2, electroplating time is
6 seconds, temperature of electroplating solution was 35 DEG C, with a thickness of 1.0 μm.
The conventional subsequent processing of the alloy copper foil layer process of above-mentioned electrolyzing and coarsening (including plating copper coating or nickel on alloy-layer
Coating or zinc coating or in which the combination of any one), thus with resin substrate lamination prepare printed circuit board stacking version simultaneously
It is tested for the property.
Comparative example 1-3:
Contain the sodium molybdate of 0.6g/L, 10g/L cobaltous sulfate in the electrodeposit liquid of comparative example 1；Contain 0.6g/L in comparative example 2
Sodium molybdate, 10g/L nickel sulfate；Sodium molybdate of the comparative example 3 containing 0.6g/L, 10g/L cobaltous sulfate, 10g/L nickel sulfate compare
As a result such as the following table 1:
1 comparative test result of table
* picking evaluation: often flat cm area is observed using visual method under microscope, it is excellent, 3- that nothing or granule number, which are 1-2,
8 to be good, 9-12 are, 13 the above are bad.
From table 1 it follows that can significantly inhibit the roughened layer of electrolytic copper foil after using technical solution of the present invention
Lose powder phenomenon, while obtaining higher peel strength.
Finally, it should be noted that embodiment described above, the only specific embodiment of the application, to illustrate the application
Technical solution, rather than its limitations, the protection scope of the application is not limited thereto, although with reference to the foregoing embodiments to this Shen
It please be described in detail, those skilled in the art should understand that: anyone skilled in the art
Within the technical scope of the present application, it can still modify to technical solution documented by previous embodiment or can be light
It is readily conceivable that variation or equivalent replacement of some of the technical features；And these modifications, variation or replacement, do not make
The essence of corresponding technical solution is detached from the spirit and scope of the embodiment of the present application technical solution.The protection in the application should all be covered
Within the scope of.Therefore, the protection scope of the application should be based on the protection scope of the described claims.
Claims (5)
1. a kind of copper foil for printed circuit board, it is characterised in that: the one side that copper foil is engaged with resin substrate is Cu-Ti-Nb-Mo's
Copper alloy layer, other three kinds of alloying element Ti-Nb-Mo add up to institute's accounting to be 0.0005-2%wt in the copper alloy layer, described
Ti:Nb:Mo=10:1:39 in copper alloy layer, the peel strength of copper foil are 2.0-2.5kg/cm, the copper foil for printed circuit board
The preparation method comprises the following steps: by untreated copper foil carry out plating, form the copper alloy layer of Cu-Ti-Nb-Mo, plating solution is conventional sulfuric acid
Copper electrolyte, wherein the compound containing Ti, Nb, Mo, adds up to 0.01-5g/L, the source Ti is titanyl sulfate, metatitanic acid
Four butyl esters, metatitanic acid, titanium tetrachloride, titanium trichloride, Mo are from molybdic acid, sodium molybdate, potassium molybdate, ammonium molybdate, the source Nb
Niobium oxalate, further include on the alloy-layer copper coating or nickel coating or zinc coating or in which the combination of any one；Electricity is heavy
The concentration that hydrops contains copper sulphate is 70-80g/L, sulfuric acid concentration 110-150g/L, current density 25-35A/dm2, plating
Liquid temperature is 20-40 DEG C, and electroplating time is 4-8 seconds, with a thickness of 0.25-2.0 μm.
2. copper foil for printed circuit board according to claim 1, it is characterised in that: other three kinds of alloy members in copper alloy layer
Plain Ti-Nb-Mo adds up to institute's accounting to be 0.0005-0.1%wt.
3. copper foil for printed circuit board according to claim 1 or 2, which is characterized in that other three kinds of conjunctions in copper alloy layer
Gold element Ti-Nb-Mo adds up to institute's accounting to be 0.005-0.05%wt.
4. copper foil for printed circuit board according to claim 3, it is characterised in that: the source Ti is titanium tetrachloride.
5. copper foil for printed circuit board according to claim 3, it is characterised in that: described with a thickness of 0.5-1.0 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810944963.5A CN109056009B (en) | 2018-08-19 | 2018-08-19 | A kind of copper foil for printed circuit board and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810944963.5A CN109056009B (en) | 2018-08-19 | 2018-08-19 | A kind of copper foil for printed circuit board and preparation method thereof |
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| CN109056009A CN109056009A (en) | 2018-12-21 |
| CN109056009B true CN109056009B (en) | 2019-11-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US10697082B1 (en) * | 2019-08-12 | 2020-06-30 | Chang Chun Petrochemical Co., Ltd. | Surface-treated copper foil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111567A (en) * | 1993-12-28 | 1995-11-15 | 日本电解株式会社 | Copper clad laminate, multilayer printed circuit board and their processing method |
| CN101012520A (en) * | 2007-01-26 | 2007-08-08 | 金龙精密铜管集团股份有限公司 | Niobium micro-alloying copper and copper alloy material |
| CN103958743B (en) * | 2011-11-04 | 2016-12-28 | Jx日矿日石金属株式会社 | Copper foil for printed circuit |
| CN102560584B (en) * | 2012-02-14 | 2014-06-11 | 联合铜箔(惠州)有限公司 | Additive for electrolytic copper foil and surface treatment process of very low profile electrolytic copper foil |
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Effective date of registration: 20191017 Address after: 341000 Xinzhen Industrial Park, Longnan economic and Technological Development Zone, Longnan County, Ganzhou City, Jiangxi Province (Longnan Lingde Industrial Co., Ltd.) Applicant after: Jiangxi weichuangfeng circuit Co., Ltd. Address before: 519031 Room 105-44336, No. 6 Baohua Road, Hengqin New District, Zhuhai City, Guangdong Province Applicant before: Zhuhai Wanshun Rui Tong Technology Co. Ltd. |
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