CN104968155A - Organic composition for forming ultra-thin copper foil release layer and preparation and application thereof - Google Patents
Organic composition for forming ultra-thin copper foil release layer and preparation and application thereof Download PDFInfo
- Publication number
- CN104968155A CN104968155A CN201510299266.5A CN201510299266A CN104968155A CN 104968155 A CN104968155 A CN 104968155A CN 201510299266 A CN201510299266 A CN 201510299266A CN 104968155 A CN104968155 A CN 104968155A
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- Prior art keywords
- copper foil
- thin copper
- organic composite
- peel ply
- extra thin
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Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/007—Manufacture or processing of a substrate for a printed circuit board supported by a temporary or sacrificial carrier
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/022—Processes for manufacturing precursors of printed circuits, i.e. copper-clad substrates
- H05K3/025—Processes for manufacturing precursors of printed circuits, i.e. copper-clad substrates by transfer of thin metal foil formed on a temporary carrier, e.g. peel-apart copper
Abstract
The invention discloses an organic composition for forming an ultra-thin copper foil release layer. The raw materials include deionized water, a phytic acid compound, an alkali solution and a thiadiazole-based compound/thiatriazole-based compound. The mass concentration of the phytic acid compound in the organic composition is 0.01-21g/L, and the mass concentration of the thiadiazole-based compound/thiatriazole-based compound in the organic composition is 0.01-5g/L. The invention is capable of surface adsorption onto a copper foil of a carrier to form a release layer, so that the subsequent electrolytically deposited ultra-thin copper foil can have stable releasability. Compared with benzotriazole, the invention can enable the ultra-thin copper foil to have more stable releasability, have little impact on the conductivity of the electrolytic deposition process, and well solve the contradictions of weak adsorption resulting in difficult release and strong adsorption resulting in poor conductivity. The invention also discloses a preparation method and application method of the above organic composition for forming the ultra-thin copper foil release layer.
Description
Technical field
The present invention relates to Copper Foil peeled film technology field, particularly relate to a kind of organic composite for the formation of extra thin copper foil peel ply and Synthesis and applications.
Background technology
Along with electronic product Highgrade integration, miniaturized development, as the peelable Copper Foil of carrier supported of the main raw material(s) of printed circuit board (PCB) (PCB) also towards more and more thinner future development.The carrier extra thin copper foil also more difficult preparation along with thickness is thinner of less than 12 μm, so extra thin copper foil is by the focus of the emphasis and the market demand that become electrolytic copper foil technical research from now on.
Copper Foil is thinner, prepares more difficult, and is easy to wrinkling in transportation and tears, and therefore prepares ultra-thin, requires also high to technology content.At home and abroad, the conventional fabrication method of extra thin copper foil adopts certain thickness foils as negative electrode, first form peel ply thereon, then acid copper, heavy copper mode mainly contains three kinds: cyanide acid copper, pyrophosphate acid copper and sulfate acid copper.After electro-deposition by the extra thin copper foil plated together with negative electrode foils together through hot pressing, be solidificated on dielectric panel, then will be used as negative electrode metallic support paper tinsel chemistry or mechanical means peel off remove.
Preparing in extra thin copper foil process, peel ply is very important, and peel ply is mainly divided into: inorganic peel ply, organic peel ply and compound peel ply, and inorganic peel ply is mainly metal level or alloy-layer; Organic peel ply is nitrogen-containing compound, sulfur-containing compound and carboxylic acid etc., often select BTA (BTA) and carboxyl benzotriazole (CBTA) etc., and organic peel ply often poorly conductive, cause occurring that Adsorption of Organic is difficult to peel off less, adsorb the drawback that many conductivity is bad; Compound peel ply often selects organic layer as peel ply together with alloy-layer, and wherein contain rare earth metal in alloy-layer, price is higher.
Along with the development of electronic product, the demand of extra thin copper foil is increasing, and therefore a kind of preparation method of cheap and enough thin extra thin copper foil is badly in need of research.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of organic composite for the formation of extra thin copper foil peel ply and Synthesis and applications, select rippability to stablize and the little organic composite of Conductivity as delamination agent, prepare extra thin copper foil, to overcome the drawback of poorly conductive, can avoid occurring that Adsorption of Organic is difficult to peel off less, the phenomenon that the many conductivity of Adsorption of Organic is bad.
A kind of organic composite that can form extra thin copper foil peel ply that the present invention proposes, its raw material comprises deionized water, phytic acid compounds, strong base solution, thiadiazole compound/thiatriazole compounds; Wherein, the mass concentration of phytic acid compounds in organic composite is 0.01-21g/L, and the thiadiazole compound/mass concentration of thiatriazole compounds in organic composite is 0.01-5g/L.
Wherein, the implication of thiadiazole compound/thiatriazole compounds is: thiadiazole compound or thiatriazole compounds.
In embodiment, the mass concentration of phytic acid compounds in organic composite can be 0.01g/L, 0.02g/L, 0.04g/L, 0.06g/L, 0.08g/L, 0.1g/L, 0.2g/L, 0.22g/L, 0.4g/L, 0.53g/L, 0.6g/L, 0.72g/L, 0.8g/L, 0.97g/L, 1g/L, 1.6g/L, 2g/L, 2.5g/L, 3g/L, 3.2g/L, 4g/L, 4.4g/L, 5g/L, 5.5g/L, 6g/L, 6.3g/L, 7g/L, 7.6g/L, 8g/L, 8.5g/L, 9g/L, 9.1g/L, 10g/L, 10.6g/L, 11g/L, 11.3g/L, 12g/L, 12.8g/L, 13g/L, 13.5g/L, 14g/L, 14.8g/L, 15g/L, 15.2g/L, 16g/L, 16.4g/L, 17g/L, 17.6g/L, 18g/L, 18.7g/L, 19g/L, 19.3g/L, 20g/L, 21g/L, the mass concentration of thiadiazole compound/thiatriazole compounds can be 0.01g/L, 0.02g/L, 0.04g/L, 0.06g/L, 0.08g/L, 0.1g/L, 0.15g/L, 0.2g/L, 0.22g/L, 0.4g/L, 0.53g/L, 0.6g/L, 0.72g/L, 0.8g/L, 0.97g/L, 1g/L, 1.6g/L, 2g/L, 2.5g/L, 3g/L, 3.2g/L, 4g/L, 4.4g/L, 5g/L.
Preferably, phytic acid compounds is phytic acid or phytate.
Preferably, the pH value of described organic composite is 4-10.
In embodiment, the pH value of organic composite can be 4,5,6,7,8,9,10.
Preferably, thiadiazole compound is for containing 1-2 substituent 2,1,3-diazosulfides, containing 1-2 substituent 1,2,3-thiadiazoles or contain 1-2 substituent 1,3,4-thiadiazoles, and wherein substituting group is hydrogen, sulfydryl, amino or methyl.
Preferably, thiatriazole compounds is for containing 1-2 substituent 1,3,4-thiatriazole, and wherein substituting group is hydrogen, sulfydryl, amino or methyl.
Preferably, strong base solution is sodium hydroxide solution or potassium hydroxide solution.
The above-mentioned preparation method that can form the organic composite of extra thin copper foil peel ply that the present invention also proposes, phytic acid compounds is added in deionized water, drip strong base solution and regulate pH, then add thiadiazole compound/thiatriazole compounds and mix the organic composite obtaining forming extra thin copper foil peel ply.
Preferably, drip strong base solution and regulate pH to 4-10.
In embodiment, pH can be 4,5,6,7,8,9,10.
The above-mentioned application process that can form the organic composite of extra thin copper foil peel ply that the present invention also proposes, impurity is removed in carrier copper foil cleaning, again with acid solution cleaning carrier copper foil surface removal oxide-film, in described organic composite, then soak 5-60s form peel ply.
At the extra thin copper foil that the carrier copper foil By Electrolysis deposit thickness containing peel ply is 5-12 μm, electrolytic parameter is as follows: Cu
2+concentration: 20-21g/L; Sulfuric acid concentration: 100-110g/L; Solution temperature: 50-60 DEG C; Current density: 4-5A/dm
2; Processing time: 100-700s.
After being peeled off by carrier copper foil, stay the organic composite film on extra thin copper foil, as corrosion inhibiter, stop the oxidation of Copper Foil, and this organic composite can also be soluble in organic solvent, harmful effect can not be produced to the production process of printed circuit board (PCB).
The beneficial effect of the inventive method is: said composition is after formation peel ply, there is good conductivity, solve delamination agent absorption to cause less being difficult to peel off, absorption causes poorly conductive more, thus affect the drawback of subsequent electrodeposition step, simultaneously relative to organic-alloy compound peel ply, technique is simple, and cost is lower.
The extra thin copper foil that the present invention obtains still can intactly be peeled off from carrier easily under the only thickness of 5 μm, and deposition surface is smooth.Relative to various inorganic with have a layer compound peel ply, technique is simpler, is more suitable for industrialization promotion, meets the requirement of the graph thinning of printed circuit board (PCB), densification, thin layer and high reliability better.
Embodiment
As Figure 1-3, Fig. 1 is the shape appearance figure of extra thin copper foil under ESEM that embodiment 4 obtains; A kind of organic composite that can form extra thin copper foil peel ply that Fig. 2 is that the present invention proposes is at Na
2sO
4the impedance scan figure of each concentration in solution; Fig. 3 is that BTA is at Na
2sO
4the impedance scan figure of each concentration in solution.
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
A kind of organic composite that can form extra thin copper foil peel ply that the present invention proposes, its raw material comprises deionized water, sodium phytate, 1,3,4-thiatriazole and sodium hydroxide solution; Wherein, the mass concentration of sodium phytate in organic composite is the mass concentration of 5g/L, 1,3,4-thiatriazole in organic composite is 3g/L, and the pH value of organic composite is 4.
Embodiment 2
A kind of organic composite that can form extra thin copper foil peel ply that the present invention proposes, its raw material comprises deionized water, POTASSIUM PHYTATE, 2,1,3-diazosulfides and potassium hydroxide solution; Wherein, the mass concentration of POTASSIUM PHYTATE in organic composite is the mass concentration of 18g/L, 2,1,3-diazosulfide in organic composite is 0.5g/L, and the pH value of organic composite is 10.
Embodiment 3
A kind of organic composite that can form extra thin copper foil peel ply that the present invention proposes, its raw material comprises deionized water, phytic acid, sulfhydryl amino thiadiazoles and sodium hydroxide solution; Wherein, the mass concentration of phytic acid in organic composite is 7g/L, and the mass concentration of sulfhydryl amino thiadiazoles in organic composite is 1g/L.
The above-mentioned preparation method that can form the organic composite of extra thin copper foil peel ply that the present invention also proposes, phytic acid compounds is added in deionized water, drip strong base solution and regulate pH to 10, then add thiadiazole compound/thiatriazole compounds and mix the organic composite obtaining forming extra thin copper foil peel ply.
Embodiment 4
The present invention adopts thickness to be 35 μm, has the Copper Foil of matsurface (i.e. dull surface) and shiny surface (i.e. wet look) as carrier copper foil, wherein with the wet look of carrier copper foil for electrode surface.
Carrier copper foil is soaked in acetone 120s and remove the impurity such as oil stain, by washed with de-ionized water, then to be placed in mass concentration be that the dilute sulfuric acid of 98g/L cleans 200s and removes the oxide on surface and other impurity to guarantee clean surface, obtains carrier copper foil after pickling;
Carrier copper foil deionized water after pickling is carried out rinsing, in the organic composite then carrier copper foil immersion embodiment 3 after pickling obtained, soaks the carrier copper foil that 30s obtains containing organic peel ply.
Embodiment 5
The carrier copper foil containing organic peel ply embodiment 4 obtained is placed in copper-bath and carries out cathode electrodeposition, then the extra thin copper foil that carrier copper foil obtains containing organic peel ply is peeled off, wherein copper-bath contains the sulfuric acid of 21g/L copper ion and 110g/L, electrodeposition temperature is 55 DEG C, and electrodeposition time is 600s.
Current density is wherein selected to be 3A/dm successively
2, 4A/dm
2, 5A/dm
2, 6A/dm
2carry out electro-deposition, extra thin copper foil is examined under a microscope, known 4-5A/dm
2the surface evenness of lower deposition is best, and prepared Copper Foil is all easy to complete stripping.
Embodiment 6
The carrier copper foil containing organic peel ply embodiment 4 obtained is placed in copper-bath and carries out cathode electrodeposition, then the extra thin copper foil that carrier copper foil obtains containing organic peel ply is peeled off, wherein copper-bath contains the sulfuric acid of 21g/L copper ion and 110g/L, and electro-deposition current density is 4A/dm
2, electrodeposition time is 600s.
Wherein electrodeposition temperature selects 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C successively, and extra thin copper foil is examined under a microscope, and at known 55-60 DEG C, the surface evenness of deposition is best.Prepared Copper Foil is all easy to complete stripping.
Embodiment 7
The carrier copper foil containing organic peel ply embodiment 4 obtained is placed in copper-bath and carries out cathode electrodeposition, then the extra thin copper foil that carrier copper foil obtains containing organic peel ply is peeled off, wherein copper-bath contains the sulfuric acid of 21g/L copper ion and 110g/L, electrodeposition temperature is 55 DEG C, and electro-deposition current density is 4A/dm
2.
Wherein electrodeposition time is followed successively by 400s, 500s, 600s, 700s.With the thickness of miking extra thin copper foil, corresponding copper thickness is listed as follows shown in table.Examined under a microscope by extra thin copper foil, known current density elects 4A/cm as
2, temperature is 55 DEG C, and the surface evenness under different sedimentation time is all good, and prepared Copper Foil is all easy to complete stripping.
| t/s | 400 | 500 | 600 | 700 |
| d/μm | 6 | 7 | 10 | 11 |
Embodiment 8
The carrier copper foil containing organic peel ply embodiment 4 obtained is placed in copper-bath and carries out cathode electrodeposition, then the extra thin copper foil that carrier copper foil obtains containing organic peel ply is peeled off, wherein copper-bath contains the sulfuric acid of 21g/L copper ion and 110g/L, electrodeposition temperature is 55 DEG C, and electro-deposition current density is 4A/dm
2, electrodeposition time is 600s.
With ESEM scanning extra thin copper foil surface topography, as shown in Figure 1, visible copper particle, with layer growth, forms smooth surface to the pattern of extra thin copper foil under ESEM.
Embodiment 9
For comparing the conductivity of the present invention and other organic stripper, so carry out Tafel curved scanning and ac impedance spectroscopy (EIS) scanning to it, compare the two conductivity by ac impedance spectroscopy.Other organic stripper select BTA (BTA).
Electrolyte is the Na of 0.5mol/L
2sO
4solution, add organic composite or BTA (BTA) wherein, the concentration of organic composite or BTA (BTA) is respectively 0.25g/L, 0.5g/L, 0.75g/L, 1.0g/L.Tafel curved scanning potential range is 0.15 to-0.05V, sweep speed for 5mV/s, time of repose is 10s, obtain the corrosion potential of each electrolyte, the ac impedance spectroscopy (EIS) of solution is scanned afterwards under the corrosion potential of correspondence, range of scanned frequencies is 0.1-100KHz, and time of repose is 20s.
The ac impedance spectroscopy of organic composite and BTA as shown in Figures 2 and 3.From Fig. 2 and Fig. 3, the impedance of organic composite is much less than BTA (BTA), and this illustrates that its conductivity is fine.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of extra thin copper foil under ESEM that embodiment 4 obtains.
A kind of organic composite that can form extra thin copper foil peel ply that Fig. 2 is that the present invention proposes is at Na
2sO
4the impedance scan figure of each concentration in solution.
Fig. 3 is that BTA is at Na
2sO
4the impedance scan figure of each concentration in solution.
Claims (9)
1. can form an organic composite for extra thin copper foil peel ply, it is characterized in that, its raw material comprises deionized water, phytic acid compounds, strong base solution, thiadiazole compound/thiatriazole compounds; Wherein, the mass concentration of phytic acid compounds in organic composite is 0.01-21g/L, and the thiadiazole compound/mass concentration of thiatriazole compounds in organic composite is 0.01-5g/L.
2. can form the organic composite of extra thin copper foil peel ply according to claim 1, it is characterized in that, phytic acid compounds is phytic acid or phytate.
3. can form the organic composite of extra thin copper foil peel ply according to claim 1 or 2, it is characterized in that, the pH value of described organic composite is 4-10.
4. can form the organic composite of extra thin copper foil peel ply according to claim 3, it is characterized in that, thiadiazole compound is for containing 1-2 individual substituent 2,1,3-diazosulfide, containing 1-2 substituent 1,2,3-thiadiazoles or containing 1-2 substituent 1,3,4-thiadiazoles, wherein substituting group is hydrogen, sulfydryl, amino or methyl.
5. can form the organic composite of extra thin copper foil peel ply according to claim 3 or 4, it is characterized in that, thiatriazole compounds is for containing 1-2 substituent 1,3,4-thiatriazole, and wherein substituting group is hydrogen, sulfydryl, amino or methyl.
6. can form the organic composite of extra thin copper foil peel ply according to any one of claim 1-5, it is characterized in that, strong base solution is sodium hydroxide solution or potassium hydroxide solution.
7. one kind can form the preparation method of the organic composite of extra thin copper foil peel ply as described in any one of claim 1-6, it is characterized in that, phytic acid compounds is added in deionized water, drip strong base solution and regulate pH, then add thiadiazole compound/thiatriazole compounds and mix the organic composite obtaining forming extra thin copper foil peel ply.
8. can form the preparation method of the organic composite of extra thin copper foil peel ply according to claim 7, it is characterized in that, drip strong base solution and regulate pH to 4-10.
9. one kind can form the organic composite of extra thin copper foil peel ply as described in any one of claim 1-6, it is characterized in that, impurity is removed in carrier copper foil cleaning, then with acid solution cleaning carrier copper foil surface removal oxide-film, in described organic composite, then soaks 5-60s form peel ply.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510299266.5A CN104968155B (en) | 2015-06-03 | 2015-06-03 | A kind of organic composite and preparation and application for being used to form extra thin copper foil peel ply |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510299266.5A CN104968155B (en) | 2015-06-03 | 2015-06-03 | A kind of organic composite and preparation and application for being used to form extra thin copper foil peel ply |
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| CN104968155B CN104968155B (en) | 2018-01-02 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112853408A (en) * | 2020-12-31 | 2021-05-28 | 江西理工大学 | Preparation method of ultrathin carrier-attached copper foil easy to peel and pure in interface |
| CN114672855A (en) * | 2022-03-29 | 2022-06-28 | 电子科技大学 | Preparation method of ultrathin copper foil |
| CN115058711A (en) * | 2022-06-17 | 2022-09-16 | 山东大学 | Preparation method of easy-to-peel ultrathin carrier copper foil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112853408A (en) * | 2020-12-31 | 2021-05-28 | 江西理工大学 | Preparation method of ultrathin carrier-attached copper foil easy to peel and pure in interface |
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| CN114672855B (en) * | 2022-03-29 | 2023-09-26 | 电子科技大学 | Preparation method of ultrathin copper foil |
| CN115058711A (en) * | 2022-06-17 | 2022-09-16 | 山东大学 | Preparation method of easy-to-peel ultrathin carrier copper foil |
| CN115058711B (en) * | 2022-06-17 | 2022-12-27 | 山东大学 | Preparation method of easily-stripped ultrathin carrier copper foil |
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