CN116641018A - Extra thin copper foil with carrier and its preparing process - Google Patents
Extra thin copper foil with carrier and its preparing process Download PDFInfo
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- CN116641018A CN116641018A CN202310552455.3A CN202310552455A CN116641018A CN 116641018 A CN116641018 A CN 116641018A CN 202310552455 A CN202310552455 A CN 202310552455A CN 116641018 A CN116641018 A CN 116641018A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 238000000034 method Methods 0.000 title claims abstract description 75
- 239000011889 copper foil Substances 0.000 title claims abstract description 65
- 230000008569 process Effects 0.000 title description 12
- 239000010410 layer Substances 0.000 claims abstract description 215
- 239000010949 copper Substances 0.000 claims abstract description 82
- 229910052802 copper Inorganic materials 0.000 claims abstract description 79
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000009713 electroplating Methods 0.000 claims abstract description 43
- 230000004888 barrier function Effects 0.000 claims abstract description 42
- 239000011248 coating agent Substances 0.000 claims abstract description 37
- 238000000576 coating method Methods 0.000 claims abstract description 37
- 239000011888 foil Substances 0.000 claims abstract description 31
- 230000008719 thickening Effects 0.000 claims abstract description 30
- 229910052786 argon Inorganic materials 0.000 claims abstract description 27
- 238000005516 engineering process Methods 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 238000001771 vacuum deposition Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000004381 surface treatment Methods 0.000 claims abstract description 13
- 239000002335 surface treatment layer Substances 0.000 claims abstract description 11
- 238000004544 sputter deposition Methods 0.000 claims abstract description 10
- 238000000151 deposition Methods 0.000 claims abstract description 7
- 238000010849 ion bombardment Methods 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims description 27
- 230000000903 blocking effect Effects 0.000 claims description 21
- 239000013077 target material Substances 0.000 claims description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 16
- 238000005546 reactive sputtering Methods 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 5
- 238000004070 electrodeposition Methods 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 3
- 238000003490 calendering Methods 0.000 claims description 3
- 238000007747 plating Methods 0.000 description 31
- 150000002500 ions Chemical class 0.000 description 29
- 239000002253 acid Substances 0.000 description 15
- 238000000926 separation method Methods 0.000 description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 12
- 238000004380 ashing Methods 0.000 description 9
- 238000007788 roughening Methods 0.000 description 9
- 238000002161 passivation Methods 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 6
- 229910000365 copper sulfate Inorganic materials 0.000 description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical group [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 6
- PEVJCYPAFCUXEZ-UHFFFAOYSA-J dicopper;phosphonato phosphate Chemical group [Cu+2].[Cu+2].[O-]P([O-])(=O)OP([O-])([O-])=O PEVJCYPAFCUXEZ-UHFFFAOYSA-J 0.000 description 6
- 238000004806 packaging method and process Methods 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 6
- 229910000077 silane Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 6
- 238000004804 winding Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005240 physical vapour deposition Methods 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 239000002346 layers by function Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000306 component Substances 0.000 description 3
- -1 copper metals Chemical class 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003780 insertion Methods 0.000 description 3
- 230000037431 insertion Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses an extra-thin copper foil with a carrier and a preparation method thereof, wherein the method comprises the following steps: s1, carrying out ion bombardment on the surface of a carrier foil by utilizing an ion source under argon to obtain a carrier layer; the surface of the carrier layer is clean and uniform; s2, forming a compact barrier/stripping layer on the surface of the carrier layer by utilizing a sputtering coating technology, wherein the barrier/stripping layer has a barrier layer function and a stripping layer function; s3, depositing copper metal on the barrier/stripping layer by utilizing a vacuum coating technology to obtain a seed copper layer; s4, electroplating a thickening layer on the surface of the seed copper layer by utilizing an electroplating technology to obtain a pretreated copper foil; the thickness of the thickening layer is the target thickness; s5, carrying out surface treatment on the pretreated copper foil to form a surface treatment layer, and obtaining the extra-thin copper foil with the carrier. The barrier/stripping layer has the functions of a barrier layer and a stripping layer, and realizes that the separating force of the carrier layer and the ultrathin copper layer is stable and controllable within a certain range.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to an extra-thin copper foil with a carrier and a preparation method thereof.
Background
Printed Circuit Boards (PCBs) are important core components of products such as 5G technology, automotive electronics, consumer electronics, etc., and with the rapid development of the market, electronic products are rapidly advancing toward high integration, miniaturization, convenience and multifunctionality, and copper foil as a main material of PCBs must be thinner and thinner following the trend of the times. The ultra-fine circuit is the key of miniaturization of electronic products, and the line width and line distance are required to be lower than 50 mu m, so that the traditional circuit etching method is difficult to realize and only the latest improved semi-addition method can be used. The improved semi-additive method requires that the copper foil is an extremely thin copper foil, the thickness of the copper foil is generally not more than 5 mu m, the thinner the copper foil is, the more difficult the preparation, transportation and application of the copper foil are, and the copper foil with a carrier is produced to solve the problem. The ultra-thin copper layer is deposited on the carrier layer, the carrier layer can be some metal foil or high polymer, etc., after hot pressing and solidification on the insulating plate, the carrier layer is separated out, and the ultra-thin copper layer is left. The preparation of the intermediate stripping layer and the barrier layer has the main difficulty that after high-temperature hot pressing, the bonding force between the intermediate stripping layer and the barrier layer can not be too large or too small when the carrier layer and the ultrathin copper layer are separated, so that the carrier layer and the ultrathin copper layer are ensured to be well separated, and various problems can occur in the production and processing process of the copper-clad plate. Currently, the preparation methods of the stripping layer in the industry are mainly divided into two types, namely an electrochemical deposition method and a physical vapor deposition (Physical Vapor Deposition, PVD) method.
The physical vapor deposition technology is a preparation method for finally forming a film layer by adopting physical forms such as evaporation or sputtering and the like to convert a material source (solid or liquid) into a vapor phase substance in an atomic, molecular or ionic state under a vacuum condition so that the vapor phase substance carries energy and is deposited on the surface of a workpiece. The physical vapor deposition method is favored by virtue of the advantages of environmental protection, high precision and the like, and in the production process of the extra thin copper foil with the carrier, the stripping layer and the blocking layer are mostly prepared by adopting a simple substance or alloy mode of magnetron sputtering Ni/Mo/Co/Cr/Fe/Ti/W/Zn at present. On one hand, after the carrier layer is separated from the ultrathin copper layer, other non-copper metals remain on a separation interface, so that the yield of a downstream fine circuit preparation working section is affected; on the other hand, the introduction of non-copper metal increases the transmission loss of the electrical signal after fine line etching.
Disclosure of Invention
The invention provides an extra-thin copper foil with a carrier and a preparation method thereof, which can solve the problem of introducing other non-copper metals when preparing a stripping layer and a barrier layer.
In one aspect, the invention provides a method for preparing an extra thin copper foil with a carrier, which comprises the following steps:
s1, carrying out ion bombardment on the surface of a carrier foil by utilizing an ion source under argon to obtain a carrier layer; the surface of the carrier layer is clean and uniform;
s2, forming a compact barrier/stripping layer on the surface of the carrier layer by utilizing a sputtering coating technology, wherein the barrier/stripping layer has a barrier layer function and a stripping layer function;
s3, depositing copper metal on the barrier/stripping layer by utilizing a vacuum coating technology to obtain a seed copper layer;
s4, electroplating a thickening layer on the surface of the seed copper layer by utilizing an electroplating technology to obtain a pretreated copper foil; the thickness of the thickening layer is the target thickness;
s5, carrying out surface treatment on the pretreated copper foil to form a surface treatment layer, and obtaining the extra-thin copper foil with the carrier.
Optionally, the step S1 includes:
preparing a carrier foil by an electrochemical deposition method or a calendaring annealing method;
and carrying out ion bombardment on the surface to be treated of the carrier foil material under argon by an ion source to obtain a carrier layer with a clean and uniform surface.
Optionally, the carrier foil is an HTE green foil, an RTF green foil or an HVLP green foil.
Optionally, the carrier foil has a thickness of 12-35 μm.
Optionally, the Rz roughness of the surface to be treated in the carrier foil is 0.2-2.0 μm and the Ra roughness is 0.05-0.30 μm.
Optionally, the step S2 includes:
forming a compact blocking/stripping layer on the surface of the carrier layer by using an intermediate frequency magnetron alternating current reactive sputtering coating technology; the thickness of the blocking/stripping layer is 5-50nm.
Optionally, the medium-frequency magnetron alternating-current reactive sputtering coating technology comprises the following steps:
filling argon with purity higher than 99.99% into the cavity at a flow rate of 100-300 sccm;
filling oxygen with purity higher than 99.99% into the cavity at a flow rate of 20-120 sccm;
the copper target is used as a target material, and the coating power is 1-5KW.
Optionally, the step S3 includes:
depositing copper metal on the barrier/stripping layer by using a direct current magnetron sputtering vacuum coating technology to obtain a seed copper layer; the thickness of the seed copper layer is 5-200nm.
Optionally, the direct current magnetron sputtering vacuum coating technology comprises the following steps:
filling argon with purity higher than 99.99% into the cavity at a flow rate of 100-300 sccm;
the copper target is used as a target material, and the coating power is 5-20KW.
Optionally, the electroplating technology in the step S4 includes an acid method electroplating thickening method, an alkali method electroplating thickening method or an alkali-acid composite electroplating method; the thickness of the thickening layer is 1-7 mu m.
Optionally, the surface treatment in the step S5 includes at least one of roughening, curing, blackening, ashing, passivation, and coating with a coupling agent.
Optionally, the ion source in the step S1 is at least one of an anode layer ion source, a hall ion source, a kofuman ion source, and an ICP ion source; the power of the ion source is 1-10KW, and the treatment time is 1-30min.
On the other hand, the invention provides an extra-thin copper foil with a carrier, which comprises a carrier layer, a blocking/stripping layer, a seed copper layer, a thickening layer and a surface treatment layer.
In an exemplary embodiment, the thickness of the barrier/release layer is 5-50nm.
In an exemplary embodiment, the seed copper layer has a thickness of 5-200nm.
In an exemplary embodiment, the thickening layer has a thickness of 1-7 μm.
The extra-thin copper foil with the carrier and the preparation method thereof provided by the invention have the following technical effects:
1. the invention provides a method for preparing a barrier/stripping layer (Cu) by adopting magnetron intermediate frequency alternating current reactive sputtering plating x O y ) The barrier/release layer has a barrier function and a release layer function, and can serve as both a release layer and a barrier layer; the thickness and the components of the film layer can be regulated and controlled by the sputtering power and oxygen filling amount of the target material, so that the separation force of the carrier layer and the ultrathin copper layer is stable and controllable in a certain range;
2. in the invention, when the stripping/blocking layer is prepared, no other non-copper metal is introduced, so that the transmission loss of the electric signal after the etching of the fine circuit is greatly reduced.
3. The stripping/blocking layer and the seed layer are prepared by a vacuum coating method, and each functional layer has good film continuity and higher thickness consistency; the preparation method of the invention is green and environment-friendly and has no pollution.
Drawings
In order to more clearly illustrate the embodiments of the present description or the technical solutions and advantages of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort to a person skilled in the art.
Fig. 1 is a schematic flow chart of a method for preparing an extra thin copper foil with carrier according to an embodiment of the present disclosure;
fig. 2 is a schematic structural view of an extra thin copper foil with carrier according to an embodiment of the present disclosure;
FIG. 3 is a schematic diagram illustrating an example of a separation of a carrier layer from an ultrathin copper layer according to an embodiment of the disclosure;
fig. 4 is a schematic diagram illustrating an example two of a separation manner of a carrier layer and an ultrathin copper layer according to an embodiment of the present disclosure.
Wherein, the reference numerals in the figures correspond to:
1-carrier layer, 2-blocking/stripping layer, 3-seed copper layer, 4-thickening layer and 5-surface treatment layer.
Detailed Description
The technical solutions of the embodiments of the present specification will be clearly and completely described below with reference to the drawings of the embodiments of the present specification, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It is noted that the terms "comprises" and "comprising," and any variations thereof, in the description and claims of the present invention and in the foregoing figures, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or server comprising a list of steps or elements is not necessarily limited to those steps or elements expressly listed or inherent to such process, method, article, or apparatus.
In the following, a method for manufacturing an extra thin copper foil with carrier according to the present invention is described, and fig. 1 is a schematic flow chart of a method for manufacturing an extra thin copper foil with carrier according to an embodiment of the present invention, and the present invention provides the steps of the method according to the embodiment or the flow chart, but may include more or less steps based on conventional or non-inventive labor. The order of steps recited in the embodiments is merely one way of performing the order of steps and does not represent a unique order of execution. When implemented in a real system or server product, the methods illustrated in the embodiments or figures may be performed sequentially or in parallel (e.g., in a parallel processor or multithreaded environment). As shown in fig. 1, the method may include:
s1, carrying out ion bombardment on the surface of a carrier foil by utilizing an ion source under argon to obtain a carrier layer; the surface of the carrier layer is clean and uniform; the pretreatment effect of the carrier foil can be regulated and controlled by adjusting the power, the treatment time and the argon inflation amount of the ion source, so that the surface of the carrier foil is clean and uniform.
S2, forming a compact barrier/stripping layer on the surface of the carrier layer by utilizing a sputtering coating technology, wherein the barrier/stripping layer has a barrier layer function and a stripping layer function; the thickness and the components of the functional layer can be regulated and controlled by adjusting the coating power, time, oxygen aeration quantity and the like. Wherein the barrier/release layer is a metallic copper oxide layer (Cu x O y )。
S3, depositing copper metal on the barrier/stripping layer by utilizing a vacuum coating technology to obtain a seed copper layer; thereby facilitating the implementation of the subsequent electroplating thickening working section and regulating and controlling the thickness of the functional layer by adjusting the coating power, time, argon inflation amount and the like.
S4, electroplating a thickening layer on the surface of the seed copper layer by utilizing an electroplating technology to obtain a pretreated copper foil; the thickness of the thickening layer is the target thickness; the product in the step S3 can be transferred to an electroplating thickening machine, and thickened to the target thickness by adjusting the current density and the running speed.
S5, carrying out surface treatment on the pretreated copper foil to form a surface treatment layer, and obtaining the extra-thin copper foil with the carrier. The surface treatment can comprise the steps of roughening, curing, blackening, ashing, passivating, coating with a coupling agent and the like, so that the performances of oxidation resistance, chemical resistance, peeling strength and the like of the copper foil can meet the target requirements, and finally the extra thin copper foil with the carrier can be obtained.
In an exemplary embodiment, the step S1 includes:
preparing a carrier foil by an electrochemical deposition method or a calendaring annealing method;
and carrying out ion bombardment on the surface to be treated of the carrier foil material under argon by an ion source to obtain a carrier layer with a clean and uniform surface.
In an exemplary embodiment, the carrier foil is an HTE green foil, an RTF green foil, or an HVLP green foil.
In an exemplary embodiment, the carrier foil has a thickness of 12-35 μm.
In an exemplary embodiment, the Rz roughness of the surface to be treated in the carrier foil is 0.2-2.0 μm and the Ra roughness is 0.05-0.30 μm.
In an exemplary embodiment, the ion source in the step S1 is at least one of an anode layer ion source, a hall ion source, a kaufman ion source, and an ICP ion source; the power of the ion source is 1-10KW, and the treatment time is 1-30min.
In an exemplary embodiment, the step S2 includes:
forming a compact blocking/stripping layer on the surface of the carrier layer by using an intermediate frequency magnetron alternating current reactive sputtering coating technology; the thickness of the blocking/stripping layer is 5-50nm.
In an exemplary embodiment, the medium frequency magnetron ac reactive sputter coating technique includes:
filling argon with purity higher than 99.99% into the cavity at a flow rate of 100-300 sccm;
filling oxygen with purity higher than 99.99% into the cavity at a flow rate of 20-120 sccm;
the copper target is used as a target material, and the coating power is 1-5KW.
In an exemplary embodiment, the step S3 includes:
depositing copper metal on the barrier/stripping layer by using a direct current magnetron sputtering vacuum coating technology to obtain a seed copper layer; the thickness of the seed copper layer is 5-200nm.
In an exemplary embodiment, the dc magnetron sputtering vacuum coating technique includes:
filling argon with purity higher than 99.99% into the cavity at a flow rate of 100-300 sccm;
the copper target is used as a target material, and the coating power is 5-20KW.
In an exemplary embodiment, the electroplating technology in the step S4 includes an acid-process electroplating thickening method, an alkali-process electroplating thickening method or an alkali-acid composite electroplating method; the thickness of the thickening layer is 1-7 mu m.
In an exemplary embodiment, the surface treatment in the step S5 includes at least one of roughening, curing, blackening, ashing, passivation, and coupling agent coating.
On the other hand, the invention provides an extra thin copper foil with a carrier, as shown in figure 2, which comprises a carrier layer 1, a blocking/stripping layer 2, a seed copper layer 3, a thickening layer 4 and a surface treatment layer 5; wherein the carrier layer 1, the barrier/release layer 2, the seed copper layer 3, the thickening layer 4 and the surface treatment layer 5 are sequentially arranged in sequence.
In an exemplary embodiment, the thickness of the barrier/release layer is 5-50nm.
In an exemplary embodiment, the seed copper layer has a thickness of 5-200nm.
In an exemplary embodiment, the thickening layer has a thickness of 1-7 μm.
The present invention will be described in further detail with reference to specific examples.
Example 1
A whole roll of RTF copper foil having a thickness of 18 μm, a smooth Rz roughness of 0.9 μm and an Ra roughness of 0.1 μm was fixed on a winding system in a vacuum coater, and the vehicle speed was set at 3m/min. The ion source is an anode layer ion source, the power is set to be 1.5KW, and the treatment time is known to be 2 minutes according to the vehicle speed; preparing a blocking/stripping layer by adopting an intermediate frequency magnetron alternating current reactive sputtering plating method, wherein the target material is a copper target, the argon filling amount is 170sccm, the oxygen filling amount is 30sccm, the purity is 99.99%, the coating power is 4KW, and the film forming thickness is 20nm; the seed layer is prepared by adopting a direct current magnetron sputtering method, the target material is a copper target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 10KW, and the film forming thickness is 50nm, so that the seed copper layer is obtained.
And placing the whole roll of copper foil subjected to vacuum coating treatment on an electroplating treatment line, electroplating and thickening the surface of a seed copper layer, sequentially passing through an alkaline plating tank, a rinsing tank, an acid plating tank, a rinsing tank, a roughening tank, a curing tank, a rinsing tank, a blackening tank, a rinsing tank, an ashing tank, a rinsing tank, a passivation tank, a rinsing tank, a silane coating tank and an oven, and then carrying out rolling packaging on the copper foil after tension adjustment. Wherein the alkali plating tank is copper pyrophosphate/potassium pyrophosphate electroplating solution, the acid plating tank is copper sulfate/sulfuric acid electroplating solution, the thickness of the metal layer is thickened to 3 mu m, and other specific surface treatment processes are the same as those of the surface of the copper foil for the conventional electronic circuit.
Example 2
A whole roll of RTF copper foil having a thickness of 18 μm, a smooth Rz roughness of 0.9 μm and an Ra roughness of 0.1 μm was fixed on a winding system in a vacuum coater, and the vehicle speed was set at 3m/min. The ion source is an anode layer ion source, the power is set to be 1.5KW, and the treatment time is known to be 2 minutes according to the vehicle speed; preparing a blocking/stripping layer by adopting an intermediate frequency magnetron alternating current reactive sputtering plating method, wherein the target material is a copper target, the argon filling amount is 170sccm, the oxygen filling amount is 70sccm, the purity is 99.99%, the coating power is 3KW, and the film forming thickness is 20nm; the seed layer is prepared by adopting a direct current magnetron sputtering method, the target material is a copper target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 10KW, and the film forming thickness is 50nm, so that the seed copper layer is obtained.
And placing the whole roll of copper foil subjected to vacuum coating treatment on an electroplating treatment line, electroplating and thickening the surface of a seed copper layer, sequentially passing through an alkaline plating tank, a rinsing tank, an acid plating tank, a rinsing tank, a roughening tank, a curing tank, a rinsing tank, a blackening tank, a rinsing tank, an ashing tank, a rinsing tank, a passivation tank, a rinsing tank, a silane coating tank and an oven, and then carrying out rolling packaging on the copper foil after tension adjustment. Wherein the alkali plating tank is copper pyrophosphate/potassium pyrophosphate electroplating solution, the acid plating tank is copper sulfate/sulfuric acid electroplating solution, the thickness of the metal layer is thickened to 3 mu m, and other specific surface treatment processes are the same as those of the surface of the copper foil for the conventional electronic circuit.
Example 3
A whole roll of RTF copper foil having a thickness of 18 μm, a smooth Rz roughness of 0.9 μm and an Ra roughness of 0.1 μm was fixed on a winding system in a vacuum coater, and the vehicle speed was set at 3m/min. The ion source is an anode layer ion source, the power is set to be 1.5KW, and the treatment time is known to be 2 minutes according to the vehicle speed; preparing a blocking/stripping layer by adopting an intermediate frequency magnetron alternating current reactive sputtering plating method, wherein the target material is a copper target, the argon filling amount is 170sccm, the oxygen filling amount is 110sccm, the purity is 99.99%, the coating power is 2KW, and the film forming thickness is 20nm; the seed layer is prepared by adopting a direct current magnetron sputtering method, the target material is a copper target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 10KW, and the film forming thickness is 50nm, so that the seed copper layer is obtained.
And placing the whole roll of copper foil subjected to vacuum coating treatment on an electroplating treatment line, electroplating and thickening the surface of a seed copper layer, sequentially passing through an alkaline plating tank, a rinsing tank, an acid plating tank, a rinsing tank, a roughening tank, a curing tank, a rinsing tank, a blackening tank, a rinsing tank, an ashing tank, a rinsing tank, a passivation tank, a rinsing tank, a silane coating tank and an oven, and then carrying out rolling packaging on the copper foil after tension adjustment. Wherein the alkali plating tank is copper pyrophosphate/potassium pyrophosphate electroplating solution, the acid plating tank is copper sulfate/sulfuric acid electroplating solution, the thickness of the metal layer is thickened to 3 mu m, and other specific surface treatment processes are the same as those of the surface of the copper foil for the conventional electronic circuit.
Comparative example 1
A whole roll of RTF copper foil having a thickness of 18 μm, a smooth Rz roughness of 0.9 μm and an Ra roughness of 0.1 μm was fixed on a winding system in a vacuum coater, and the vehicle speed was set at 3m/min. The ion source is an anode layer ion source, the power is set to be 1.5KW, and the treatment time is known to be 2 minutes according to the vehicle speed; preparing a blocking/stripping layer by adopting a direct current magnetron sputtering method, wherein the target material is a nickel target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 20KW, and the film forming thickness is 20nm; the seed layer is prepared by adopting a direct current magnetron sputtering method, the target material is a copper target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 10KW, and the film forming thickness is 50nm, so that the seed copper layer is obtained.
And placing the whole roll of copper foil subjected to vacuum coating treatment on an electroplating treatment line, electroplating and thickening the surface of a seed copper layer, sequentially passing through an alkaline plating tank, a rinsing tank, an acid plating tank, a rinsing tank, a roughening tank, a curing tank, a rinsing tank, a blackening tank, a rinsing tank, an ashing tank, a rinsing tank, a passivation tank, a rinsing tank, a silane coating tank and an oven, and then carrying out rolling packaging on the copper foil after tension adjustment. Wherein the alkali plating tank is copper pyrophosphate/potassium pyrophosphate electroplating solution, the acid plating tank is copper sulfate/sulfuric acid electroplating solution, the thickness of the metal layer is thickened to 3 mu m, and other specific surface treatment processes are the same as those of the surface of the copper foil for the conventional electronic circuit.
Comparative example 2
A whole roll of RTF copper foil having a thickness of 18 μm, a smooth Rz roughness of 0.9 μm and an Ra roughness of 0.1 μm was fixed on a winding system in a vacuum coater, and the vehicle speed was set at 3m/min. The ion source is an anode layer ion source, the power is set to be 1.5KW, and the treatment time is known to be 2 minutes according to the vehicle speed; preparing a blocking/stripping layer by adopting a direct current magnetron sputtering method, wherein the target material is a nickel target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 15KW, and the film forming thickness is 20nm; the seed layer is prepared by adopting a direct current magnetron sputtering method, the target material is a copper target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 10KW, and the film forming thickness is 50nm, so that the seed copper layer is obtained.
And placing the whole roll of copper foil subjected to vacuum coating treatment on an electroplating treatment line, electroplating and thickening the surface of a seed copper layer, sequentially passing through an alkaline plating tank, a rinsing tank, an acid plating tank, a rinsing tank, a roughening tank, a curing tank, a rinsing tank, a blackening tank, a rinsing tank, an ashing tank, a rinsing tank, a passivation tank, a rinsing tank, a silane coating tank and an oven, and then carrying out rolling packaging on the copper foil after tension adjustment. Wherein the alkali plating tank is copper pyrophosphate/potassium pyrophosphate electroplating solution, the acid plating tank is copper sulfate/sulfuric acid electroplating solution, the thickness of the metal layer is thickened to 3 mu m, and other specific surface treatment processes are the same as those of the surface of the copper foil for the conventional electronic circuit.
Comparative example 3
A whole roll of RTF copper foil having a thickness of 18 μm, a smooth Rz roughness of 0.9 μm and an Ra roughness of 0.1 μm was fixed on a winding system in a vacuum coater, and the vehicle speed was set at 3m/min. The ion source is an anode layer ion source, the power is set to be 1.5KW, and the treatment time is known to be 2 minutes according to the vehicle speed; preparing a blocking/stripping layer by adopting a direct current magnetron sputtering method, wherein the target material is a nickel target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 10KW, and the film forming thickness is 20nm; the seed layer is prepared by adopting a direct current magnetron sputtering method, the target material is a copper target, the argon filling amount is 200sccm, the purity is 99.99%, the coating power is 10KW, and the film forming thickness is 50nm, so that the seed copper layer is obtained.
And placing the whole roll of copper foil subjected to vacuum coating treatment on an electroplating treatment line, electroplating and thickening the surface of a seed copper layer, sequentially passing through an alkaline plating tank, a rinsing tank, an acid plating tank, a rinsing tank, a roughening tank, a curing tank, a rinsing tank, a blackening tank, a rinsing tank, an ashing tank, a rinsing tank, a passivation tank, a rinsing tank, a silane coating tank and an oven, and then carrying out rolling packaging on the copper foil after tension adjustment. Wherein the alkali plating tank is copper pyrophosphate/potassium pyrophosphate electroplating solution, the acid plating tank is copper sulfate/sulfuric acid electroplating solution, the thickness of the metal layer is thickened to 3 mu m, and other specific surface treatment processes are the same as those of the surface of the copper foil for the conventional electronic circuit.
The products obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to a separation force test between a carrier layer and an extremely thin copper layer and an insertion loss test at 5GHz, and the test results obtained are shown in table 1 below.
In the process of testing the separation force of the product, various separation formulas can be adopted; FIG. 3 is a schematic diagram showing an example of a separation of a carrier layer from an ultra-thin copper layer; when separating, separating from the contact surfaces of the barrier/stripping layer 2 and the seed copper layer 3 to obtain a two-part structure, wherein one part comprises the carrier layer 1 and the barrier/stripping layer 2, and the other part comprises the seed copper layer 3, the thickening layer 4 and the surface treatment layer 5;
fig. 4 is a schematic diagram illustrating an example two of a separation manner of a carrier layer and an ultrathin copper layer according to an embodiment of the present disclosure; the separation starts from the contact surface of the carrier layer 1 and the barrier/release layer 2, and a two-part structure is obtained, wherein one part comprises the carrier layer 1, and the other part comprises the barrier/release layer 2, the seed copper layer 3, the thickening layer 4 and the surface treatment layer 5. The test of examples 1 to 3 and comparative examples 1 to 3 were carried out in a separation manner shown in FIG. 4.
TABLE 1
From the experimental results in table 1, it can be seen that when the barrier/release layer is prepared by using the method of magnetron alternating current reactive sputtering plating, the oxygen filling amount is increased, and the separation force between the carrier layer and the ultrathin copper layer is reduced after the sputtering power of the target is reduced. Under the standard test board with the impedance value of 100 omega, the insertion loss is tested by adopting a vector network analyzer, and from the experimental result, the insertion loss at 5GHz is about 2-5% lower on average when the barrier/release layer is prepared without introducing other non-copper metals.
The embodiment of the carrier-attached ultrathin copper foil and the preparation method thereof provided by the invention can realize stable and controllable separation force between the carrier layer and the ultrathin copper layer and reduce transmission loss of electric signals by adopting the method for preparing the blocking/stripping layer through medium-frequency magnetron alternating-current reactive sputtering plating. The method has simple steps and easy operation, can effectively improve the product quality, and has great application value.
The extra-thin copper foil with the carrier and the preparation method thereof provided by the invention have the following technical effects:
1. the invention provides a method for preparing a barrier/stripping layer (Cu) by adopting magnetron intermediate frequency alternating current reactive sputtering plating x O y ) The barrier/release layer has a barrier function and a release layer function, and can serve as both a release layer and a barrier layer; the thickness and the components of the film layer can be regulated and controlled by the sputtering power and oxygen filling amount of the target material, so that the separating force of the carrier layer and the ultrathin copper layer is realized at a certain levelThe range is stable and controllable;
2. in the invention, when the stripping/blocking layer is prepared, no other non-copper metal is introduced, so that the transmission loss of the electric signal after the etching of the fine circuit is greatly reduced.
3. The stripping/blocking layer and the seed layer are prepared by a vacuum coating method, and each functional layer has good film continuity and higher thickness consistency; the preparation method of the invention is green and environment-friendly and has no pollution.
It should be noted that: the embodiment sequence of the present disclosure is only for description, and does not represent the advantages and disadvantages of the embodiments. And the foregoing description has been directed to specific embodiments of this specification. Other embodiments are within the scope of the following claims.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The preparation method of the extra-thin copper foil with the carrier is characterized by comprising the following steps:
s1, carrying out ion bombardment on the surface of a carrier foil by utilizing an ion source under argon to obtain a carrier layer; the surface of the carrier layer is clean and uniform;
s2, forming a compact barrier/stripping layer on the surface of the carrier layer by utilizing a sputtering coating technology, wherein the barrier/stripping layer has a barrier layer function and a stripping layer function;
s3, depositing copper metal on the barrier/stripping layer by utilizing a vacuum coating technology to obtain a seed copper layer;
s4, electroplating a thickening layer on the surface of the seed copper layer by utilizing an electroplating technology to obtain a pretreated copper foil; the thickness of the thickening layer is the target thickness;
s5, carrying out surface treatment on the pretreated copper foil to form a surface treatment layer, and obtaining the extra-thin copper foil with the carrier.
2. The method according to claim 1, wherein the step S1 comprises:
preparing a carrier foil by an electrochemical deposition method or a calendaring annealing method;
and carrying out ion bombardment on the surface to be treated of the carrier foil material under argon by an ion source to obtain a carrier layer with a clean and uniform surface.
3. The method according to claim 2, wherein the carrier foil is HTE green foil, RTF green foil or HVLP green foil.
4. Method according to claim 2, characterized in that the carrier foil has a thickness of 12-35 μm.
5. A method according to claim 2, characterized in that the surface to be treated in the carrier foil has an Rz roughness of 0.2-2.0 μm and an Ra roughness of 0.05-0.30 μm; the ion source is at least one of an anode layer ion source, a Hall ion source, a kofuman ion source and an ICP ion source; the power of the ion source is 1-10KW, and the treatment time is 1-30min.
6. The method according to claim 1, wherein the step S2 comprises:
forming a compact blocking/stripping layer on the surface of the carrier layer by using an intermediate frequency magnetron alternating current reactive sputtering coating technology; the thickness of the blocking/stripping layer is 5-50nm.
7. The method of claim 6, wherein the medium frequency magnetron ac reactive sputter coating technique comprises:
filling argon with purity higher than 99.99% into the cavity at a flow rate of 100-300 sccm;
filling oxygen with purity higher than 99.99% into the cavity at a flow rate of 20-120 sccm;
the copper target is used as a target material, and the coating power is 1-5KW.
8. The method according to claim 1, wherein the step S3 comprises:
depositing copper metal on the barrier/stripping layer by using a direct current magnetron sputtering vacuum coating technology to obtain a seed copper layer; the thickness of the seed copper layer is 5-200nm.
9. The method of claim 8, wherein the dc magnetron sputtering vacuum coating technique comprises:
filling argon with purity higher than 99.99% into the cavity at a flow rate of 100-300 sccm;
the copper target is used as a target material, and the coating power is 5-20KW.
10. An extra-thin copper foil with carrier, characterized in that the extra-thin copper foil with carrier comprises a carrier layer, a blocking/stripping layer, a seed copper layer, an electroplating thickening layer and a surface treatment layer, and the extra-thin copper foil with carrier is prepared by adopting the preparation method of any one of claims 1-9.
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