CN112951800A - Structure and method for improving metallization bonding strength of glass substrate - Google Patents
Structure and method for improving metallization bonding strength of glass substrate Download PDFInfo
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- CN112951800A CN112951800A CN202110219178.5A CN202110219178A CN112951800A CN 112951800 A CN112951800 A CN 112951800A CN 202110219178 A CN202110219178 A CN 202110219178A CN 112951800 A CN112951800 A CN 112951800A
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- glass substrate
- coating
- triethoxysilane
- silane coupling
- coupling agent
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- 239000011521 glass Substances 0.000 title claims abstract description 115
- 239000000758 substrate Substances 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000001465 metallisation Methods 0.000 title claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 65
- 239000002184 metal Substances 0.000 claims abstract description 65
- 238000000576 coating method Methods 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 34
- 230000007062 hydrolysis Effects 0.000 claims abstract description 27
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 27
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000413 hydrolysate Substances 0.000 claims abstract description 15
- 108010009736 Protein Hydrolysates Proteins 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 69
- -1 benzimidazolyl triethoxysilane Chemical group 0.000 claims description 37
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 25
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 230000003301 hydrolyzing effect Effects 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 claims description 9
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 9
- RCNRJBWHLARWRP-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane;platinum Chemical compound [Pt].C=C[Si](C)(C)O[Si](C)(C)C=C RCNRJBWHLARWRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004100 electronic packaging Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 56
- 239000010949 copper Substances 0.000 description 29
- 230000000052 comparative effect Effects 0.000 description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 9
- 238000009713 electroplating Methods 0.000 description 8
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 4
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 125000005372 silanol group Chemical group 0.000 description 3
- CNODSORTHKVDEM-UHFFFAOYSA-N 4-trimethoxysilylaniline Chemical compound CO[Si](OC)(OC)C1=CC=C(N)C=C1 CNODSORTHKVDEM-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- NHBRUUFBSBSTHM-UHFFFAOYSA-N n'-[2-(3-trimethoxysilylpropylamino)ethyl]ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCNCCN NHBRUUFBSBSTHM-UHFFFAOYSA-N 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000007788 roughening Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- CMQCNTNASCDNGR-UHFFFAOYSA-N toluene;hydrate Chemical compound O.CC1=CC=CC=C1 CMQCNTNASCDNGR-UHFFFAOYSA-N 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- WJKMUGYQMMXILX-UHFFFAOYSA-N 2-trimethylsilylacetonitrile Chemical compound C[Si](C)(C)CC#N WJKMUGYQMMXILX-UHFFFAOYSA-N 0.000 description 1
- OLBGECWYBGXCNV-UHFFFAOYSA-N 3-trichlorosilylpropanenitrile Chemical compound Cl[Si](Cl)(Cl)CCC#N OLBGECWYBGXCNV-UHFFFAOYSA-N 0.000 description 1
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 description 1
- TZZGHGKTHXIOMN-UHFFFAOYSA-N 3-trimethoxysilyl-n-(3-trimethoxysilylpropyl)propan-1-amine Chemical compound CO[Si](OC)(OC)CCCNCCC[Si](OC)(OC)OC TZZGHGKTHXIOMN-UHFFFAOYSA-N 0.000 description 1
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- CTLDFURRFMJGON-UHFFFAOYSA-N dimethoxy-methyl-(3-piperazin-1-ylpropyl)silane Chemical compound CO[Si](C)(OC)CCCN1CCNCC1 CTLDFURRFMJGON-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QIOYHIUHPGORLS-UHFFFAOYSA-N n,n-dimethyl-3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN(C)C QIOYHIUHPGORLS-UHFFFAOYSA-N 0.000 description 1
- JXLQREJGIDQFJP-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)acetamide Chemical compound CO[Si](OC)(OC)CCCNC(C)=O JXLQREJGIDQFJP-UHFFFAOYSA-N 0.000 description 1
- KOVKEDGZABFDPF-UHFFFAOYSA-N n-(triethoxysilylmethyl)aniline Chemical compound CCO[Si](OCC)(OCC)CNC1=CC=CC=C1 KOVKEDGZABFDPF-UHFFFAOYSA-N 0.000 description 1
- WUFHQGLVNNOXMP-UHFFFAOYSA-N n-(triethoxysilylmethyl)cyclohexanamine Chemical compound CCO[Si](OCC)(OCC)CNC1CCCCC1 WUFHQGLVNNOXMP-UHFFFAOYSA-N 0.000 description 1
- UMXXGDJOCQSQBV-UHFFFAOYSA-N n-ethyl-n-(triethoxysilylmethyl)ethanamine Chemical compound CCO[Si](OCC)(OCC)CN(CC)CC UMXXGDJOCQSQBV-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
- H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
- H01L23/498—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers
- H01L23/49866—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials
- H01L23/49894—Materials of the insulating layers or coatings
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4846—Leads on or in insulating or insulated substrates, e.g. metallisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/12—Mountings, e.g. non-detachable insulating substrates
- H01L23/13—Mountings, e.g. non-detachable insulating substrates characterised by the shape
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/12—Mountings, e.g. non-detachable insulating substrates
- H01L23/14—Mountings, e.g. non-detachable insulating substrates characterised by the material or its electrical properties
- H01L23/15—Ceramic or glass substrates
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a structure and a method for improving the metallization bonding strength of a glass substrate, and belongs to the field of advanced electronic packaging. The structure comprises a glass substrate, a coarsening structure formed on the glass substrate, a coating formed on the coarsening structure and a metal circuit manufactured on the coating, wherein the coarsening structure is formed by performing structural treatment on the glass substrate, the coating is formed by providing a nitrogen-containing silane coupling agent, performing hydrolysis treatment on the nitrogen-containing silane coupling agent to obtain a hydrolysate, and coating the hydrolysate on the surface of the glass substrate with the coarsening structure. Compared with a silane coupling agent or a nitrogen-containing silane coupling agent, the hydrolysate of the nitrogen-containing silane coupling agent can effectively improve the binding force between the metal circuit and the glass substrate, and the method is simple to operate and low in cost.
Description
Technical Field
The invention belongs to the field of advanced electronic packaging, relates to a method for solving the problem of bonding force between glass and a metal circuit when the glass is used as a packaging substrate, and particularly relates to a structure and a method for improving the metalized bonding strength of a glass substrate.
Background
Three-dimensional integrated packaging technology has evolved rapidly over the past few years. Three-dimensional integration is a novel system-level architecture, and a circuit system of the three-dimensional integration has a stack of a plurality of chips, and the chips are interconnected in a vertical direction by using Through Silicon Vias (TSVs), so that the system realizes higher integration level, higher operation speed and lower power consumption. However, in the application field of high-frequency signals, silicon-based materials have high dielectric loss and high manufacturing cost, and cannot meet the requirement of a radio frequency circuit on high quality factors of devices; glass has many advantages such as higher dimensional stability, isotropy, high transparency, high insulating property and small dielectric loss, and is a preferred scheme for a chip packaging substrate and a method for manufacturing a Glass substrate Through hole (TGV).
However, the bonding force between the glass and the metal of the seed layer and between the glass and the metal of the circuit is weak, and the existing method for roughening the surface of the glass and directly sputtering the metal layer only forms physical contact and electrostatic adsorption effect with the surface of the glass, so the bonding force is poor;
the silane coupling agent is a kind of silane with organic functional group, and its molecule possesses both the reaction group capable of chemically combining with inorganic material (such as glass, silica sand and metal) and the reaction group capable of chemically combining with organic material (synthetic resin, etc.), so that it can be used as "molecular bridge" for connecting inorganic material and organic material, and can be used for connecting two materials with different properties together, i.e. forming inorganic phase-silane coupling agent-organic phase combined layer so as to raise the binding strength between resin base material and inorganic pigment and filler.
At present, the silane coupling agent is used for chemically combining an organic film and glass, and then a Ti/Cu metal seed layer is chemically deposited/sputtered. However, the method has high cost, the CTE of the organic film is greatly different from the CTE of glass, and the organic film is easy to be buried and expands under heat to cause the failure of the device and other reliability hidden troubles.
Disclosure of Invention
The invention aims to provide a structure for improving the metallization bonding strength of a glass substrate, and the structure can effectively improve the bonding force between a metal circuit and the glass substrate.
Another object of the present invention is to provide a method for improving the metalized bonding strength of a glass substrate, by which the bonding force between a metal wiring and the glass substrate can be effectively improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the structure comprises a glass substrate, a coarsening structure formed on the glass substrate, a coating formed on the coarsening structure and a metal circuit manufactured on the coating, wherein the coarsening structure is formed by performing structural treatment on the glass substrate, the coating is formed by providing a nitrogen-containing silane coupling agent, performing hydrolysis treatment on the nitrogen-containing silane coupling agent to obtain a hydrolysate, and coating the hydrolysate on the surface of the glass substrate with the coarsening structure.
In the prior art, the conventional method for improving the bonding force between a substrate and a metal circuit by adopting a semi-additive method is adopted for manufacturing a Ti/Cu metal seed layer, and high-purity metal Ti is expensive. The metal circuit comprises a Cu metal seed layer manufactured on the surface of the coating layer and a heavy wiring layer manufactured on the Cu metal seed layer through electroplating, or a Ti metal seed layer, a Cu metal seed layer and a heavy wiring layer manufactured on the Cu metal seed layer through electroplating, or a Ni metal seed layer, a Cu metal seed layer and a heavy wiring layer manufactured on the Cu metal seed layer through electroplating, wherein the Ti metal seed layer is manufactured on the surface of the coating layer, the Cu metal seed layer and the heavy wiring layer are manufactured on the surface of the coating layer, the heavy wiring layer is manufactured on the Cu metal seed layer through electroplating, the Ti metal seed layer serving as an intermediate dielectric layer is unnecessary, Cu is directly manufactured to serve as the seed layer under the condition that the Ti metal seed layer does not exist, an attachment area can be provided for subsequent electroplating Cu, and the Ti metal seed layer. Therefore, compared with the conventional means, the method is simple to operate and lower in cost, and can ensure that the bonding force between the metal circuit and the glass substrate is improved.
The seed layer may be formed by any one or a combination of a vacuum sputtering method, a Physical Vapor Deposition (PVD) method, a Chemical Vapor Deposition (CVD) method, a direct copper foil attachment method, an evaporation method, and a gel method, which are not described in detail herein.
In the invention, the surface of the glass substrate is subjected to structuring treatment to form a coarsening structure with a special shape, and the actually measured shape of the coarsening structure is pyramid, terrace, inverted bowl or pit.
Further, the specific steps of forming the structure by performing the structuring process on the glass substrate are: after the glass substrate is cleaned, the glass substrate is soaked by adopting an etching solution, the direction is converted once at intervals of 3s (the direction is converted once at intervals of 3s respectively from top to bottom, left to right, front to back), and the time is 1-20min, for example: 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min, 20min and the like to obtain the glass substrate with the coarsened structure.
Wherein, the etching liquid mainly comprises hydrofluoric acid solution, and also comprises other acids, salts and water; the above-mentioned other acids, such as: sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid; salts, such as: ammonium bifluoride, ammonium fluoride.
The inventor of the present application verified through experiments: the pyramid coarsening structure formed on the surface of the glass substrate can ensure that the peeling strength between the glass substrate and the copper metal layer reaches 9.3N/cm; the terrace-shaped coarsening structure formed on the surface of the glass substrate can ensure that the peeling strength between the glass substrate and the copper metal layer reaches 10.7N/cm; the pit-shaped coarsening structure formed on the surface of the glass substrate can ensure that the peeling strength between the glass substrate and the copper metal layer reaches 5.4N/cm; the peel strength was measured under conditions in which only the structured glass substrate was directly metallized. And further forming a coating on the basis of forming a coarsening structure on the glass substrate, wherein the coarsening structure and the coating interact with each other, so that the peeling strength between the glass substrate and the copper metal layer is higher and is 5-15N/cm.
In the present invention, the adhesion manner of the hydrolysate on the glass substrate includes one or a combination of several of a coating method, a soaking method, a spin coating method, a spraying method, and an evaporation method, which are not described in detail.
In the invention, the molecular formula of the hydrolysate of the nitrogen-containing silane coupling agent is as follows: Y-R-Si (OH)3Wherein Y is any one of vinyl, amino, epoxy and mercapto, and R is a carbon chain having a saturated or unsaturated bond. The Y group and the Si-OH generated after hydrolysis can play the role of inorganic-inorganic bonding and can be respectively bonded with inorganic glass and metal Cu. Therefore, compared with the nitrogen-containing silane coupling agent, the hydrolysate of the nitrogen-containing silane coupling agent can effectively improve the bonding force between the metal line and the glass substrate.
As a preferable scheme of the structure for improving the metalized bonding strength of the glass substrate, the hydrolyzing agent for hydrolyzing the nitrogen-containing silane coupling agent is A-water, wherein A is any one of acetic acid, ethanol, methanol and toluene. Adopting any one of acetic acid-water, ethanol-water, methanol-water and toluene-water as a hydrolytic agent of the nitrogenous silane coupling agent, and hydrolyzing to form a hydrolysis product Y-R-Si (OH)3The effect can be fully exerted to effectively connect the metal circuit and the glass substrate.
Further, the volume ratio of a to water is 9:1, and lower or higher volume ratio affects the bonding force between the metal wiring and the glass substrate.
Further, the concentration of the nitrogen-containing silane coupling agent in the hydrolytic agent is 1-50%, and the excessive high concentration or the excessive low concentration can affect the bonding force between the metal circuit and the glass substrate to a certain extent.
As a preferable scheme of the structure for improving the metallization bonding strength of the glass substrate, the nitrogen-containing silane coupling agent is benzimidazolyl triethoxysilane shown in a structural formula (1) or 2-methylimidazolyl triethoxysilane shown in a structural formula (2);
further, the nitrogen-containing silane coupling agent may also be selected from any of the following compounds: 3-ureidopropyltriethoxysilane, diethylaminomethyltriethoxysilane, p-aminophenyltrimethoxysilane, cyclohexylaminomethyltriethoxysilane, trimethylsilylcyanomethane, acetamidopropyltrimethoxysilane, methyltributanonoximosilane, diethylenetriaminopropyltrimethoxysilane, anilinomethyltriethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, gamma-piperazinylpropylmethyldimethoxysilane, 2-cyanoethyltrichlorosilane, bis (3-trimethoxysilylpropyl) amine, p-aminophenyltrimethoxysilane, N-diethyl-3-aminopropyltrimethoxysilane, N-diethyl-1, 1, 1-trimethylsilylamine, N-propyltriethoxysilane, N-propyltrimethoxysilane, p-aminoethyltrimethoxysilane, p-ethyltrimethoxysilane, p, (N, N-dimethyl-3-aminopropyl) trimethoxysilane.
The inventor of the present application verifies through experiments that the nitrogen-containing silane coupling agent represented by the structural formula (1) or (2) has a more significant effect of improving the bonding force between the glass substrate and the metal line compared with other nitrogen-containing silane coupling agents or silane coupling agents.
The benzimidazolyl triethoxysilane is prepared by the following preparation method, and the reaction formula is as follows:
s10a, dissolving gamma-aminopropyl triethoxysilane in a toluene solution, and then mixing with benzimidazole;
s20a, adding a catalyst 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0), heating to 50-70 ℃, and stirring to distill off excessive toluene;
s30a, extracting unreacted gamma-aminopropyl triethoxysilane by using an extracting agent to obtain benzimidazolyl triethoxysilane.
Further, the temperature in the step S20 is 60 ℃, magnetic stirring is adopted, and the stirring time is 15 hours;
the preparation of raw materials of gamma-aminopropyltriethoxysilane, toluene, benzimidazole and catalyst 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0) and the temperature rise and stirring are necessary technical characteristics for preparing benzimidazolyl triethoxysilane of which the hydrolysate has the function of improving the binding force between a glass substrate and a metal circuit, and the preparation method is not indispensable.
Further, the concentration of the γ -aminopropyltriethoxy silicon in the toluene solution is 1 to 50%, for example, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.8%, 2%, 2.3%, 2.5%, 2.8%, 3%, 3.5%, 4%, 4.5%, 5%, 6%, 8%, 10%, 12%, 15%, 18%, 20%, 22%, 25%, 27.5%, 30%, 32%, 35%, 40%, 45%, or 48%, etc.; the benzimidazole is at a concentration of 1 to 50%, for example, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.8%, 2%, 2.3%, 2.5%, 2.8%, 3%, 3.5%, 4%, 4.5%, 5%, 6%, 8%, 10%, 12%, 15%, 18%, 20%, 22%, 25%, 27.5%, 30%, 32%, 35%, 40%, 45%, or 48% based on the total raw material; the concentration of the 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0) as the catalyst is 1 to 10% by weight, for example, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.8%, 2%, 2.3%, 2.5%, 2.8%, 3%, 3.5%, 4%, 4.5%, 5%, 6%, 8%, or 10% by weight based on the total raw material.
Further, the mass ratio of the γ -aminopropyltriethoxysilane, the toluene, the benzimidazole, and the 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0) is 10:10:10: 3. The benzimidazolyl triethoxysilane prepared by adopting the specific proportion is hydrolyzed and then coated on the surface of the glass substrate to form a coating, so that the bonding strength between the glass substrate and the copper metal layer can reach more than 5N/cm.
As another preferable scheme of the structure for improving the metalized bonding strength of the glass substrate, the nitrogen-containing silane coupling agent is 2-methylimidazolyl triethoxy silicon, and the 2-methylimidazolyl triethoxy silane is prepared by the following preparation method, wherein the reaction formula is as follows:
s10b, dissolving gamma-aminopropyl triethoxysilane in a toluene solution, and then adding 2-methylimidazole;
s20b, heating to 50-70 ℃ in a water bath, and stirring to obtain 2-methylimidazolyl triethoxysilane;
the preparation of raw materials of gamma-aminopropyltriethoxysilane, toluene and 2-methylimidazole and the temperature rise and stirring are necessary technical characteristics for preparing the 2-methylimidazolyl triethoxysilane of which the hydrolysate has the function of improving the binding force between a glass substrate and a metal circuit, and the defect is that the preparation is not necessary.
Further, the concentration of the γ -aminopropyltriethoxysilane in the toluene solution is 1 to 50%, for example, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.8%, 2%, 2.3%, 2.5%, 2.8%, 3%, 3.5%, 4%, 4.5%, 5%, 6%, 8%, 10%, 12%, 15%, 18%, 20%, 22%, 25%, 27.5%, 30%, 32%, 35%, 40%, 45%, or 48%, etc.; the concentration of the 2-methylimidazole is 1 to 50%, for example, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.8%, 2%, 2.3%, 2.5%, 2.8%, 3%, 3.5%, 4%, 4.5%, 5%, 6%, 8%, 10%, 12%, 15%, 18%, 20%, 22%, 25%, 27.5%, 30%, 32%, 35%, 40%, 45%, or 48%.
Further, the mass ratio of the gamma-aminopropyltriethoxysilane to the toluene to the 2-methylimidazole is 1:1: 1. The 2-methylimidazolyl triethoxysilane prepared by adopting the specific proportion is hydrolyzed and then coated on the surface of the glass substrate to form a coating, so that the bonding strength between the glass substrate and the copper metal layer can reach more than 3N/cm.
The invention also provides a method for improving the metallization bonding strength of the glass substrate, which forms the structure for improving the metallization bonding strength of the glass substrate and comprises the following steps: carrying out structuring treatment on the glass substrate to form a glass substrate with a coarsening structure; manufacturing a coating on the glass substrate with the coarsening structure to form the glass substrate with the coating; and manufacturing metal lines on the glass substrate with the coating.
Specifically, the method for improving the metalized bonding strength of the glass substrate comprises the following steps:
cleaning the surface of the glass substrate, soaking the glass substrate by adopting etching liquid, converting the direction once at intervals of 3s for 1-20min, and obtaining the glass substrate with a coarsening structure;
adding the self-synthesized nitrogenous silane coupling agent benzimidazolyl triethoxysilane or 2-methylimidazolyl triethoxysilane into a hydrolyzing agent for hydrolysis, and controlling the hydrolysis concentration to be 1-50%;
preparing a hydrolysis product on the surface of the glass substrate with the coarsening mechanism to form a coating;
drying treatment;
carrying out surface cleaning by adopting plasma;
manufacturing a seed layer on the surface of the coating;
pressing a photosensitive dry film above the seed layer, and electroplating to manufacture a copper redistribution layer after exposure and development by adopting LDI equipment;
and removing the residual photosensitive dry film, and etching off the seed layer exposed out of the rewiring layer.
The invention has the beneficial effects that: the hydrolysate of the invention can play a role in bonding inorganic-inorganic substances and can be respectively bonded with inorganic glass and metal Cu. Compared with a silane coupling agent or a nitrogen-containing silane coupling agent, the hydrolysate of the nitrogen-containing silane coupling agent can effectively improve the binding force between the metal circuit and the glass substrate, and the method is simple to operate and low in cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the embodiments of the present invention will be briefly described below. It is obvious that the drawings described below are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a schematic cross-sectional view of a coated bonded glass substrate and metal circuitry according to an embodiment of the present invention.
Fig. 2 is an enlarged view of a portion a of fig. 1.
FIG. 3 is a schematic representation of the method of the present invention for forming a glass substrate metallized bond strength enhancement.
In the figure:
10. a glass substrate; 20. coating; 21. a silanol group; 22. saturated or unsaturated carbon chains; 23. a Y group; 30. a metal line; 40. and (4) roughening the structure.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
Example 1
Preparation of benzimidazolyl triethoxysilane:
s10, dissolving gamma-aminopropyl triethoxysilane in a toluene solution, and then mixing with benzimidazole;
s20, adding a catalyst 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0), heating to 60 ℃, and magnetically stirring for 15 hours to distill off excessive toluene;
s30, extracting unreacted gamma-aminopropyl triethoxysilane by using an extracting agent n-hexane to obtain benzimidazolyl triethoxysilane;
wherein the mass ratio of the gamma-aminopropyltriethoxysilane, the toluene, the benzimidazole and the 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0) is 10:10:10: 3.
Adding the benzimidazolyl triethoxysilane prepared by the method into a hydrolytic agent ethanol-water (volume ratio is 9:1), and controlling the hydrolytic concentration to be 30 percent preferably; cleaning the surface of the glass substrate 10, soaking the glass substrate 10 by using etching liquid, converting the direction once at intervals of 3s for 10min, and obtaining the glass substrate 10 with a coarsening structure; coating the hydrolysis product on the surface of a glass substrate 10 with a coarsening structure to form a coating 20 (figure 1), drying and then cleaning the surface by adopting plasma; manufacturing a Cu metal seed layer on the surface of the coating by a vacuum sputtering method; after the photosensitive dry film is pressed, exposing and developing by adopting LDI equipment, and then electroplating to manufacture a copper redistribution layer; and removing the residual photosensitive dry film, and etching the Cu metal seed layer exposed out of the rewiring layer.
Example 2
This embodiment is substantially the same as embodiment 1 above, except that the seed layer is formed: and sequentially manufacturing a Ti metal seed layer and a Cu metal seed layer on the surface of the coating by a vacuum sputtering method.
Example 3
Preparation of 2-methylimidazolyltriethoxysilane:
s10b, dissolving gamma-aminopropyl triethoxysilane in a toluene solution, and then adding 2-methylimidazole;
s20b, heating to 60 ℃ in a water bath, and magnetically stirring for 10 hours to obtain 2-methylimidazolyl triethoxysilane;
wherein the mass ratio of the gamma-aminopropyltriethoxysilane to the toluene to the 2-methylimidazole is 1:1: 1.
Adding the 2-methylimidazolyl triethoxysilane prepared by the method into a hydrolysis agent methanol-water (volume ratio of 9:1), and preferably controlling the hydrolysis concentration to be 45%; cleaning the surface of the glass substrate 10, soaking the glass substrate 10 by using etching liquid, converting the direction once at intervals of 3s for 10min, and obtaining the glass substrate 10 with a coarsening structure; coating the hydrolysis product on the surface of a glass substrate 10 with a coarsening structure to form a coating 20, drying and then cleaning the surface by adopting plasma; manufacturing a Cu metal seed layer on the surface of the coating by a vacuum sputtering method; after the photosensitive dry film is pressed, exposing and developing by adopting LDI equipment, and then electroplating to manufacture a copper redistribution layer; and removing the residual photosensitive dry film, and etching the Cu metal seed layer exposed out of the rewiring layer.
Example 4
This embodiment is substantially the same as embodiment 3 above, except that the seed layer is formed: and sequentially manufacturing a Ti metal seed layer and a Cu metal seed layer on the surface of the coating by a vacuum sputtering method.
In the above-described examples 1 to 4, as shown in fig. 2, the seed layer and the rewiring layer constitute the metal wiring 30, and the coating layer 20 includes the silanol group 21 bonded to the glass substrate 10, the Y group 23 bonded to the metal wiring 30, and the saturated or unsaturated carbon chain 22 connected to the silanol group 21 and the Y group 23, respectively.
Comparative example 1
The hydrolysis product was prepared by adding gamma-aminopropyltriethoxysilane instead of benzimidazolyl triethoxysilane in example 1 to the hydrolysis agent toluene-water (9: 1 by volume), the concentration of the hydrolysis product was controlled to 30%, and the subsequent steps were the same as in example 1.
Comparative example 2
3-aminopropyltrimethoxysilane was added to a methanol-water (9: 1 by volume) as a hydrolysis agent in place of 2-methylimidazolyltriethoxysilane in example 3 to control the hydrolysate concentration to 45%, and the subsequent steps were the same as in example 3 above.
Comparative example 3
Hydrolysis product was prepared by adding gamma- (2, 3-glycidoxy) propyltrimethoxysilane instead of benzimidazolyl triethoxysilane in example 2 to the hydrolysis agent ethanol-water (9: 1 by volume), and the subsequent procedure was the same as in example 2 above, with the concentration of hydrolysis product controlled to 30%.
Comparative example 4
The hydrolysis product was prepared by adding gamma-aminoethylaminopropyltrimethoxysilane instead of the benzimidazolyltriethoxysilane in example 1 to methanol-water (9: 1 by volume) as a hydrolysis agent, and the concentration of the hydrolysis product was controlled to 30%, and the subsequent steps were the same as in example 1.
Comparative example 5
Diethylenetriaminopropyltrimethoxysilane was added to the hydrolysis agent methanol-water (volume ratio 9:1) instead of the benzimidazolyltriethoxysilane of example 1 to prepare a hydrolysate, the concentration of the hydrolysate was controlled to 30%, and the subsequent steps were the same as those of example 4.
Comparative example 6
3-aminopropyltrimethoxysilane was added to the hydrolysis agent methanol-water (9: 1 by volume) in place of the benzimidazolyl triethoxysilane in example 3 to prepare a hydrolyzate, the concentration of which was controlled to 30%, and the subsequent steps were the same as in example 3.
Comparative example 7
The difference from example 1 is: after the surface of the glass substrate 10 is cleaned and degreased, the hydrolysate is coated on the surface of the glass substrate 10 to form a coating 20.
Test example
Basic performance parameters of the gamma-aminopropyltriethoxysilane used as the starting material in examples 1-4 and the benzimidazolyl triethoxysilane and 2-methylimidazolyl triethoxysilane obtained were tested and the results are shown in Table 1:
TABLE 1 Performance parameters of the raw material gamma-aminopropyltriethoxysilane and the resulting nitrogenous silane coupling agent
| Composition of | Boiling point (. degree.C.) | Flash Point (. degree.C.) | Density (25 ℃, g/mL) | Molecular weight |
| Gamma-aminopropyltriethoxysilane | 217 | 96 | 0.946 | 221.4 |
| Benzimidazolyl triethoxysilane | 198 | 98 | 1.15 | 337.18 |
| 2-methylimidazolyl triethoxysilane | 215 | 150 | 1.25 | 301.18 |
The nitrogen-containing silane coupling agents obtained in examples 1 to 4 and the silane coupling agents used in comparative examples 1 to 6 were tested for their degree of hydrolysis and for the peel strength between the glass substrate and the metal wiring in examples 1 to 4 and comparative examples 1 to 6, and the results are shown in Table 2:
TABLE 2 hydrolysis degree and peel strength test results of the silane coupling agent in each embodiment
| Type (B) | Degree of hydrolysis/%) | Peel strength (N/cm) |
| Example 1 | 100 | 10.4 |
| Example 2 | 100 | 11.2 |
| Example 3 | 100 | 11.7 |
| Example 4 | 100 | 12.7 |
| Comparative example 1 | 95.4 | 2.3 |
| Comparative example 2 | 98.8 | 4.2 |
| Comparative example 3 | 73.7 | 0.8 |
| Comparative example 4 | 100 | 2.3 |
| Comparative example 5 | 97.5 | 3.3 |
| Comparative example 6 | 100 | 3.1 |
| Comparative example 7 | 100 | 5.5 |
Through comparison of the data, the benzimidazolyl triethoxysilane and the 2-methylimidazolyl triethoxysilane prepared by the method of the embodiment are hydrolyzed and then prepared on the surface of the glass substrate, and the hydrolysate can effectively improve the binding force between the glass substrate and the metal circuit no matter whether the seed layer contains a Ti metal seed layer or not. Meanwhile, the glass substrate is subjected to structural treatment and then is made into a coating, so that the bonding force between the glass substrate and the metal circuit can be further effectively improved.
It should be understood that the above-described embodiments are merely preferred embodiments of the invention and the technical principles applied thereto. It will be understood by those skilled in the art that various modifications, equivalents, changes, and the like can be made to the present invention. However, such variations are within the scope of the invention as long as they do not depart from the spirit of the invention. In addition, certain terms used in the specification and claims of the present application are not limiting, but are used merely for convenience of description.
Claims (10)
1. A structure with improved glass substrate metallization bonding strength is characterized by comprising a glass substrate, a coarsening structure formed on the glass substrate, a coating formed on the coarsening structure and a metal circuit manufactured on the coating;
the coarsening structure is formed by carrying out structuralization treatment on the glass substrate;
the coating is formed by providing a nitrogen-containing silane coupling agent, hydrolyzing the nitrogen-containing silane coupling agent to obtain a hydrolysate, and coating the hydrolysate on the surface of the glass substrate with the coarsening structure.
2. The glass substrate metalized bonding strength enhanced structure according to claim 1, wherein the roughened structure is pyramid-shaped, terrace-shaped, inverted bowl-shaped or pit-shaped.
3. The glass substrate metallized bond strength enhanced structure of claim 1, wherein said step of structuring comprises: and cleaning the glass substrate, soaking the glass substrate by using etching liquid, converting the direction once at intervals of 3s for 1-20min, and obtaining the glass substrate with the coarsening structure.
4. The glass substrate metallized bond strength enhanced structure of claim 1 wherein said nitrogen-containing silane coupling agent is a benzimidazolyl triethoxysilane represented by structural formula (1) or a 2-methylimidazolyl triethoxysilane represented by structural formula (2);
5. the structure for improving the metallized bonding strength of a glass substrate according to claim 1, wherein the hydrolyzing agent used for the hydrolysis of the nitrogen-containing silane coupling agent is a-water, wherein a is any one of acetic acid, ethanol, methanol and toluene;
preferably, the volume ratio of a to water is 9: 1;
the concentration of the nitrogen-containing silane coupling agent in the hydrolytic agent is 1-50%.
6. The glass substrate metallized bond strength enhanced structure of claim 4 wherein said benzimidazolyl triethoxysilane is produced using the following preparation method:
s10a, dissolving gamma-aminopropyl triethoxysilane in a toluene solution, and then mixing with benzimidazole;
s20a, adding a catalyst 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0), heating to 50-70 ℃, and stirring to distill off excessive toluene;
s30a, extracting unreacted gamma-aminopropyl triethoxysilane by using an extracting agent to obtain benzimidazolyl triethoxysilane.
7. The glass substrate metallized bond strength enhanced structure of claim 6 wherein the concentration of said γ -aminopropyltriethoxy silicon in said toluene solution is 1 to 50%, the concentration of said benzimidazole is 1 to 50%, the concentration of said catalyst 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0) is 1 to 10%;
preferably, the mass ratio of the gamma-aminopropyltriethoxysilane, the toluene, the benzimidazole and the 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0) is 10:10:10: 3.
8. The glass substrate metallized bond strength enhanced structure of claim 4, wherein said 2-methylimidazolyl triethoxysilane is produced using the following preparation method:
s10b, dissolving gamma-aminopropyl triethoxysilane in a toluene solution, and then adding 2-methylimidazole;
s20b, heating to 50-70 ℃ in a water bath, and stirring to obtain the 2-methylimidazolyl triethoxysilane.
9. The glass substrate metallized bond strength enhanced structure of claim 8, wherein said gamma-aminopropyltriethoxysilane is present in a toluene solution at a concentration of 1-50%, and said 2-methylimidazole is present at a concentration of 1-50%;
preferably, the mass ratio of the gamma-aminopropyltriethoxysilane, the toluene and the 2-methylimidazole is 1:1: 1.
10. A method of glass substrate metallized bond strength enhancement, forming a glass substrate metallized bond strength enhanced structure according to any of claims 1-9, comprising:
carrying out structuring treatment on the glass substrate to form a glass substrate with a coarsening structure;
manufacturing a coating on the glass substrate with the coarsening structure to form the glass substrate with the coating;
and manufacturing a metal circuit on the glass substrate with the coating.
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| JP2006338837A (en) * | 2005-06-06 | 2006-12-14 | Fuji Electric Device Technology Co Ltd | Plating method on glass substrate, method for manufacturing disk substrate for vertical magnetic recording medium, disk substrate for vertical magnetic recording medium, and the vertical magnetic recording medium |
| JP2010030792A (en) * | 2008-07-25 | 2010-02-12 | Asahi Glass Co Ltd | Glass plate with ultraviolet shielding film and method for producing the same |
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