CN107810539A - 包含润滑油的导电糊料和半导体装置 - Google Patents
包含润滑油的导电糊料和半导体装置 Download PDFInfo
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- CN107810539A CN107810539A CN201680035028.6A CN201680035028A CN107810539A CN 107810539 A CN107810539 A CN 107810539A CN 201680035028 A CN201680035028 A CN 201680035028A CN 107810539 A CN107810539 A CN 107810539A
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- conducting paste
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- 125000001204 arachidyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
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- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
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- UZZQDQADMNZGLQ-UHFFFAOYSA-N butanoic acid;2-(2-hydroxyethoxy)ethanol Chemical class CCCC(O)=O.OCCOCCO UZZQDQADMNZGLQ-UHFFFAOYSA-N 0.000 description 1
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- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
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- RHFOYRRUVLOOJP-UHFFFAOYSA-N ethoxyethane;propanoic acid Chemical compound CCOCC.CCC(O)=O RHFOYRRUVLOOJP-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229940116333 ethyl lactate Drugs 0.000 description 1
- FMMOOAYVCKXGMF-MURFETPASA-N ethyl linoleate Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(=O)OCC FMMOOAYVCKXGMF-MURFETPASA-N 0.000 description 1
- LVGKNOAMLMIIKO-QXMHVHEDSA-N ethyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC LVGKNOAMLMIIKO-QXMHVHEDSA-N 0.000 description 1
- 229940093471 ethyl oleate Drugs 0.000 description 1
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 125000000755 henicosyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
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- 229940070765 laurate Drugs 0.000 description 1
- 125000002463 lignoceryl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- WTTJVINHCBCLGX-NQLNTKRDSA-N methyl linoleate Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(=O)OC WTTJVINHCBCLGX-NQLNTKRDSA-N 0.000 description 1
- CCRCUPLGCSFEDV-BQYQJAHWSA-N methyl trans-cinnamate Chemical compound COC(=O)\C=C\C1=CC=CC=C1 CCRCUPLGCSFEDV-BQYQJAHWSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 125000002819 montanyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 125000002465 nonacosyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001196 nonadecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
- 125000002460 pentacosyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
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- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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- 239000011118 polyvinyl acetate Substances 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
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- 239000000057 synthetic resin Substances 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
- TYHJXGDMRRJCRY-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) tin(4+) Chemical compound [O-2].[Zn+2].[Sn+4].[In+3] TYHJXGDMRRJCRY-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/08—Homopolymers or copolymers of acrylic acid esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/022433—Particular geometry of the grid contacts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/095—Dispersed materials, e.g. conductive pastes or inks for polymer thick films, i.e. having a permanent organic polymeric binder
-
- H—ELECTRICITY
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Abstract
本发明涉及导电糊料，其包含50‑97重量％的导电粒子、3‑50重量％的有机介质和0‑20重量％的玻璃料，所述有机介质含有溶剂，其中有机介质另外包含10‑90重量％的烃基润滑油和2‑60重量％的聚合物组分，各自基于有机介质的总量计，所述聚合物组分具有在润滑油中的溶解度为至少100g/kg。本发明还涉及半导体装置，其包含半导体基底，在半导体基底的至少一个表面上使用此糊料印刷导电图案。
Description
本发明涉及导电糊料，其包含50-97重量％的导电粒子、3-50重量％的有机介质和0-20重量％的玻璃料，其中有机介质含有溶剂。
导电糊料或油墨可以用于形成电极，例如导电栅线，例如银栅线，以及在半导体基底或来自绝缘材料的基底的表面上的汇流条。一种特别优选的用途是在用于生产太阳能电池或光伏电池的半导体基底上丝网印刷电极；当来自阳光的光子在半导体上激发电子从价带到导带上时，这些电池将太阳能转化成电能。流向导带的电子被与半导体接触的金属电极收集。
除了用于在用于生产太阳能电池或光伏电池的半导体基底上印刷电极之外，导电糊料或油墨可以用于在用于生产印刷电路板的绝缘基底上印刷栅线，或在陶瓷基底上印刷混合电路。
为了在半导体基底或绝缘基底上印刷细线，丝网印刷方法通常用于成本有效的大规模生产。但是，对于丝网印刷而言，获得均匀的窄线且没有线中断是一个挑战，特别是对于高速丝网印刷而言。工业印刷速度取决于应用要求。此速度在80-800mm/s范围内，优选不小于150mm/s,例如在太阳能电池印刷中，印刷速度是150-300mm/s。
当导电糊料用于在半导体基底上印刷时，糊料通常包含导电粒子、有机介质和任选地玻璃料，其中导电粒子通常是金属粉末。有机介质通常包含至少一种有机液体，例如有机溶剂或有机盐或在室温下呈液态的其它有机化合物。有机介质任选地包含聚合物组分。为了形成金属触点，将导电糊料印刷到基底上。根据材料的类型，然后将基底在约150-950℃的温度下加热，此时有机介质被分解，并且无机物质形成导电轨道和与基底之间的电接触。
随着对于在高速印刷情况下产生细线的需求日益增加，在糊料组合物中的有机介质越来越复杂。如图1所示，印刷的细线通常具有与线主体相邻的不规则形状区域的薄层。这种不规则形状区域的膜厚度比线主体的厚度显著更小，所以此区域的缺点是显著更高的电阻并增加印刷线宽度，这导致所印刷的太阳能电池的遮蔽增大以及电池效率降低。此区域称为“渗流”。在高速丝网印刷中，希望在没有线中断和没有渗流的情况下获得细线。
用于导电糊料的典型组合物例如可以参见US-A 2012/0164777、WO-A 2011/055995、WO-A 2009/157727或US 6,156,237。但是，所有公知的糊料存在的缺点是当用于设计线宽度小于40μm的高速丝网印刷中时，不能排除印刷线具有不需要的中断或在边缘处具有渗流，进而印刷线比设计的可接受性更宽。
所以，本发明的目的是提供导电糊料，其可以进行高速丝网印刷加工，并且其中印刷线是窄的，且在边缘处没有渗流，并且没有不需要的中断。
此目的是通过一种导电糊料实现的，其包含50-97重量％的导电粒子、3-50重量％的有机介质和0-20重量％的玻璃料，所述有机介质含有溶剂，其中有机介质另外包含10-90重量％的烃基润滑油和2-60重量％的聚合物组分，各自基于有机介质的总量计，所述聚合物组分具有在润滑油中的溶解度为至少100g/kg。
令人惊奇的是，发现加入烃基润滑油和溶解度为至少100g/kg的聚合物组分能改进导电糊料在高速丝网印刷中的性能。与公知的组合物相比，本发明的导电糊料具有两个优点。首先，此糊料能印刷较窄的线，并且在边缘处没有渗流。第二，此糊料允许使用具有更细网孔的丝网，其具有较低的线中断趋势。这使得电路的线电阻降低，并且金属消耗减少。在太阳能电池的应用中，较少的渗流减少了对半导体表面的遮蔽，因此提高了电池效率。
溶解在烃基润滑油中的聚合物组分优选是聚丙烯酸酯，聚甲基丙烯酸酯，聚丙烯酸酯或聚甲基丙烯酸酯的共聚物，或它们的混合物。
在一个特别优选的实施方案中，聚合物组分是具有以下通式的聚甲基丙烯酸酯：
其中n是整数，R是直链或支化C1-C22烷基。
一般而言，用于形成聚合物的(甲基)丙烯酸酯是甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、戊基、己基、庚基、辛基、2-乙基己基、2-丙基庚基、壬基、癸基、硬脂基、月桂基、十八烷基、十七烷基、十九烷基、二十烷基、二十一烷基、二十二烷基、二十三烷基、二十四烷基、二十五烷基、二十六烷基、二十七烷基、二十八烷基、二十九烷基、三十烷基、山俞基的甲基丙烯酸酯或丙烯酸酯，优选月桂基、十七烷基和硬脂基的甲基丙烯酸酯或丙烯酸酯，或这些单体的混合物。优选的聚合物是聚聚甲基丙烯酸酯的共聚物，其中R是甲基和一个或多个选自C5-C22烷基的基团。
也可以使用羟基、环氧基或氨基官能的甲基丙烯酸酯和丙烯酸酯。
丙烯酸酯和甲基丙烯酸酯和其混合物的用量通常是50-100重量％，优选80-100重量％，基于组分的单体总量计。
作为其它共聚单体，例如可以使用至多50重量％、优选至多20重量％的以下单体：乙烯基芳族化合物，例如苯乙烯，α-甲基苯乙烯，乙烯基甲苯或对-(叔丁基)苯乙烯；丙烯酸和甲基丙烯酸；丙烯酰胺和甲基丙烯酰胺；马来酸及其酰亚胺和C1-C10烷基酯；富马酸及其酰亚胺和C1-C10烷基酯；衣康酸酸及其酰亚胺和C1-C10烷基酯；丙烯腈和甲基丙烯腈。
常规的自由基聚合方法可以用于制备在本发明导电糊料中所用的聚甲基丙烯酸酯的共聚物。甲基丙烯酸烷基酯单体的聚合反应可以在各种条件下进行，包括本体聚合、溶液聚合，通常在有机溶剂中进行。
在溶液聚合中，反应混合物包含稀释剂、(甲基)丙烯酸烷基酯单体、聚合引发剂，和通常包含链转移剂和任选地交联剂。
在本发明导电糊料中所用的聚甲基丙烯酸酯的共聚物具有约10,000-1,000,000g/mol的相对重均分子量。通常，此重均分子量可以是约20,000-600,000g/mol。分子量可以例如通过GPC使用聚甲基丙烯酸甲酯标准进行检测。所以，所测得的平均分子量是相对值，而不是绝对值。
聚合物具有1-10的PDI值，优选2-8，最优选2-6。PDI表示多分散指数，这衡量分子量分布。关于PDI，例如可以参见“S.S.Rane,P.Choi,Chem.Mater.2005,17,926”。
用于导电糊料的烃基润滑油优选选自环烷烃油，链烷烃油，芳族油，或其中至少两种的混合物。
优选用于本发明的烃基润滑油包括矿物油，聚α-烯烃合成油，天然油例如植物油或动物油，以及它们的混合物。合适的基础油也包括通过合成蜡和疏松石蜡的异构获得的油，以及通过原油的芳族和极性组分进行加氢裂化得到的基料(而不是溶剂萃取)。一般而言，矿物油和合成基础油将各自具有在100℃下的动力粘度为约1-40mm2/s，但是典型的应用将要求每种油具有在100℃下的粘度为约1-10mm2/s。
用于本发明的烃基润滑油包括所有常规的矿物油基料。这将包括在化学结构上属于环烷烃、链烷烃或芳族的那些油。环烷烃油是由在环中的亚甲基和与环附接的链烷烃侧链构成的。其倾点通常低于链烷烃油的倾点。链烷烃油包括饱和、直链或支化的烃。
具有高分子量的直链链烷烃提高了油的倾点，并通常通过脱蜡除去。芳族油是具有半饱和性质的闭合碳环烃，其可以具有附接的侧链。这种油比链烷烃和环烷烃油更容易降解，导致产生腐蚀性副产物。
在实践中，基料通常含有化学组合物，其含有一定比例的所有这三种类型物质(链烷烃、环烷烃和芳族)。关于基料的类型，可以参见例如“Motor Oils and EngineLubricating，A.Schilling,Scientific Publications,1968,小节2.2-2.5”。
聚合物组分可以用于链烷烃、环烷烃和芳族类型的油中。例如，聚合物组分可以用于根据API基料分类的I-V组基础油中。这些分组是本领域技术人员公知的。另外，聚合物组分可以用于气液油中。
气液油(GTL)是本领域公知的。气体来源包括多种物质，例如天然气、甲烷、C1-C3链烷、堆填区沼气等。这些气体可以通过气液(GTL)工艺被转化成适合用作润滑基础油的液体烃产物，例如US 6,497,812中所述的方法，将其全部内容引入本文以供参考。
油可以通过常规技术使用酸、碱和粘土或其它试剂例如氯化铝精制，或可以是萃取的油，例如通过用溶剂进行萃取得到，溶剂例如是苯酚、二氧化硫、糠醛、二氯二乙醚等。它们可以进行加氢处理或加氢精制，通过骤冷或催化脱蜡方法脱蜡，或加氢裂化。矿物油可以从天然来源生产，或由异构化蜡材料或其它精制工艺的残余物组成。优选的合成油是α-烯烃的低聚物，特别是1-癸烯的低聚物，也称为聚α-烯烃或PAO。
矿物油可以衍生自精制的油、再精制的油或其混合物。未精制的油是直接从天然来源或合成来源获得的(例如煤、页岩或油砂沥青)且没有进一步提纯或处理。未精制的油的例子包括通过干馏操作直接得到的页岩油，从蒸馏直接得到的石油润滑油，或从酯化工艺直接得到的酯油，它们各自然后在未进一步处理的情况下使用。精制油与未精制的油相似，区别在于精制油已经在一个或多个提纯步骤中处理以改进一个或多个性能。合适的提纯技术包括蒸馏、加氢处理、脱蜡、溶剂萃取、酸或碱萃取、过滤和渗透，这些都是本领域技术人员公知的。再精制的油是通过在与用于得到精制油的工艺相似的工艺中处理所用的油得到的。这些再精制的油也称为再生油或再处理油，通常另外通过去除已用过的添加剂和油裂解产物的技术进行加工。
在导电糊料中存在的导电粒子可以是由任何导电材料组成的具有任何几何形状的粒子。优选，导电粒子包含碳，银，金，铝，铂，钯，锡，镍，镉，镓，铟，铜，锌，铁，铋，钴，锰，钼，铬，钒，钛，钨，或它们的混合物或合金，或者是其核-壳结构的形式。用于导电粒子的优选材料是银或铝，特别是银，这是由于优良的电导率和优良的抗氧化性。
导电粒子的平均粒径优选在10nm至100μm的范围内。更优选，平均粒径是在100nm至50μm的范围内，特别优选在500nm至10μm的范围内。导电粒子可以具有本领域技术人员公知的任何所需的形状。例如，粒子可以是薄片、棒、线、条、球或任何其混合形式。在本发明中，球形粒子也包括实际形状偏离理想球形的粒子。例如，由于生产，球形粒子也可以具有液滴形状或是截断的。可以用于制备导电糊料的合适粒子是本领域技术人员公知的，并可以商购。特别优选，使用球形的银粒子。球形粒子的优点是具有比不规则形状粒子改进的流变性能。
在组合物中的导电粒子的比例是50-97重量％。此比例优选是70-95重量％，特别是85-92重量％。固体粒子的此重量百分比通常称为固含量。
粒子的形状和尺寸不会改变本发明的性质。粒子可以作为不同形状和尺寸的混合物使用。本领域技术人员公知的是，当具有不同形状或尺寸的混合物的粒子分散在相同的有机介质中时，可以导致更高或更低的粘度。在这种情况下，本领域技术人员知道需要相应地调节有机介质。这种调节可以包括但不限于改变固含量、溶剂含量、聚合物含量、触变剂含量和/或表面活性剂的含量。作为一个例子，通常当使用纳米粒子代替微米尺寸的粒子时，必须降低固含量以避免糊料的粘度增加，这会导致较高含量的有机组分。
导电粒子，尤其当其由金属制成时，通常在生产过程中被有机添加剂涂布。在制备用于印刷导电轨道的组合物的过程中，通常没有除去在表面上的有机添加剂，使得它们随后也存在于导电糊料中。用于稳定的添加剂的比例通常不大于10重量％，基于粒子质量计。用于涂布导电粒子的添加剂可以例如是脂肪胺或脂肪酰胺，例如十二烷基胺。适用于稳定粒子的其它添加剂例如是辛基胺、癸基胺和聚乙烯亚胺。另一个实施方案可以是脂肪酸，脂肪酸酯，其已被环氧化或未被环氧化，例如月桂酸、棕榈酸、油酸、硬脂酸或它们的盐。在粒子上的涂层不会改变本发明的性质。
在一个实施方案中，导电糊料另外包含玻璃料。如果在糊料中存在玻璃料，则可以使用本领域技术人员公知的任何玻璃料，可以基于含铅的组合物或基于不含铅的组合物。对玻璃料的形状或形式没有任何特定的限制。所用玻璃料粒子的平均粒径是在10nm至100μm的范围内。玻璃料粒子的平均粒径更优选是在100nm至50μm的范围内，特别优选500nm至10μm。所用的粒子可以具有本领域技术人员公知的任何所需的形状。例如，粒子可以是薄片、棒、线、条、球或任何其混合形式。在本发明中，球形粒子也包括实际形状偏离理想球形的粒子。例如，由于生产，球形粒子也可以具有液滴形状或是截断的。可用作玻璃料的合适粒子是本领域技术人员公知的，并可以商购。特别优选，使用球形粒子。球形粒子的优点是具有比不规则形状粒子改进的流变性能。根据本发明，玻璃料的含量是0-20重量％，优选0-10重量％，最优选1-5重量％，基于导电糊料的总质量计。
在导电糊料中的有机介质包含至少一种溶剂。在本发明的一个实施方案中，溶剂包含一种或多种选自具有至少一个氧原子的液体有机组分的溶剂。具有至少一个氧原子的液体有机组分优选选自醇、酯醇、二醇、二醇醚、酮、脂肪酸酯或萜烯衍生物，但不包括二元酯。液体有机组分例如可以是苄基醇，Texanol,乳酸乙酯，二甘醇单乙基乙酸酯，二甘醇单丁基醚，二甘醇二丁基醚，二甘醇单丁基醚乙酸酯，丁基溶纤剂，丁基溶纤剂乙酸酯,丙二醇单甲基醚，丙二醇单甲基醚乙酸酯，双丙甘醇单甲基醚，丙二醇单甲基丙酸酯，乙基醚丙酸酯，二甲基氨基甲醛，甲基乙基酮，γ-丁内酯，亚油酸乙基酯，亚麻酸乙基酯，肉桂酸乙基酯，油酸乙基酯，肉桂酸甲基酯，亚油酸甲基酯，亚麻酸甲基酯，油酸甲基酯，邻苯二甲酸二丁基酯，邻苯二甲酸二辛基酯和萜品醇。
作为具有至少一个氧原子的液体有机组分，溶剂可以在导电糊料中作为单种溶剂或作为溶剂混合物使用。在使用溶剂混合物的情况下，溶剂另外包含基于溶剂混合物的总质量计的5-50重量％的至少一种二元酯。二元酯优选选自己二酸、戊二酸、琥珀酸的二甲基酯或其混合物。
当使用单种溶剂或溶剂混合物时，必要的是，有机粘合剂可以在所选择的单种溶剂或溶剂混合物中溶解大于2重量％，从而有机介质包含至少2％的溶解的粘合剂，基于有机介质的总质量计。
在本发明的一个实施方案中，糊料另外包含0.1-20重量％的至少一种选自以下的添加剂：表面活性剂，触变剂，增塑剂，增容剂，消泡剂，干燥剂，交联剂，络合剂和/或导电聚合物粒子。这些添加剂可以单独使用，或作为两种或更多种的混合物使用。
当表面活性剂用作添加剂时，可以使用仅仅一种表面活性剂或使用多于一种表面活性剂。在原则上，本领域技术人员公知的或在现有技术中已经描述的所有表面活性剂可以是合适的。优选的表面活性剂是单种或多种化合物，例如阴离子、阳离子、两亲或非离子型表面活性剂。但是，也可以使用具有颜料亲和性锚基团的聚合物作为表面活性剂，这是本领域技术人员公知的。
在导电粒子被表面活性剂预先涂布的情况下，导电糊料可以不含额外的表面活性剂作为添加剂。
除了溶剂和其它有机添加剂之外，导电糊料也可以包含0.1-20重量％的有机粘合剂。有机粘合剂可以选自天然或合成的树脂和聚合物。如本领域技术人员公知，这些选择是基于但不限于溶剂相容性和化学稳定性。例如，现有技术中的常规粘合剂包括纤维素衍生物、丙烯酸树脂、酚树脂、脲-甲醛树脂、醇酸树脂、脂族石油树脂、蜜胺甲醛树脂、松香、聚乙烯、聚丙烯、聚苯乙烯、聚醚、聚氨酯、聚乙酸乙烯酯以及它们的共聚物。
本发明的糊料特别用于高速丝网印刷方法中，例如至少150mm/s，因为这些糊料即使在这些工艺中也能获得精细印刷线，且没有线中断和渗流。
本发明还涉及半导体装置，其包含半导体基底，在半导体基底的至少一个表面上使用上述糊料印刷导电图案。由此，通过丝网印刷在半导体基底上印刷图案。在印刷之后，带有印刷图案的半导体基底被加热到150-950℃的温度以形成半导体装置。加热工艺对应于已经用于在半导体上产生导电图案的糊料。半导体基底通常是基于硅材料。
这种半导体装置例如包括光伏电池，其包含n型区域、p型区域、p-n结和导电栅线。光伏电池任选地包含在基底表面上的防反射层。基底可以是单晶硅、多晶硅、无定形硅涂布的固体基底，或表面被多晶或无定形透明导电氧化物(TCO)涂布的基底，例如氧化铟锡(ITO)，ZnO基透明导电氧化物，例如氧化铟镓锌(IGZO)、氧化铟锌锡(IZTO)、氧化铟锌(IZO)、氧化铟钨(IWO)、氧化镓锌(GZO)。导电栅线是从导电糊料通过丝网印刷形成的。本发明导电糊料的一个或多个实施方案可以用于形成导电栅线。
实施例
在实施例中，使用根据以下表格所示的糊料组合物：
表1:对比例和实施例的糊料的组成
所用的银粉末具有0.5-2.5μm的平均直径。作为玻璃料，使用含铅的玻璃料。A型溶剂是二元酯，B型溶剂是二醇、二醇醚和脂肪酸酯的混合物。
聚合物组分是具有以下通式的聚甲基丙烯酸酯：
在实施例中，使用具有不同烷基作为基团R的不同聚甲基丙烯酸酯共聚物。在下文中，聚甲基丙烯酸酯表示为CxMA，其中Cx是在基团R中的碳原子数目。例如，C1MA是聚甲基丙烯酸酯，其中R是甲基；C12MA是聚甲基丙烯酸酯，其中R是C12H25。在聚合物组分中的不同聚甲基丙烯酸酯的量是用重量％表示，基于聚合物组分的总质量计。所有其它百分比数据是基于糊料的总质量计。
对比例：
首先混合1-3％的A型溶剂和3.5-6％的B型溶剂。将0.05-0.4重量％的乙基纤维素溶解在此溶剂混合物中以形成乙基纤维素介质，然后其进一步与所加入的0.2-2％聚甲基丙烯酸异丁基酯(有机粘合剂)、0-2％表面活性剂、0-1％增稠剂、0-1％触变剂混合以形成均匀介质。所有百分比数值是基于糊料总量计的重量％。此混合物通过在高温下机械搅拌进行均化。在另一个步骤中向介质中加入玻璃料和金属粉末以确保它们良好地分散在介质中。粉末-介质混合物用三辊磨研磨，得到均匀分散的糊料。
为了比较实施例1-5和对比例，使用相同的银粉末、玻璃料、表面活性剂、增稠剂、触变剂和乙基纤维素。
实施例1：
按照与对比例所述相同的工序制备糊料，不同之处是未加入有机粘合剂，而是加入具有润滑油的聚合物组分。相应地降低A型溶剂和B型溶剂的混合物的浓度，从而保持在糊料中的相同量的有机液体。在此实施例中，聚合物组分是25％C1MA+40％C12MA+35％C17MA的共聚物，其具有分子量Mw为127,000g/mol，并且PDI＝4.6。
实施例2：
按照与对比例所述相同的工序制备糊料，不同之处是未加入有机粘合剂，而是加入具有石油润滑油的聚合物组分。相应地降低A型溶剂和B型溶剂的混合物的浓度，从而保持在糊料中的相同量的有机液体。在此实施例中，聚合物组分是25％C1MA+75％C18MA的共聚物，其Mw为57,100g/mol，并且PDI＝3.9。
实施例3：
按照与对比例所述相同的工序制备糊料，不同之处是未加入有机粘合剂，而是加入具有石油润滑油的聚合物组分。相应地降低A型溶剂和B型溶剂的混合物的浓度，从而保持在糊料中的相同量的有机液体。在此实施例中，聚合物组分是25％C1MA+75％C18MA的共聚物，其Mw为28,000g/mol，并且PDI＝2.9。
实施例4：
按照与对比例所述相同的工序制备糊料。在此实施例中，聚合物组分是25％C1MA+75％C18MA的共聚物，其Mw为21,000g/mol，并且PDI＝2.7。当与实施例3比较时，聚合物组分的轻微区别并没有产生在可印刷性方面的明显区别。
实施例5：
按照与对比例所述相同的工序制备糊料。在此实施例中，聚合物组分是25％C1MA+20％C17MA+55％C18MA的共聚物，其Mw为529,000g/mol，PDI＝3.42。在这种情况下，聚合物组分产生比在对比例中的有机粘合剂溶液更高的粘度，所以如本领域技术人员所知，略微调节聚合物组分的浓度，但仍然在对比例定义的范围内。印刷结果具有比对比例更少的渗流。
实施例6：
按照与对比例所述相同的工序制备糊料。在此实施例中，聚合物组分是100％C18MA，其Mw为936,000g/mol，PDI＝7.1。在这种情况下，聚合物组分产生比在对比例中的有机粘合剂溶液更高的粘度，所以如本领域技术人员所知，略微调节聚合物组分的浓度，但仍然在对比例定义的范围内。
将对比例和实施例1-3的糊料在以下印刷条件下丝网印刷到固体基底上。
印刷条件：
丝网参数：
对比例和实施例1用丝网A印刷。
| 筛目计数 | 网孔 | EOM | 张力 | 角度 | 线直径 | 织物厚度 |
| 325 | 37μm | 12μm | 24N | 30° | 16μm | 28μm |
实施例1-3用丝网B印刷。
| 筛目计数 | 网孔 | EOM | 张力 | 角度 | 线直径 | 织物厚度 |
| 325 | 30μm | 12μm | 24N | 30° | 16μm | 28μm |
在光学3D显微镜下检测印刷线，用于线尺寸评价。结果如图1-5所示。
在附图中，
图1显示用丝网A印刷的对比例的印刷线，
图2显示用丝网A印刷的实施例1的印刷线，
图3显示用丝网B印刷的实施例1的印刷线，
图4显示用丝网B印刷的实施例2的印刷线，和
图5显示用丝网B印刷的实施例3的印刷线。
从这些附图可见，用对比例糊料印刷的线比用本发明糊料印刷的线更宽。另外，用本发明糊料印刷的线的渗流显著减少，因此具有较窄的线宽度。线高度的变化也减少。所有印刷品没有出现线中断。所以，这显然证明了本发明实施例获得了比对比例更好的印刷结果。
Claims (15)
1.一种导电糊料，其包含50-97重量％的导电粒子、3-50重量％的有机介质和0-20重量％的玻璃料，所述有机介质含有溶剂，其中有机介质另外包含10-90重量％的烃基润滑油和2-60重量％的聚合物组分，各自基于有机介质的总量计，所述聚合物组分具有在润滑油中的溶解度为至少100g/kg。
2.根据权利要求1的导电糊料，其中聚合物组分是聚丙烯酸酯，聚甲基丙烯酸酯，聚丙烯酸酯或聚甲基丙烯酸酯的共聚物，或它们的混合物。
3.根据权利要求1或2的导电糊料，其中聚合物组分是具有以下通式的聚甲基丙烯酸酯：
其中n是整数，R是直链或支化C1-C22烷基。
4.根据权利要求1-4中任一项的导电糊料，其中聚合物组分具有约10,000-1,000,000g/mol的相对重均分子量。
5.根据权利要求1-4中任一项的导电糊料，其中烃基润滑油是选自环烷烃油，链烷烃油，芳族油，天然油，或其中至少两种的混合物。
6.根据权利要求1-5中任一项的导电糊料，其中烃基润滑油具有在100℃温度下的粘度为1-40mm2/s。
7.根据权利要求1-6中任一项的导电糊料，其中导电粒子包含碳或银，金，铝，铂，钯，锡，镍，镉，镓，铟，铜，锌，铁，铋，钴，锰，钼，铬，钒，钛，钨，或它们的混合物或合金，或者是其核-壳结构的形式。
8.根据权利要求1-7中任一项的导电糊料，其中导电粒子被有机添加剂涂布。
9.根据权利要求1-8中任一项的导电糊料，其中溶剂包含一种或多种选自具有至少一个氧原子的液体有机组分的溶剂，所述具有至少一个氧原子的液体有机组分优选选自醇、酯醇、二醇、二醇醚、酮、脂肪酸酯或萜烯衍生物，但不包括二元酯。
10.根据权利要求9的导电糊料，其中溶剂另外包含5-50重量％的至少一种二元酯，二元酯优选选自己二酸、戊二酸、琥珀酸的二甲基酯或其混合物。
11.根据权利要求1-10中任一项的导电糊料，其中糊料另外包含0.1-20重量％的至少一种选自以下的添加剂：表面活性剂，触变剂，增塑剂，消泡剂，干燥剂，交联剂，络合剂和/或导电聚合物粒子。
12.一种半导体装置，其包含半导体基底，在半导体基底的至少一个表面上使用根据权利要求1-11中任一项的导电糊料印刷导电图案。
13.根据权利要求12的半导体装置，其中半导体基底是基于硅的。
14.根据权利要求12或13的半导体装置，其中在半导体基底上形成防反射层，并且在防反射层上印刷导电图案。
15.根据权利要求12-14中任一项的半导体装置，其中半导体装置是光伏电池，并且导电图案具有导电栅线。
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| ES2896694T3 (es) | 2016-07-05 | 2022-02-25 | Basf Se | Uso de inhibidores de la corrosión para combustibles y lubricantes |
| JP7119454B2 (ja) * | 2018-03-16 | 2022-08-17 | 住友金属鉱山株式会社 | 有機ビヒクルの製造方法、及び、導電性ペーストの製造方法 |
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- 2016-06-15 JP JP2017565782A patent/JP2018519634A/ja active Pending
- 2016-06-15 US US15/736,013 patent/US20180182506A1/en not_active Abandoned
- 2016-06-15 KR KR1020177036064A patent/KR20180019106A/ko unknown
- 2016-06-15 EP EP16729890.0A patent/EP3311388B1/en not_active Not-in-force
- 2016-06-15 CN CN201680035028.6A patent/CN107810539A/zh active Pending
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Also Published As
| Publication number | Publication date |
|---|---|
| EP3311388B1 (en) | 2019-04-17 |
| EP3311388A1 (en) | 2018-04-25 |
| KR20180019106A (ko) | 2018-02-23 |
| TW201709219A (zh) | 2017-03-01 |
| JP2018519634A (ja) | 2018-07-19 |
| PH12017502242A1 (en) | 2018-06-11 |
| WO2016202841A1 (en) | 2016-12-22 |
| US20180182506A1 (en) | 2018-06-28 |
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