TWI530533B - Organic silicon resin compositions and white prepregs and white laminates using it - Google Patents

Organic silicon resin compositions and white prepregs and white laminates using it Download PDF

Info

Publication number
TWI530533B
TWI530533B TW104111511A TW104111511A TWI530533B TW I530533 B TWI530533 B TW I530533B TW 104111511 A TW104111511 A TW 104111511A TW 104111511 A TW104111511 A TW 104111511A TW I530533 B TWI530533 B TW I530533B
Authority
TW
Taiwan
Prior art keywords
white
parts
resin
weight
resin composition
Prior art date
Application number
TW104111511A
Other languages
English (en)
Other versions
TW201623451A (zh
Inventor
guo-fang Tang
Su-Wen Ye
Peng Sun
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed filed Critical
Application granted granted Critical
Publication of TWI530533B publication Critical patent/TWI530533B/zh
Publication of TW201623451A publication Critical patent/TW201623451A/zh

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/14—Layered products comprising a layer of metal next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/10—Reinforcing macromolecular compounds with loose or coherent fibrous material characterised by the additives used in the polymer mixture
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • C08J5/241—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres
    • C08J5/244—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres using glass fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • C08J5/249—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs characterised by the additives used in the prepolymer mixture
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/10—Metal compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/05—5 or more layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
    • B32B2260/021—Fibrous or filamentary layer
    • B32B2260/023—Two or more layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/046—Synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/101—Glass fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/412—Transparent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/71—Resistive to light or to UV
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/712—Weather resistant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/718—Weight, e.g. weight per square meter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/732—Dimensional properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/748—Releasability
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C08K5/19—Quaternary ammonium compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/5398—Phosphorus bound to sulfur
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/5399—Phosphorus bound to nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Laminated Bodies (AREA)
  • Reinforced Plastic Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Description

有機矽樹脂組合物以及使用它的白色預浸料和白色層壓板
本發明涉及縮合型矽樹脂代替傳統的有機樹脂得到的有機矽樹脂組合物以及使用它的白色預浸料、層壓板及覆銅板，其具有高耐熱、高反射及優越的耐熱老化和耐紫外光照老化性能。
發光二極體(LED)是一種可以將電能直接轉換為光能的半導體器件，具有節能、環保和壽命長等特點，LED的迅速發展和廣泛應用，將引發照明領域的一場革命。
而安裝LED的PCB基板，在加工和使用過程中，由於LED具有發光的特性，因此樹脂層表面的光反射率應該越大越好；而且其印製線路板用覆銅板，在製作晶片LED的過程中要經過各種各樣的受熱過程；晶片LED在使用時，LED元件本身也會發熱，LED發光時也會產生熱應力，因而要求用於LED的白色覆銅板具有高的耐熱性。
除了需要具有常規CCL的一般性能要求外，LED白色覆銅板還需具備一些特殊性能。LED用白色CCL不僅需要高的初態反射率，而且還需要它具備長期的保持反射率的特性（包括高熱輻射板面不變色性，長期紫外線照射板面不變色性），同時還需要具有高耐熱性，以及高溫下的高剛性。使白色CCL獲得高的耐紫外線變色性及耐熱變色性，主要依靠樹脂組成中多種成分的性能改進或創新，來實現這一特殊性能的。
有機矽樹脂的結構中既含有有機基團，又含有無機基團，這種特殊的組成和分子結構使得矽樹脂兼有有機物的特性與無機物的功能於一身。有機矽樹脂是熱固性樹脂，在高溫熱氧化作用時，僅僅發生側鏈有機基的斷裂，分解而逸出其氧化物，而主鏈的矽氧鍵很少破壞，最終生成-O-Si-O-形式的聚合物，其Si-O矽氧鍵鍵能在373 KJ/mol，故其耐熱性遠優於一般有機樹脂。甲基矽氧烷對紫外光幾乎不吸收，含PhSiO 1.5或Ph 2SiO鏈節的矽氧烷也僅吸收280nm以下的光線，故有機矽樹脂具有非常好的耐候性。此外，有機矽樹脂具有突出的耐候性，是任何一直有機樹脂所望塵莫及的，即使在紫外線強烈照射下，矽樹脂耐黃變也非常優越。
因此，與一般的樹脂相比，有機矽樹脂具有優越的耐高低溫、耐氣候老化、電氣絕緣、耐臭氧、阻燃和憎水等獨特性能。
鑒於有機矽樹脂的超高耐熱、耐黃變性以及耐候性，本發明的目的之一在於提供一種有機矽樹脂組合物，使用該有機樹脂組合物得到的白色預浸料、層壓板以及覆銅板具有優異的耐熱性、耐候性以及耐黃變性。
為了實現上述目的，本發明採用了如下技術方案：
一種有機矽樹脂組合物，所述有機矽樹脂組合物，包括：
縮合型矽樹脂： 100重量份；
白色填料：5~60重量份；
催化劑：0.0001~2重量份；
助劑：0.1~10重量份。
所述白色填料的含量例如為8重量份、12重量份、16重量份、20重量份、24重量份、28重量份、32重量份、36重量份、40重量份、44重量份、48重量份、52重量份或56重量份。
所述催化劑的含量例如為0.0005重量份、0.001重量份、0.005重量份、0.01重量份、0.05重量份、0.1重量份、0.3重量份、0.5重量份、1.0重量份、1.5重量份或2.0重量份。
所述助劑的含量例如為0.5重量份、1重量份、2重量份、3重量份、4重量份、5重量份、6重量份、7重量份、8重量份或9重量份。
在本發明中，所述縮合型矽樹脂主要為甲基矽樹脂、甲基苯基矽樹脂或苯基矽樹脂中的任意一種或者至少兩種的混合物。
在本發明中，所述縮合型矽樹脂為脫水縮合、脫醇縮合或脫氫縮合中的任意一種，其反應結構如下所示：
在本發明中，所述縮合型矽樹脂為R/Si=1.0~1.7（摩爾比）（例如1.1、1.2、1.3、1.4、1.5、1.6或1.7）和Ph/(Me+Ph)= 0~1.0（摩爾比）（例如0.1、0.2、0.3、0.4、0.5、0.6、0.7、0.8、0.9或1.0）的甲基矽樹脂、甲基苯基矽樹脂或苯基矽樹脂中的任意一種或者至少兩種的混合物，其中Ph代表苯基基團，Me代表甲基基團，R代表有機官能團-CH 3、-Ph、-OCH 3、-OCH 2CH 3、-OH或-H。在縮合型矽樹脂中，R/Si（摩爾比）過小，Ph/Si（摩爾比）過低，矽樹脂固化後柔軟性差，漆膜變硬，而R/Si（摩爾比）過大，Ph/Si（摩爾比）過高層壓板硬度低，固化慢，熱固性低，故所述縮合型矽樹脂優選R/Si=1.2~1.7（摩爾比）且Ph/ (Me+Ph)=0.2~0.6（摩爾比）的甲基苯基矽樹脂。
在本發明中，所述白色填料為氧化鋁、二氧化鈦、氫氧化鋁、二氧化矽或氧化鋅中的任意一種或者至少兩種的混合物，優選二氧化鈦。
根據本發明，所述催化劑是環烷酸鋅、環烷酸錫、環烷酸鈷、環烷酸鐵、環烷酸鈰、羧酸鋅、羧酸錫、羧酸鈷、羧酸鐵、羧酸鈰、全氟磺酸、氯化磷腈、胺類、辛酸鋅、異辛酸鋅、季銨堿、鈦酸酯或胍類化合物等中的任意一種或者至少兩種的組合。
根據本發明，所述助劑為偶聯劑或/和分散劑，所述偶聯劑為矽烷偶聯劑或/和鈦酸酯偶聯劑。
本發明所述的“包括”，意指其除所述組份外，還可以包括其他組份，這些其他組份賦予所述有機矽樹脂組合物不同的特性。除此之外，本發明所述的“包括”，還可以替換為封閉式的“為”或“由……組成”。
例如，所述有機矽樹脂組合物還可以含有各種添加劑，作為具體例，可以舉出阻燃劑、抗氧劑、熱穩定劑、抗靜電劑、紫外線吸收劑、顏料、著色劑或潤滑劑等。這些各種添加劑可以單獨使用，也可以兩種或者兩種以上混合使用。
本發明的目的之二在於提供一種樹脂膠液，其是將如上所述的有機矽樹脂組合物溶解或分散在溶劑中得到。
作為本發明中的溶劑，沒有特別限定，作為具體例，可以舉出甲苯、二甲苯、正己烷、環己烷或異丙醇等。
本發明的目的之三在於提供一種白色預浸料，其包括增強材料及通過含浸乾燥後附著在增強材料上的如上所述的有機矽樹脂組合物。
本發明的白色預浸料通過矽樹脂利用縮合反應聚合交聯而成網狀結構。
示例性的預浸料的製備方法為：
將縮合型矽樹脂、催化劑、助劑、白色填料、溶劑以及任選地其他組分得到的有機矽樹脂膠液浸漬于增強材料如片狀玻纖纖維基材中，然後乾燥而得。
本發明的目的之四在於提供一種白色層壓板，所述白色層壓板含有至少一張如上所述的白色預浸料，其通過將至少一張如上所述的預浸料加熱加壓成型得到。
本發明的目的之五在於提供一種白色覆銅箔層壓板，所述白色覆銅箔層壓板包括至少一張疊合的如上所述的白色預浸料及壓覆在疊合後的預浸料的一側或兩側的銅箔。
與已有技術相比，本發明具有如下有益效果：
本發明利用有機矽的高耐熱性、優越的耐候性及耐紫外光照，替代傳統樹脂不耐熱、易黃變等缺點，通過將縮合型矽樹脂、催化劑、白色填料、助劑以及任選地其他組分複配，得到具有優異的耐熱性、耐候性以及耐黃變性的有機矽樹脂組合物，同時與加成型矽樹脂相比，縮合型矽樹脂與銅箔具有更好的剝離強度，將縮合型矽樹脂應用在LED白色覆銅板中，使其同樣具有優異的耐熱性、耐候性以及耐黃變性。
此外，本發明將有機矽樹脂代替傳統的有機樹脂應用在LED白色覆銅板中，不但能滿足LED的高耐熱性要求，而且還可克服陶瓷基板存在的成本高、加工性差的缺點，在小型、薄型的LED照明產品、液晶顯示器背光源等方面的散熱基板上得到廣泛的應用，是一種可替代陶瓷基板的新型散熱基板的基材。
下面通過具體實施方式來進一步說明本發明的技術方案。
實施例1
稱取R/Si=1.1（摩爾比），Ph/(Me+Ph)=0（摩爾比）的甲基矽樹脂100份，溶於100份甲苯溶劑中，待溶解完全後，用精准取液器量取0.003份的辛酸鋅催化劑和0.5份矽烷偶聯劑γ-縮水甘油醚氧丙基三甲氧基矽烷（美國，道康寧製造），投入到矽樹脂溶液中，攪拌均勻後，添加5.5份白色顏料金紅石型二氧化鈦，室溫下攪拌1h，乳化20min，得白色矽樹脂膠液。
用此白色矽樹脂清漆浸漬重量為104g/cm 2的玻璃纖維布，在110℃乾燥10min得到樹脂含量為58%的預浸料。將8片預浸料重疊，在該層疊體上下表面配置35μ的電解銅箔，在200℃、表面壓力30kgf/cm 2、30mmHg以下的真空下進行120min的加壓成型，獲得厚度為1.0mm的雙面覆銅層壓板。
實施例2
稱取R/Si=1.5（摩爾比），Ph/(Me+Ph)= 0.4（摩爾比）的甲基苯基矽樹脂100份，溶於100份甲苯溶劑中，待溶解完全後，用精准取液器量取0.005份乙醯丙酮鈷催化劑和1.2份γ-縮水甘油醚氧丙基三甲氧基矽烷（美國，道康寧製造），投入到矽樹脂溶液中，攪拌均勻後，添加30份白色顏料金紅石型二氧化鈦，室溫下攪拌1h，乳化20min，得白色矽樹脂膠液。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
實施例3
稱取R/Si=1.6（摩爾比），Ph/(Me+Ph)= 0.8（摩爾比）的甲基苯基矽樹脂100份，溶於100份甲苯溶劑中，待溶解完全後，用精准取液器量取0.1份的環烷酸鋁催化劑和1.8份W-903（德國，BYK公司製造），投入到矽樹脂溶液中，攪拌均勻後，添加25份白色顏料銳鈦礦型二氧化鈦和10份二氧化矽填料，室溫下攪拌1h，乳化20min，得白色矽樹脂膠液。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
實施例4
稱取R/Si=1.7（摩爾比），Ph/(Me+Ph)= 1.0（摩爾比）的苯基矽樹脂100份，溶於100份甲苯溶劑中，待溶解完全後，用精准取液器量取0.1份的環烷酸鋁催化劑和6.8份W-903（德國，BYK公司製造），投入到矽樹脂溶液中，攪拌均勻後，添加25份白色顏料銳鈦礦型二氧化鈦和35份氧化鋁填料，室溫下攪拌1h，乳化20min，得白色矽樹脂膠液。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
實施例5
稱取R/Si=1.1（摩爾比），Ph/(Ph+Me)=0 (摩爾比)的甲基矽樹脂50.0份和R/Si=1.7（摩爾比），Ph/(Ph+Me)=0.9 (摩爾比)的甲基苯基矽樹脂50.0份，溶於100份甲苯溶劑中，待溶解完全後，用精准取液器量取1.8份的鈦酸酯催化劑和1.8份W-903分散劑（德國，BYK公司製造），投入到矽樹脂溶液中，攪拌均勻後，添加25份白色顏料銳鈦礦型二氧化鈦和35份二氧化矽填料，室溫下攪拌1h，乳化20min，得白色矽樹脂膠液。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
對比例1
稱取甲基乙烯基矽樹脂100份（乙烯基品質分數為1.0%），溶入50份粘度為500mPa.s的甲基乙烯基矽油中，溶解均勻後加入2.9份甲基含氫矽油（含氫量為1.3%），高速攪拌均勻後稱取0.001份己炔醇，攪拌30min後加入0.01份鉑-甲基苯基乙烯基絡合物，繼續攪拌30min後加入30份白色顏料金紅石型二氧化鈦，室溫下攪拌1h，乳化20min，得白色加成型矽樹脂膠液。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
對比例2
稱取R/Si=1.1（摩爾比），Ph/(Me+Ph)=0（摩爾比）的甲基矽樹脂100份，溶於100份甲苯溶劑中，待溶解完全後，用精准取液器量取0.003份的辛酸鋅催化劑和0.5份矽烷偶聯劑γ-縮水甘油醚氧丙基三甲氧基矽烷（美國，道康寧製造），投入到矽樹脂溶液中，攪拌均勻後，添加2.5份白色顏料金紅石型二氧化鈦，室溫下攪拌1h，乳化20min，得白色矽樹脂膠液。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
對比例3
稱取R/Si=1.6（摩爾比），Ph/(Me+Ph)= 0.8（摩爾比）的甲基苯基矽樹脂100份，溶於100份甲苯溶劑中，待溶解完全後，用精准取液器量取0.1份的環烷酸鋁催化劑和1.8份W-903（德國，BYK公司製造），投入到矽樹脂溶液中，攪拌均勻後，添加65份白色顏料銳鈦礦型二氧化鈦和10份二氧化矽填料，室溫下攪拌1h，乳化20min，得白色矽樹脂膠液。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
對比例4
稱取R/Si=1.8（摩爾比），Ph/(Me+Ph)= 0.8（摩爾比）的甲基苯基矽樹脂100份，溶於100份甲苯溶劑中，待溶解完全後，用精准取液器量取0. 1份的環烷酸鋁催化劑和1.8份W-903（德國，BYK公司製造），投入到矽樹脂溶液中，攪拌均勻後，添加25份白色顏料銳鈦礦型二氧化鈦和10份二氧化矽填料，室溫下攪拌1h，乳化20min，得白色矽樹脂膠液。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
效果確認測試
（1）耐熱變色性
將實施例1~5及對比例1~4中得到的覆銅箔白色層壓板用切割鋸將雙面覆銅層壓板切割為大小100×100mm後進行蝕刻處理，得各有機矽白色層壓板，並在200℃下進行長時間烘烤實驗，進行反射率對比，資料請見下表。
（2）耐熱穩定性
將實施例1~5及對比例1~4的覆銅板層壓板進行蝕刻處理，得到各層壓板，使用熱重分析(TGA)測量層壓板基材熱分解溫度，其分解2%的溫度Td(2%)請見下表。
測試設備：NETZSCH TG209F3
測試條件：室溫至700℃，升溫速率可控制在10℃±0.1℃/min，氮氣流速為0.9ml/s。
（3）剝離強度測試
測試方法：使用IPC-TM-6502.4.8方法進行測試，測試資料請見下表。
<TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td>   </td><td> 實施例1 </td><td> 實施例2 </td><td> 實施例3 </td><td> 實施例4 </td><td> 實施例5 </td><td> 對比例1 </td><td> 對比例2 </td><td> 對比例3 </td><td> 對比例4 </td></tr><tr><td> 甲基苯基矽樹脂 </td><td> - </td><td> 100 </td><td> 100 </td><td> - </td><td> 50 </td><td> - </td><td> - </td><td> 100 </td><td> 100 </td></tr><tr><td> 甲基矽樹脂 </td><td> 100 </td><td> - </td><td> - </td><td> - </td><td> 50 </td><td> - </td><td> 100 </td><td> - </td><td> - </td></tr><tr><td> 苯基矽樹脂 </td><td> - </td><td> - </td><td> - </td><td> 100 </td><td> - </td><td> - </td><td> - </td><td> - </td><td> - </td></tr><tr><td> 甲基乙烯基矽樹脂 </td><td> - </td><td> - </td><td> - </td><td> - </td><td> - </td><td> 100 </td><td> - </td><td> - </td><td> - </td></tr><tr><td> R/Si </td><td> 1.1 </td><td> 1.5 </td><td> 1.6 </td><td> 1.7 </td><td> 1.1/1.7 </td><td> - </td><td> 1.1 </td><td> 1.6 </td><td> 1.8 </td></tr><tr><td> Ph/(Me+Ph) </td><td> 0 </td><td> 0.4 </td><td> 0.8 </td><td> 1.0 </td><td> 0/0.9 </td><td> - </td><td> 0 </td><td> 0.8 </td><td> 0.8 </td></tr><tr><td> 金紅石型二氧化鈦 </td><td> 5.5 </td><td> 30 </td><td> - </td><td> - </td><td> - </td><td> 30 </td><td> 2.5 </td><td> - </td><td> - </td></tr><tr><td> 銳鈦礦型二氧化鈦 </td><td> - </td><td> - </td><td> 25 </td><td> 25 </td><td> 25 </td><td> - </td><td> - </td><td> 65 </td><td> 25 </td></tr><tr><td> 二氧化矽 </td><td> - </td><td> - </td><td> 10 </td><td> - </td><td> 35 </td><td> - </td><td> - </td><td> 10 </td><td> 10 </td></tr><tr><td> 氧化鋁 </td><td> - </td><td> - </td><td>   </td><td> 35 </td><td> - </td><td> - </td><td> - </td><td> - </td><td> - </td></tr><tr><td> 測試結果 </td></tr><tr><td> 耐熱變色性 反射率% </td><td> 烘烤前 </td><td> 88.2 </td><td> 89.5 </td><td> 88.9 </td><td> 89.2 </td><td> 90.0 </td><td> 88.3 </td><td> 79.1 </td><td> 88.4 </td><td> 88.7 </td></tr><tr><td> 烘烤24h </td><td> 88.1 </td><td> 89.2 </td><td> 88.6 </td><td> 88.3 </td><td> 86.7 </td><td> 85.0 </td><td> 78.6 </td><td> 88.6 </td><td> 88.1 </td></tr><tr><td> 烘烤72h </td><td> 87.4 </td><td> 88.7 </td><td> 88.2 </td><td> 85.4 </td><td> 86.7 </td><td> 80.7 </td><td> 75.3 </td><td> 85.4 </td><td> 85.3 </td></tr><tr><td> 烘烤120h </td><td> 86.6 </td><td> 88.1 </td><td> 87.3 </td><td> 84.9 </td><td> 86.2 </td><td> 75.5 </td><td> 74.5 </td><td> 84.8 </td><td> 84.6 </td></tr><tr><td> 耐熱 穩定<img wi="2" he="2" file="IMG-2/Draw/02_image003.gif" img-format="jpg"></img>性 （分解2%溫度）℃ </td><td> 601.3 </td><td> 621.7 </td><td> 686.9 </td><td> 594.2 </td><td> 598.5 </td><td> 389.4 </td><td> 576.3 </td><td> 596.7 </td><td> 456.2 </td></tr><tr><td> 剝離強度測試N/mm </td><td> 0.58 </td><td> 0.61 </td><td> 0.65 </td><td> 0.56 </td><td> 0.56 </td><td> 0.41 </td><td> 0.54 </td><td> 0.27 </td><td> 0.50 </td></tr></TBODY></TABLE>
物性分析：從上表的資料可以看出，實施例1~5常溫下具有很好光的反射率，且在高溫下長期烘烤仍然能保持很好的光反射率，同時其在高溫下穩定性也較好，剝離強度較高，完全能符合LED白色層壓板的需求。而對比例1與實施例2相比，樹脂為甲基乙烯基矽樹脂，為加成型固化方式，覆銅板高溫反射率、耐高溫性和剝離強度都較差；對比例2與實施例1相比，由於白色填料含量較少，其常溫反射率和高溫反射率較差；對比例3與實施例3相比，由於白色填料超過範圍，導致與銅箔的剝離強度降低，無法正常使用；對比例4與實施例3相比，R/Si非常高，導致板材偏軟，並且固化不完全，其耐熱性較差。
申請人聲明，本發明通過上述實施例來說明本發明的詳細方法，但本發明並不局限於上述詳細方法，即不意味著本發明必須依賴上述詳細方法才能實施。所屬技術領域的技術人員應該明瞭，對本發明的任何改進，對本發明產品各原料的等效替換及輔助成分的添加、具體方式的選擇等，均落在本發明的保護範圍和公開範圍之內。

Claims (10)

  1. 一種有機矽樹脂組合物，其特徵在於，所述有機矽樹脂組合物，包括：縮合型矽樹脂：100重量份；白色填料：5~60重量份；催化劑：0.0001~2重量份；和助劑：0.1~10重量份；其中，所述縮合型矽樹脂為R/Si=1.0~1.7(摩爾比)和Ph/(Me+Ph)=0~1.0(摩爾比)的甲基矽樹脂、甲基苯基矽樹脂或苯基矽樹脂中的任意一種或者至少兩種的混合物，其中Ph代表苯基基團，Me代表甲基基團，R代表有機官能團-CH3、-Ph、-OCH3、-OCH2CH3、-H或-OH。
  2. 如申請專利範圍第1項所述的有機矽樹脂組合物，其中，所述縮合型矽樹脂為R/Si=1.2~1.7(摩爾比)且Ph/(Me+Ph)=0.2-0.6(摩爾比)的甲基苯基矽樹脂。
  3. 如申請專利範圍第1或2項中任一項所述的有機矽樹脂組合物，其特徵在於，所述白色填料為氧化鋁、二氧化鈦、氫氧化鋁、二氧化矽或氧化鋅中的任意一種或者至少兩種的混合物。
  4. 如申請專利範圍第1或2項中任一項所述的有機矽樹脂組合物，其特徵在於，所述白色填料為二氧化鈦。
  5. 如申請專利範圍第1或2項中任一項所述的有機矽樹脂組合物，其特徵在於，所述催化劑是環烷酸鋅、環烷酸錫、環烷酸鈷、環烷酸鐵、環烷酸鈰、羧酸鋅、羧酸錫、羧酸鈷、羧酸鐵、羧酸鈰、全氟磺酸、氯化磷腈、胺類、 辛酸鋅、異辛酸鋅、季銨堿、鈦酸酯或胍類化合物等中的任意一種或者至少兩種的組合。
  6. 如申請專利範圍第1或2項中任一項所述的有機矽樹脂組合物，其特徵在於，所述助劑為偶聯劑或/和分散劑，所述偶聯劑為矽烷偶聯劑或/和鈦酸酯偶聯劑。
  7. 一種樹脂膠液，其特徵在於，其是將如申請專利範圍第1或2項中任一項所述的有機矽樹脂組合物溶解或分散在溶劑中得到。
  8. 一種白色預浸料，其特徵在於，其包括增強材料及通過含浸乾燥後附著在增強材料上的如申請專利範圍第1或2項中任一項所述的矽樹脂組合物。
  9. 一種白色層壓板，其特徵在於，所述白色層壓板含有至少一張如如申請專利範圍第8項所述的白色預浸料。
  10. 一種白色覆銅箔層壓板，其特徵在於，所述白色覆銅箔層壓板包括至少一張疊合的如申請專利範圍第8項所述的白色預浸料及壓覆在疊合後的預浸料的一側或兩側的銅箔。
TW104111511A 2014-12-25 2015-04-10 Organic silicon resin compositions and white prepregs and white laminates using it TWI530533B (zh)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410829372.5A CN105778505B (zh) 2014-12-25 2014-12-25 一种有机硅树脂组合物以及使用它的白色预浸料和白色层压板

Publications (2)

Publication Number Publication Date
TWI530533B true TWI530533B (zh) 2016-04-21
TW201623451A TW201623451A (zh) 2016-07-01

Family

ID=56149106

Family Applications (1)

Application Number Title Priority Date Filing Date
TW104111511A TWI530533B (zh) 2014-12-25 2015-04-10 Organic silicon resin compositions and white prepregs and white laminates using it

Country Status (7)

Country Link
US (1) US10336905B2 (zh)
EP (1) EP3239245B1 (zh)
JP (1) JP6510650B2 (zh)
KR (1) KR101909851B1 (zh)
CN (1) CN105778505B (zh)
TW (1) TWI530533B (zh)
WO (1) WO2016101537A1 (zh)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102101704B1 (ko) * 2018-09-05 2020-04-20 삼성전기주식회사 적층 세라믹 전자부품
CN110112341B (zh) * 2019-04-19 2022-05-17 宁波芯合为一电子科技有限公司 一种电池模块用受热膨胀材料及电池模块
CN110128997A (zh) * 2019-05-17 2019-08-16 陈定方 一种有效提高导热系数的有机硅灌封胶及制备方法
CN111599925B (zh) * 2020-05-29 2021-09-21 河南大学 一种以双（甲酸）二甲基锡n型半导体薄膜作为电子传输层的太阳能电池及其制备方法
CN111690370A (zh) * 2020-06-29 2020-09-22 广东昭信照明科技有限公司 一种复合陶瓷材料围坝胶及其紫外led陶瓷封装基板的制备方法
CN113801628A (zh) * 2021-10-20 2021-12-17 烟台德邦科技股份有限公司 一种uv固化有机硅披覆胶及其制备方法
CN115339175B (zh) * 2022-09-26 2023-08-18 苏州苏绝电工材料股份有限公司 一种有机硅层压玻璃布板及其制备方法
CN117594735B (zh) * 2023-11-20 2024-04-30 南通惟怡新材料科技有限公司 一种层压板及其制备方法

Family Cites Families (42)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3018270A (en) * 1960-07-28 1962-01-23 Union Carbide Corp Process for producing silicone resins
JPS5734150A (en) * 1980-08-08 1982-02-24 Toray Silicone Co Ltd Organopolysiloxane resin composition
US4657986A (en) * 1984-12-26 1987-04-14 Kanegafuchi Chemical Industry Co., Ltd. Curable resinous composition comprising epoxy resin and silicon-containing elastomeric polymer
US5280098A (en) * 1992-09-30 1994-01-18 Dow Corning Corporation Epoxy-functional silicone resin
JP3121188B2 (ja) * 1993-10-26 2000-12-25 信越化学工業株式会社 耐水性に優れた室温速硬化性オルガノポリシロキサン組成物、その硬化方法及びそれにより得られる硬化物
JP3031821B2 (ja) * 1994-07-21 2000-04-10 信越化学工業株式会社 耐熱性の改良された積層板
KR100272785B1 (ko) * 1995-06-27 2000-11-15 우찌가사끼 이사오 인쇄배선판용프리프래그,수지니스,수지조성물및상기물질을사용하여제조된인쇄배선판용적층판
KR101001121B1 (ko) * 2002-10-22 2010-12-14 유겡가이샤 소피아 프로덕트 광소자용 봉착재 조성물, 봉착 구조체 및 광소자
US20050021566A1 (en) * 2003-05-30 2005-01-27 Arkivio, Inc. Techniques for facilitating backup and restore of migrated files
DE102004005222A1 (de) * 2004-02-03 2005-08-18 Degussa Ag Silikonkautschuk
US6992440B2 (en) * 2004-02-26 2006-01-31 Asahi Glass Company, Limited Light-emitting device and process for its production
US7732496B1 (en) * 2004-11-03 2010-06-08 Ohio Aerospace Institute Highly porous and mechanically strong ceramic oxide aerogels
JP4791083B2 (ja) * 2005-05-30 2011-10-12 信越化学工業株式会社 光関連デバイス封止用樹脂組成物およびその硬化物
JP2007012876A (ja) 2005-06-30 2007-01-18 Asahi Glass Co Ltd 回路基板用積層体およびその製造方法
JP2007106944A (ja) * 2005-10-17 2007-04-26 Shin Etsu Chem Co Ltd 室温硬化性オルガノポリシロキサン組成物
DE102006033976A1 (de) 2006-07-22 2008-01-31 Dr.Ing.H.C. F. Porsche Ag Abgasturbolader für eine Brennkraftmaschine
JP5057022B2 (ja) 2006-10-13 2012-10-24 信越化学工業株式会社 コーティング用エマルジョン組成物
MY148660A (en) * 2007-04-10 2013-05-15 Sumitomo Bakelite Co Resin composition, prepreg, laminated board, multilayer printed wiring board and semiconductor device
US8258251B2 (en) * 2007-11-30 2012-09-04 The United States Of America, As Represented By The Administrator Of The National Aeronautics And Space Administration Highly porous ceramic oxide aerogels having improved flexibility
EP2222807A2 (en) * 2007-12-05 2010-09-01 Corinne Jean Greyling A polymeric high voltage insulator with a hard, hydrophobic surface
JP4623322B2 (ja) * 2007-12-26 2011-02-02 信越化学工業株式会社 光半導体ケース形成用白色熱硬化性シリコーン樹脂組成物並びに光半導体ケース及びその成形方法
JP4678415B2 (ja) 2008-03-18 2011-04-27 信越化学工業株式会社 光半導体ケース形成用白色熱硬化性シリコーン樹脂組成物並びに光半導体ケース
CN101565600A (zh) * 2008-05-14 2009-10-28 广州市回天精细化工有限公司 低硬度高柔韧性的双组分缩合型有机硅灌封胶组合物
JP2010018786A (ja) * 2008-06-09 2010-01-28 Shin-Etsu Chemical Co Ltd 光半導体ケース形成用白色熱硬化性シリコーン樹脂組成物及び光半導体ケース
JP2010021533A (ja) * 2008-06-09 2010-01-28 Shin-Etsu Chemical Co Ltd 光半導体ケース形成用白色熱硬化性シリコーン樹脂組成物及び光半導体ケース
CN101381515A (zh) * 2008-09-26 2009-03-11 哈尔滨工业大学 硅树脂基复合材料的制备方法
JP2010106243A (ja) * 2008-09-30 2010-05-13 Shin-Etsu Chemical Co Ltd 光半導体装置用シリコーン樹脂組成物
JP5108825B2 (ja) * 2009-04-24 2012-12-26 信越化学工業株式会社 光半導体装置用シリコーン樹脂組成物及び光半導体装置
CN101724268B (zh) * 2009-11-27 2012-12-05 佛山市金银河机械设备有限公司 硅酮胶的生产方法
JP5463586B2 (ja) * 2009-12-21 2014-04-09 利昌工業株式会社 プリプレグ、積層板、及び金属箔張り積層板
KR101763975B1 (ko) * 2010-05-07 2017-08-01 스미토모 베이클리트 컴퍼니 리미티드 회로 기판용 에폭시 수지 조성물, 프리프레그, 적층판, 수지 시트, 프린트 배선판용 적층기재, 프린트 배선판, 및 반도체 장치
US20140194019A1 (en) * 2010-12-22 2014-07-10 Dow Corning Corporation Silicone Composition, Silicone Adhesive, Coated and Laminated Substrates
US8735733B2 (en) * 2011-01-18 2014-05-27 Hitachi Chemical Company, Ltd. Resin composition, prepreg laminate obtained with the same and printed-wiring board
US9079376B2 (en) * 2011-01-18 2015-07-14 Hitachi Chemical Company, Ltd. Prepreg, laminate obtained with the same and printed-wiring board
CN103328543B (zh) * 2011-01-18 2015-07-15 日立化成株式会社 改性硅酮化合物,使用其的热固化性树脂组合物、预浸料坯、层叠板和印刷布线板
CN102181264B (zh) * 2011-04-15 2013-03-13 东莞兆舜有机硅新材料科技有限公司 一种高性能光伏组件用有机硅密封胶及其制备方法
JP6026095B2 (ja) * 2011-10-31 2016-11-16 太陽インキ製造株式会社 熱硬化性樹脂組成物及びその硬化物、並びにそれを用いたプリント配線板
JP5650092B2 (ja) 2011-11-01 2015-01-07 信越化学工業株式会社 シリコーンプリプレグ、それを用いたシリコーン樹脂板、シリコーン金属張積層板、シリコーン金属ベース基板及びｌｅｄ実装基板
JP5729270B2 (ja) 2011-11-21 2015-06-03 信越化学工業株式会社 Ｌｅｄリフレクターとして有用な白色熱硬化性シリコーン樹脂組成物及び該組成物を用いた光半導体装置
KR101881604B1 (ko) * 2011-11-21 2018-07-24 신에쓰 가가꾸 고교 가부시끼가이샤 Ｌｅｄ 리플렉터로서 유용한 백색 열경화성 실리콘 수지 조성물 및 상기 조성물을 이용한 광반도체 장치
JP5941847B2 (ja) * 2013-01-17 2016-06-29 信越化学工業株式会社 シリコーン・有機樹脂複合積層板及びその製造方法、並びにこれを使用した発光半導体装置
JP5996085B2 (ja) * 2013-02-27 2016-09-21 株式会社朝日ラバー 白色反射膜用インク、白色反射膜用粉体塗料及び白色反射膜の製造方法

Also Published As

Publication number Publication date
JP2018507279A (ja) 2018-03-15
CN105778505A (zh) 2016-07-20
WO2016101537A1 (zh) 2016-06-30
EP3239245A1 (en) 2017-11-01
KR20170100625A (ko) 2017-09-04
US20180016436A1 (en) 2018-01-18
EP3239245B1 (en) 2021-01-13
TW201623451A (zh) 2016-07-01
EP3239245A4 (en) 2018-08-22
KR101909851B1 (ko) 2018-12-18
US10336905B2 (en) 2019-07-02
CN105778505B (zh) 2019-04-30
JP6510650B2 (ja) 2019-05-08

Similar Documents

Publication Publication Date Title
TWI530533B (zh) Organic silicon resin compositions and white prepregs and white laminates using it
TWI685495B (zh) 含有縮水甘油基乙炔脲類的組成物
TWI500511B (zh) 矽氧積層基板及其製法、矽氧樹脂組成物以及ｌｅｄ裝置
JP2018523592A (ja) オルガノシリコーン樹脂アルミベース銅張積層板及びその調製方法
TWI767249B (zh) 環氧改性矽樹脂組合物及其應用
KR102235501B1 (ko) 무기충전재 및 이를 포함하는 에폭시 수지 조성물
JP5650092B2 (ja) シリコーンプリプレグ、それを用いたシリコーン樹脂板、シリコーン金属張積層板、シリコーン金属ベース基板及びｌｅｄ実装基板
TW201623454A (zh) 無鹵無磷矽樹脂組合物以及使用它的預浸料、層壓板和印製電路板
CN103459493A (zh) 树脂组合物、预浸料及覆金属箔层压板
CN103492481A (zh) 树脂组合物、预浸料和覆金属箔层压板
TW201412879A (zh) 樹脂片、附設樹脂層之支持體、疊層板及覆金屬箔疊層板
JP5099911B2 (ja) 熱硬化性組成物及び光半導体装置
JP2011042760A (ja) 熱硬化性シリコーン樹脂用組成物
TWI777939B (zh) 覆銅層合板及其製造方法
JP2010280807A (ja) ポリイミド樹脂用組成物
JP2018030977A (ja) シリコーン樹脂基板、金属層形成シリコーン樹脂基板、シリコーン樹脂硬化基板及び金属層形成シリコーン樹脂硬化基板
JP5517042B2 (ja) 接着剤樹脂組成物、接着剤シート
JP6575699B2 (ja) プリント配線板用樹脂組成物、プリプレグ、樹脂シート、積層板、金属箔張積層板、プリント配線板、及び多層プリント配線板
JP6645911B2 (ja) シリコーン樹脂基板及びその製造方法、並びに光半導体装置
JP6023677B2 (ja) シアネートエステル樹脂プリプレグ、積層基板、シアネートエステル樹脂金属張積層板、及びｌｅｄ実装基板
JP2014099439A (ja) 半導体ウエハ用保護フィルム及び半導体チップの製造方法
JP2021138926A (ja) 樹脂膜の製造方法およびそれを用いたフレキシブルデバイスの製造方法
JP2017039854A (ja) 熱硬化性白色コート剤用ポリエステル樹脂組成物
JP2016199645A (ja) 熱硬化性白色コート剤及びそれを用いた基板
JP2006036913A (ja) 樹脂ペーストの製造方法及び樹脂ペースト