CN106364067A - P10 copper-clad laminate - Google Patents
P10 copper-clad laminate Download PDFInfo
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- CN106364067A CN106364067A CN201610755394.0A CN201610755394A CN106364067A CN 106364067 A CN106364067 A CN 106364067A CN 201610755394 A CN201610755394 A CN 201610755394A CN 106364067 A CN106364067 A CN 106364067A
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- 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
- B32B5/22—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
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- 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
- B32B2255/00—Coating on the layer surface
- B32B2255/02—Coating on the layer surface on 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
- B32B2255/00—Coating on the layer surface
- B32B2255/26—Polymeric coating
-
- 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
- B32B2307/70—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
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
-
- 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
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/206—Organic displays, e.g. OLED
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a P10 copper-clad laminate. A preparation method of the P10 copper-clad laminate includes the steps: (1) stacking a plurality of pieces of prepreg to form a lamination, and coating copper foils on one surface or two surfaces of two outer side surfaces of the lamination to obtain a semi-finished product; (2) performing hot pressing for the semi-finished product to obtain the P10 copper-clad laminate. Glue solution for preparing the P10 copper-clad laminate comprises, by weight, 300-400 parts of liquid epoxy resin, 100-200 parts of solid epoxy resin, 175-235 parts of phenolic resin, 0.3-0.4 part of curing accelerator, 280-360 parts of solvents, 100-600 parts of inorganic fillers and 0.5-1.0 part of fluorescent whitening agent. The P10 copper-clad laminate has excellent adhesion, ultraviolet-resistant functions, acid and alkali resistance, solvent resistance and heat resistance and is whiter, flat and bright as compared with an existing product, so that LED (light-emitting diode) light is whiter, brighter and more colorful.
Description
Technical field
The present invention relates to a kind of p10 copper-clad plate.
Background technology
In recent years, a class resistance to ultra violet discoloration and resistance to thermochromism is excellent, LED lamp light radiation output is high copper-clad plate (p10
Copper-clad plate), rapidly developed in led (light emitting diode) application.It has become and has met particularity in copper-clad plate
The class product that can require.
However, temperature rising can make transparent epoxy resin degree be decreased obviously, barton research finds that temperature reaches 140 DEG C
When, epoxy resin serious degradation, affect LED lamp service life, when temperature reaches 150 DEG C, transparent epoxy resin degree is decreased obviously,
Thus leading to LED lamp light radiation output to weaken.
Presently, generally adopt plus appropriate inorganic filler reduces copper-clad plate thermal coefficient of expansion.Copper Foil, glass-fiber-fabric, resin
Three's thermal coefficient of expansion difference is larger, adds appropriate filler can alleviate the difference of expanding with heat and contract with cold of three, so can avoid high temperature
Lower three deforms different led to circuit deformation fracture, to avoid causing catastrophic to lose efficacy.But p10 copper-clad plate is come
Say, its production cost is still higher at present, and resin transparent degree under high temperature declines and yet suffers from, service life and resistance to ultraviolet
Linearly can need to be improved further.
Content of the invention
Technical problem solved by the invention is to overcome the high cost of existing p10 copper-clad plate, resistance to acids and bases and resistance to
Hot and epoxy resin the defect such as weakens because temperature resistant transparent degree reduces impact LED lamp light radiation output, there is provided a kind of p10 covers
Copper coin glue, prepreg and copper-clad plate and preparation method.The glue of the present invention not only has good adhesive force and anti-purple
Outside line function, also has good thermostability, has excellent resistance to acids and bases, solvent resistance, thermostability.Glue by the present invention
The prepreg being obtained further has the physicochemical property as it with copper-clad plate, and more existing product is whiter and smooth
Light, can make led light seem whiter, brighter and more bright-coloured.
The present invention solves above-mentioned technical problem by the following technical programs.
The invention provides a kind of p10 glue solution for copper-clad plate, it is obtained by following raw materials, and described raw material includes following weight
The component of part: 300-400 part liquid-state epoxy resin, 100-200 part solid epoxy resin, 175-235 part phenolic resin, 0.3-
0.4 part of curing accelerator, 280-360 part solvent, 100-600 part inorganic filler and 0.5-1.0 part fluorescent whitening agent.
Wherein, described liquid-state epoxy resin and described solid epoxy resin can be using various normal in this area copper-clad plate glue
The epoxy resin that rule use；Described liquid-state epoxy resin is preferably bisphenol type liquid-state epoxy resin, more preferably for Bisphenol A Type liquid
State epoxy resin.Described solid epoxy resin is preferably bisphenol type solid epoxy resin, more preferably for Bisphenol A Type solid epoxidic
Resin.In the present invention, using the different epoxy resin of polymerization degree n (molecular weight or epoxide equivalent).In general, epoxide equivalent is got over
High (molecular weight is bigger) pliability is better, thus improving the pliability of sheet material；Increase curing reaction degree simultaneously, shorten reaction
Time.In the present invention, arranged in pairs or groups using solid and liquid-state epoxy resin simultaneously, the flatulence of heat type of prepreg being subsequently obtained can be made
Contraction coefficients are minimum, have anti-ultraviolet function.The epoxide equivalent of described liquid-state epoxy resin is preferably 195-200g/eq
(i.e. gram/equivalent)；The epoxide equivalent of described solid epoxy resin is preferably 980-1070g/eq.
The parts by weight of described liquid-state epoxy resin are preferably 320-380 part；The weight portion of described solid epoxy resin
Number is preferably 120-180 part.
In the present invention, phenolic resin is used for replacing conventional use of dicyandiamide at present, uses as firming agent.Invention Crinis Carbonisatus
Existing, subotituted dicyardiamide is come using phenolic resin, it can not only strengthen toughness, cohesion is strong, excellent storage stability, moulded manufacturability
Good, can also act as resin content, thus reducing the input amount of epoxy resin.
Preferably 80-120 DEG C of the softening point of described phenolic resin, more preferably for 85-100 DEG C, such as 95-100 DEG C.This
In invention, described softening point refers to the temperature of material softening, refers generally to the temperature that amorphous polymer starts during deliquescing, the i.e. present invention
Described in phenolic resin start temperature during deliquescing.
The parts by weight of described phenolic resin are preferably 190-210 part.
Wherein, described curing accelerator can be curing accelerator commonly used in the art, preferably imidazoles solidification
Accelerator, more preferably for 2-methylimidazole and/or 2- phenylimidazole.The parts by weight of described curing accelerator are preferably
0.35-0.40 part.Described curing accelerator is 2-methylimidazole and during 2- phenylimidazole, described 2-methylimidazole and 2- phenyl miaow
The weight of azoles is than preferably (1-2): (4-5).
Wherein, described solvent can be solvent commonly used in the art, preferably ketones solvent and/or ether solvent,
It is more preferably one or more of acetone, butanone and propylene glycol monomethyl ether.The parts by weight of described solvent are preferably 360-370
Part.When described solvent is acetone, butanone and propylene glycol monomethyl ether, the weight of described acetone, butanone and propylene glycol monomethyl ether is than preferably
Ground is (2-4): (1-3): (1-2).
Wherein, described inorganic filler can be inorganic filler commonly used in the art, preferably aluminium hydroxide, hydroxide
One or more of magnesium, calcium oxide, silicon dioxide and Pulvis Talci.The parts by weight of described inorganic filler are preferably 100-
300 parts.When described inorganic filler is aluminium hydroxide, silicon dioxide and Pulvis Talci, described aluminium hydroxide, silicon dioxide and Talcum
The weight of powder is than preferably (3-5): (6-8): (1-2).
Wherein, described fluorescent whitening agent can be the fluorescent whitening agent being usually used in the fabric brightenings such as cotton and nylon, preferably
The sunwhite line fluorescent brightening agent that (granary) Fine Chemical Co., Ltd of rising sun Thailand produces, such as sunwhite fg-e fluorescence increase
White agent.In the present invention, employ fluorescent whitening agent, (wave-length coverage is about 60- not only can to absorb sightless ultraviolet light
380nm), it is converted into the visible ray of longer wavelengths of blue light or purple, and then compensate undesired micro- Huang in sheet material substrate
Color, reflects the original incident more visible rays (wavelength is in 400-600nm) of ratio simultaneously, so as to use in follow-up copper-clad plate
In make led light seem whiter, brighter, more bright-coloured.
Present invention also offers a kind of preparation method of p10 glue solution for copper-clad plate, it comprises the steps:
(1) under agitation, mixture a is mixed with described liquid-state epoxy resin；Then with 2500-3000rpm's
Speed carries out shearing 3-5 hour, then is mixed with mixture b, obtains mixture c；
Described mixture a is mixed to get by the described solvent of described solid epoxy resin and 40%-60%；Described mixture
B is mixed to get by described phenolic resin and remaining described solvent；
(2) under agitation, described mixture c, described curing accelerator and described fluorescent whitening agent are mixed, then
Mix with described inorganic filler again, sheared with the speed of 2000-3000rpm, obtain final product after ripening.
By common sense in the field, when solvent adopts multi-solvents species, use after in advance all solvents being mixed, institute
State mixing to be defined by mix homogeneously, stir 0.1-0.2 hour preferably under the rotating speed of 500-800rpm.
In the preparation of described mixture a, described mixing is so that described solid epoxy resin is completely dissolved and is defined, preferably
It is that 6-8 hour is stirred with the rotating speed of 1500-2000rpm.
In the preparation of described mixture b, described mixing so that described phenolic resin is completely dissolved and is defined, preferably with
The rotating speed stirring 6-8 hour of 1500-2000rpm.
In step (1), the method for described stirring and condition can be the conventional method in this area and condition.Described stirring turn
Speed is preferably 1500-2000rpm.The time of described stirring is preferably 3-5 hour.
In step (1), the method for " being mixed with mixture b " and condition can be the conventional method in this area and condition,
Preferably 3-5 hour is stirred with the rotating speed of 1500-2000rpm.
In step (2), the time of described shearing is preferably 0.5-1.5 hour.The speed of described shearing is preferably
2000-2500rpm.
In step (2), the method for described ripening and condition can be the conventional method in this area and condition.Described ripening is relatively
It is that 6-10 hour is stirred with the rotating speed of 1000-1500rpm goodly.
Present invention also offers a kind of preparation method of p10 copper-clad plate prepreg, it comprises the steps: in electronics
Described p10 glue solution for copper-clad plate is coated on grade fiberglass cloth, after drying, obtains final product.
Described E-glass cloth is the E-glass cloth in conventional use of prepreg raw material in this area.
It is preferred that described E-glass cloth is electronic-grade glass fiber cloth 7628.
It is preferred that the equipment of described coating is gluing machine.
It is preferred that the speed of described coating is 17-25m/min；It is more preferably 16-19m/min, such as 18m/min.
It is preferred that the temperature of described drying is 170-230 DEG C；More preferably it is 200-220 DEG C.
Present invention also offers a kind of p10 copper-clad plate prepreg being obtained by above-mentioned preparation method.
In the present invention, the resin content (rc) of described p10 copper-clad plate prepreg is generally 40-60%.Described p10 covers
The gel time (gt) of copper coin prepreg is generally 65-85s.Described p10 copper-clad plate prepreg fluidity (rf)
As be 18-25%.The fugitive constituent of described p10 copper-clad plate prepreg is typically below 0.25%.4 inch of * 4 inch area
The weight (ppw) of described p10 copper-clad plate prepreg is typically in 4.0-4.6g.
Present invention also offers a kind of preparation method of p10 copper-clad plate, it comprises the steps:
1. lamination: several described prepregs are carried out folding and joins, form lamination；Two lateral surface of lamination one side or
It is covered with Copper Foil on two sides, obtain semi-finished product；
2. described semi-finished product are carried out hot pressing compacting, obtain final product.
In the present invention, the described folded method stacking prepreg joined for copper-clad plate preparation technology field routine, usually
Neatly stacked with several prepregs of size and shape identical, i.e. the stacking of each side all alignment of prepreg.This
In invention, described folded join do not need pressure, described folded join typically follow four big principles: gel content high level matches with low level principle, cloth type one
Cause principle, symmetrical configuration principle and left and right collocating principle.
Step 1. in, described Copper Foil can be Copper Foil commonly used in the art.
Step 2. in, the method for described hot pressing compacting and condition can be the conventional method in this area and condition.Described hot pressing
The pressure of compacting is preferably 20-40kg/cm2；Preferably 90-220 DEG C of the temperature of described hot pressing compacting；Described hot pressing compacting
Time be preferably 80-120min.
In the present invention, the preparation method of described copper-clad plate, typically also carry out follow-up sharp processing and inspection process, with true
Protect the quality of product.
Present invention also offers a kind of p10 copper-clad plate obtained by described preparation method.
On the basis of meeting common sense in the field, above-mentioned each optimum condition, can combination in any, obtain final product each preferable reality of the present invention
Example.
Agents useful for same of the present invention and raw material are all commercially available.
The positive effect of the present invention is:
The p10 glue solution for copper-clad plate of the present invention not only has good adhesive force and anti-ultraviolet function, also has very well
Thermostability, there is excellent resistance to acids and bases, solvent resistance, thermostability.The semi-solid preparation being obtained further by the glue of the present invention
Piece has the physicochemical property as it with copper-clad plate, and more existing product is whiter and smooth, and led light can be made to show
Get Geng Bai, brighter and more bright-coloured.
Specific embodiment
Further illustrate the present invention below by the mode of embodiment, but therefore do not limit the present invention to described reality
Apply among a scope.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or according to business
Product description selects.
In following embodiments, number used is parts by weight.
In following embodiments, fluorescent whitening agent used is that (granary) Fine Chemical Co., Ltd of rising sun Thailand produces
Sunwhite fg-e system fluorescent whitening agent.
In following embodiments, the epoxide equivalent of the Bisphenol A Type liquid-state epoxy resin being used is 195-200g/eq；Made
The epoxide equivalent of Bisphenol A Type solid epoxy resin is 980-1070g/eq.
Embodiment 1
The composition of raw materials of p10 glue solution for copper-clad plate is as follows:
(softening point is for 370 parts of Bisphenol A Type liquid-state epoxy resin, 160 parts of Bisphenol A Type liquid-state epoxy resin, phenolic resin
95-100 DEG C) 200 parts, 0.20 part of 2- phenylimidazole, 0.15 part of 2-methylimidazole, 140 parts of acetone, 100 parts of butanone, propylene glycol first
130 parts of ether, 300 parts of aluminium hydroxide, 100 parts of soft silicon, 50 parts of Pulvis Talci and 0.5 part of fluorescent whitening agent.
The preparation method of glue is as follows:
(1) acetone, butanone and propylene glycol monomethyl ether are stirred 0.1 hour under the rotating speed of 500rpm and obtain mixed solvent；Take
Half mixed solvent is mixed with solid epoxy resin, is stirred 6 hours with 1500 rotating speed, obtains mixture a；Take another meromict
Solvent is mixed with phenolic resin, is stirred 6 hours with the rotating speed of 1500rpm, obtains mixture b；
Under the speed of agitator of 1500rpm, mixture a is mixed with liquid-state epoxy resin, stir 6-8 hour, then with
The speed of 2500rpm carries out shearing 6 hours；Mixed then at mixture b, stirred 3 hours with the rotating speed of 1500rpm, obtain
Mixture c；
(2) under agitation, mixture c, 2- phenylimidazole, 2-methylimidazole and fluorescent whitening agent are mixed, then
Mix with aluminium hydroxide, soft silicon and Pulvis Talci, carry out shearing 0.5 hour with the speed of 2000rpm, in turning with 1000rpm
Speed stirring carries out ripening in 6 hours, obtains final product.
The preparation method of p10 copper-clad plate prepreg: institute is coated on electronic-grade glass fiber cloth 7628 with gluing machine
State p10 glue solution for copper-clad plate, after drying, obtain final product.The control parameter of p10 copper-clad plate prepreg is as follows:
Oven for gluing machine temperature: 210 DEG C；
Gluing speed: 19m/min；
Resin content: rc is up to 45%；
The gel time gt:70s of prepreg；
The fluidity rf:19% of prepreg；
The fugitive constituent vc:0.25% of prepreg；
Weight ppw:4.2g of prepreg.
The preparation method of p10 copper-clad plate (1.5mm plate) is as follows:
1. lamination: 6 7628 prepregs are carried out folding and joins, form lamination；One side overlying in two lateral surface of lamination
The Copper Foil of upper 12 μ m-thick, obtains semi-finished product；
2. semi-finished product are carried out hot pressing compacting, obtain final product；Hot pressing pressure: 30kg/cm2；Hot pressing press temperature: 175 DEG C；Hot pressing
Press time: 80min.
After testing, the performance parameter of obtained p10 copper-clad plate is as shown in table 1.
Table 1
| Pilot project | Unit | Examination criteria | Embodiment 1 |
| 1. heat decomposition temperature (td) | ℃ | 10 DEG C/min, n, 5%wtloss | 401 |
| 2. anti-flammability | - | ul94v-0 | v-0 |
| 3. thermal stress, 288 DEG C, 20 seconds | - | Surface is no layered, no bubbles | No destroy |
| 4. thermostability, 288 DEG C (tma method) | min | ≥30 | 60 |
| 5.tg value, (dsc method) | ℃ | ≥170 | 180 |
| 6. water absorption rate, maximum | % | ≤0.5 | 0.12 |
| 7. chemical resistance (process solvent infusion method) | - | 60 minutes colour-fast | No destroy |
| 8. peel strength | lbs/in | ≥5 | 8.1 |
From table 1, the p10 copper-clad plate combination property obtained by embodiment 1 is good.
Additionally, carrying out ocular estimate to obtained p10 copper-clad plate with prepreg, it is commercially for respect to existing
The prepreg preparing p10 copper-clad plate is whiter, and more smooth；After testing, carry out aging examination at 140-150 DEG C
Test, reduce under the transparency of this p10 copper-clad plate prepreg, therefore obtained p10 copper-clad plate making in actual use
With life-span length, and do not result in LED lamp light radiation output and weaken.
Embodiment 2
The composition of raw materials of p10 glue solution for copper-clad plate is as follows:
350 parts of Bisphenol A Type liquid-state epoxy resin, 150 parts of Bisphenol A Type solid-liquid epoxy resin, phenolic resin (softening point
For 95-100 DEG C) 205 parts, 0.10 part of 2- phenylimidazole, 0.25 part of 2-methylimidazole, 130 parts of acetone, 110 parts of butanone, propylene glycol
130 parts of methyl ether, 350 parts of aluminium hydroxide, 50 parts of silica 1,60 parts of Pulvis Talci and 0.6 part of fluorescent whitening agent.
The preparation method of glue is as follows:
(1) acetone, butanone and propylene glycol monomethyl ether are stirred 0.2 hour under the rotating speed of 800rpm and obtain mixed solvent；Take
40% mixed solvent is mixed with solid epoxy resin, is stirred 8 hours with the rotating speed of 2000rpm, obtains mixture a；Take remaining mixed
Bonding solvent is mixed with phenolic resin, is stirred 8 hours with the rotating speed of 2000rpm, obtains mixture b；
Under the speed of agitator of 2000rpm, mixture a is mixed with liquid-state epoxy resin, stir 8 hours, then with
The speed of 3000rpm carries out shearing 8 hours；Mixed then at mixture b, 3-5 hour is stirred with the rotating speed of 2000rpm, obtains
To mixture c；
(2) under agitation, mixture c, 2- phenylimidazole, 2-methylimidazole and fluorescent whitening agent are mixed, then
Mix with aluminium hydroxide, silicon dioxide and Pulvis Talci, carry out shearing 1.5 hours with the speed of 2500rpm, with 1500rpm's
Rotating speed stirring carries out ripening in 10 hours, obtains final product.
The preparation method of p10 copper-clad plate prepreg: institute is coated on electronic-grade glass fiber cloth 7628 with gluing machine
State p10 glue solution for copper-clad plate, after drying, obtain final product.The control parameter of p10 copper-clad plate prepreg is as follows:
Oven for gluing machine temperature: 220 DEG C；
Gluing speed: 21m/min；
Resin content: rc is up to 55%；
The gel time gt:75s of prepreg；
The fluidity rf:18% of prepreg；
The fugitive constituent vc:0.20% of prepreg；
Weight ppw:4.1g of prepreg.
The preparation method of p10 copper-clad plate (1.0mm plate) is as follows:
1. lamination: 4 7628 prepregs are carried out folding and joins, form lamination；Two sides overlying in two lateral surface of lamination
The Copper Foil of upper 15 μ m-thick, obtains semi-finished product；
2. semi-finished product are carried out hot pressing compacting, obtain final product；Hot pressing pressure: 32kg/cm2；Hot pressing press temperature: 185 DEG C；Hot pressing
Press time: 90min.
After testing, the performance parameter of obtained p10 copper-clad plate is as shown in table 2.
Table 2
| Pilot project | Unit | Examination criteria | Embodiment 1 |
| 1. heat decomposition temperature (td) | ℃ | 10 DEG C/min, n, 5%wtloss | 385 |
| 2. anti-flammability | - | ul94v-0 | v-0 |
| 3. thermal stress, 288 DEG C, 20 seconds | - | Surface is no layered, no bubbles | No destroy |
| 4. thermostability, 288 DEG C (tma method) | min | ≥30 | 80 |
| 5.tg value, (dsc method) | ℃ | ≥170 | 175 |
| 6. water absorption rate, maximum | % | ≤0.5 | 0.19 |
| 7. chemical resistance (process solvent infusion method) | - | 60 minutes colour-fast | No destroy |
| 8. peel strength | lbs/in | ≥5 | 7.8 |
From table 2, the p10 copper-clad plate combination property obtained by embodiment 2 is good.
Additionally, carrying out ocular estimate to obtained p10 copper-clad plate with prepreg, it is commercially for respect to existing
The prepreg preparing p10 copper-clad plate is whiter, and more smooth；After testing, carry out aging examination at 140-150 DEG C
Test, reduce under the transparency of this p10 copper-clad plate prepreg, therefore obtained p10 copper-clad plate making in actual use
With life-span length, and do not result in LED lamp light radiation output and weaken.
Embodiment 3
The composition of raw materials of p10 glue solution for copper-clad plate is as follows:
(softening point is for 300 parts of Bisphenol A Type liquid-state epoxy resin, 200 parts of Bisphenol A Type solid epoxy resin, phenolic resin
95-100 DEG C) 210 parts, 0.25 part of 2- phenylimidazole, 0.10 part of 2-methylimidazole, 140 parts of acetone, 120 parts of butanone, propylene glycol first
100 parts of ether, 400 parts of aluminium hydroxide, 130 parts of silicon powder, 70 parts of Pulvis Talci and 0.4 part of fluorescent whitening agent.
The preparation method of glue is as follows:
(1) acetone, butanone and propylene glycol monomethyl ether are stirred 0.15 hour under the rotating speed of 600rpm and obtain mixed solvent；Take
40% mixed solvent is mixed with solid epoxy resin, is stirred 7 hours with the rotating speed of 1800rpm, obtains mixture a；Take remaining mixed
Bonding solvent is mixed with phenolic resin, is stirred 7 hours with the rotating speed of 1800rpm, obtains mixture b；
Under the speed of agitator of 1800rpm, mixture a is mixed with liquid-state epoxy resin, stir 6-8 hour, then with
The speed of 2700rpm carries out shearing 7 hours；Mixed then at mixture b, 3-5 hour is stirred with the rotating speed of 1800rpm, obtains
To mixture c；
(2) under agitation, mixture c, 2- phenylimidazole, 2-methylimidazole and fluorescent whitening agent are mixed, then
Mix with aluminium hydroxide, silicon powder and Pulvis Talci, carry out shearing 1 hour with the speed of 2200rpm, with the rotating speed of 1200rpm
Stirring carries out ripening in 8 hours, obtains final product.
The preparation method of p10 copper-clad plate prepreg: institute is coated on electronic-grade glass fiber cloth 7628 with gluing machine
State p10 glue solution for copper-clad plate, after drying, obtain final product.The control parameter of p10 copper-clad plate prepreg is as follows:
Oven for gluing machine temperature: 215 DEG C；
Gluing speed: 18m/min；
Resin content: rc is up to 60%；
The gel time gt:65s of prepreg；
The fluidity rf:19% of prepreg；
The fugitive constituent vc:0.22% of prepreg；
Weight ppw:4.4g of prepreg.
The preparation method of p10 copper-clad plate (0.8mm plate) is as follows:
1. lamination: 3 7628 prepregs are carried out folding and joins, form lamination；Two sides overlying in two lateral surface of lamination
The Copper Foil of upper 18 μ m-thick, obtains semi-finished product；
2. semi-finished product are carried out hot pressing compacting, obtain final product；Hot pressing pressure: 35kg/cm2；Hot pressing press temperature: 170 DEG C；Hot pressing
Press time: 95min.
After testing, the performance parameter of obtained p10 copper-clad plate is as shown in table 3.
Table 3
From table 3, the p10 copper-clad plate combination property obtained by embodiment 3 is good.
Additionally, carrying out ocular estimate to obtained p10 copper-clad plate with prepreg, it is commercially for respect to existing
The prepreg preparing p10 copper-clad plate is whiter, and more smooth；After testing, carry out aging examination at 140-150 DEG C
Test, reduce under the transparency of this p10 copper-clad plate prepreg, therefore obtained p10 copper-clad plate making in actual use
With life-span length, and do not result in LED lamp light radiation output and weaken.
Claims (10)
1. a kind of p10 copper-clad plate is it is characterised in that it is obtained by following preparation methoies:
1. lamination: several prepregs are carried out folding and joins, form lamination；One or both sides overlying in two lateral surface of lamination
Upper Copper Foil, obtains semi-finished product；
2. described semi-finished product are carried out hot pressing compacting, obtain final product；
Wherein, described prepreg is obtained by following preparation methoies: coats p10 copper-clad plate glue on electronic-grade glass fiber cloth
Liquid, after drying, obtains final product；Described p10 glue solution for copper-clad plate is obtained by following raw materials, and described raw material includes the group of following weight parts
Point: 300-400 part liquid-state epoxy resin, 100-200 part solid epoxy resin, 175-235 part phenolic resin, 0.3-0.4 part are solid
Change accelerator, 280-360 part solvent, 100-600 part inorganic filler and 0.5-1.0 part fluorescent whitening agent.
2. p10 copper-clad plate as claimed in claim 1 is it is characterised in that described liquid-state epoxy resin is bisphenol type liquid epoxy
Resin；
And/or, described solid epoxy resin is bisphenol type solid epoxy resin；
And/or, the parts by weight of described liquid-state epoxy resin are 320-380 part；
And/or, the parts by weight of described solid epoxy resin are 120-180 part；
And/or, the softening point of described phenolic resin is 80-120 DEG C；
And/or, the parts by weight of described phenolic resin are 190-210 part；
And/or, described curing accelerator is imidazoles curing accelerator；
And/or, the parts by weight of described curing accelerator are 0.35-0.40 part；
And/or, described solvent is ketones solvent and/or ether solvent；
And/or, the parts by weight of described solvent are 360-370 part；
And/or, described inorganic filler is one of aluminium hydroxide, magnesium hydroxide, calcium oxide, silicon dioxide and Pulvis Talci or many
Kind；
And/or, the parts by weight of described inorganic filler are 100-300 part；
And/or, described fluorescent whitening agent is sunwhite line fluorescent brightening agent.
3. p10 copper-clad plate as claimed in claim 2 is it is characterised in that described liquid-state epoxy resin is Bisphenol A Type liquid epoxy
Resin；
And/or, described solid epoxy resin is Bisphenol A Type solid epoxy resin；
And/or, the softening point of described phenolic resin is 85-100 DEG C；
And/or, described curing accelerator is 2-methylimidazole and/or 2- phenylimidazole；
And/or, described solvent is one or more of acetone, butanone and propylene glycol monomethyl ether；
And/or, described inorganic filler is aluminium hydroxide, silicon dioxide and Pulvis Talci, described aluminium hydroxide, silicon dioxide and Talcum
The weight ratio of powder is (3-5): (6-8): (1-2)；
And/or, described fluorescent whitening agent is sunwhite fg-e fluorescent whitening agent.
4. the p10 copper-clad plate as described in any one of claim 1-3 is it is characterised in that the epoxy of described liquid-state epoxy resin is worked as
Measure as 195-200g/eq；
And/or, the epoxide equivalent of described solid epoxy resin is 980-1070g/eq；
And/or, described curing accelerator is 2-methylimidazole and 2- phenylimidazole, described 2-methylimidazole and 2- phenylimidazole
Weight ratio is (1-2): (4-5)；
And/or, described solvent is acetone, butanone and propylene glycol monomethyl ether, and the weight ratio of described acetone, butanone and propylene glycol monomethyl ether is
(2-4): (1-3): (1-2).
5. the p10 copper-clad plate as described in any one of claim 1-3 is it is characterised in that described p10 glue solution for copper-clad plate is by following
Preparation method is obtained:
(1) under agitation, mixture a is mixed with described liquid-state epoxy resin；Then with the speed of 2500-3000rpm
Carry out shearing 3-5 hour, then mixed with mixture b, obtain mixture c；
Described mixture a is mixed to get by the described solvent of described solid epoxy resin and 40%-60%；Described mixture b by
Described phenolic resin and remaining described solvent are mixed to get；
(2) under agitation, by described mixture c, described curing accelerator and described fluorescent whitening agent mix, then again with
Described inorganic filler mixing, is sheared with the speed of 2000-3000rpm, is obtained final product after ripening.
6. p10 copper-clad plate as claimed in claim 5 is it is characterised in that in the preparation of described mixture a, described is mixed into
6-8 hour is stirred with the rotating speed of 1500-2000rpm；
And/or, in the preparation of described mixture b, described being mixed into stirs 6-8 hour with the rotating speed of 1500-2000rpm；
And/or, in step (1), the rotating speed of described stirring is 1500-2000rpm；
And/or, in step (1), the time of described stirring is 3-5 hour；
And/or, in step (1), being mixed in " being mixed with mixture b " stirs 3-5 with the rotating speed of 1500-2000rpm
Hour；
And/or, in step (2), the time of described shearing is 0.5-1.5 hour；
And/or, in step (2), the speed of described shearing is 2000-2500rpm；
And/or, in step (2), described ripening is to stir 6-10 hour with the rotating speed of 1000-1500rpm.
7. p10 copper-clad plate as claimed in claim 1 is it is characterised in that described E-glass cloth is electronic-grade glass
Cloth 7628；
And/or, the equipment of described coating is gluing machine；
And/or, the speed of described coating is 17-25m/min；The temperature of described drying is 170-230 DEG C.
8. preparation method as claimed in claim 7 is it is characterised in that the speed of described coating is 18m/min；Described drying
Temperature is 200-220 DEG C.
9. p10 copper-clad plate as claimed in claim 1 is it is characterised in that the resin content of described p10 copper-clad plate prepreg
For 40-60%；The gel time of described p10 copper-clad plate prepreg is 65-85s；Described p10 copper-clad plate prepreg stream
Dynamic degree 18-25%；The fugitive constituent of described p10 copper-clad plate prepreg is below 0.25%.
10. p10 copper-clad plate as claimed in claim 1 it is characterised in that step 2. in, the pressure of described hot pressing compacting is 20-
40kg/cm2；
And/or, the temperature of described hot pressing compacting is 90-220 DEG C；
And/or, the time of described hot pressing compacting is 80-120min.
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107955331A (en) * | 2017-11-14 | 2018-04-24 | 浙江元集新材料科技股份有限公司 | A kind of preparation method of the special copper-clad plate of LED display |
| CN109535716A (en) * | 2018-10-18 | 2019-03-29 | 江苏澳盛复合材料科技有限公司 | A kind of and good polyphenylene sulfide/carbon fibre composite of metal adhesion |
| CN113524874A (en) * | 2021-07-19 | 2021-10-22 | 安徽鸿海新材料股份有限公司 | Preparation method of copper-clad plate with excellent shading property |
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| CN101798438A (en) * | 2009-02-06 | 2010-08-11 | 太阳油墨制造株式会社 | Heat curable resin composition, dry film and printed wiring board and method for preparing the same |
| CN102796478A (en) * | 2012-08-03 | 2012-11-28 | 金安国纪科技股份有限公司 | Copper foil clad laminated board with UV shielding function, adhesive and preparation methods thereof |
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| EP1197514A1 (en) * | 2000-10-13 | 2002-04-17 | Hitachi Chemical Co., Ltd. | Incombustible resin composition, prepreg, laminated plate, metal-clad laminated plate, printed wiring board and multi-layer printed wiring board |
| CN101798438A (en) * | 2009-02-06 | 2010-08-11 | 太阳油墨制造株式会社 | Heat curable resin composition, dry film and printed wiring board and method for preparing the same |
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| CN107955331A (en) * | 2017-11-14 | 2018-04-24 | 浙江元集新材料科技股份有限公司 | A kind of preparation method of the special copper-clad plate of LED display |
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| CN113524874A (en) * | 2021-07-19 | 2021-10-22 | 安徽鸿海新材料股份有限公司 | Preparation method of copper-clad plate with excellent shading property |
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