CN102310607B - Copper-clad plate with low-dielectric constant - Google Patents
Copper-clad plate with low-dielectric constant Download PDFInfo
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- CN102310607B CN102310607B CN 201110190895 CN201110190895A CN102310607B CN 102310607 B CN102310607 B CN 102310607B CN 201110190895 CN201110190895 CN 201110190895 CN 201110190895 A CN201110190895 A CN 201110190895A CN 102310607 B CN102310607 B CN 102310607B
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- 229920000647 polyepoxide Polymers 0.000 claims abstract description 37
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 16
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- 238000002360 preparation method Methods 0.000 claims abstract description 13
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 16
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- 239000010959 steel Substances 0.000 claims description 11
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- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910000077 silane Inorganic materials 0.000 claims description 10
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- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 5
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- HZEOUPCNUWSUFL-UHFFFAOYSA-N 4,5,5-trimethyl-4-pentan-3-yl-1H-imidazole Chemical class C(C)C(C1(N=CNC1(C)C)C)CC HZEOUPCNUWSUFL-UHFFFAOYSA-N 0.000 claims description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
The invention relates to a copper-clad plate with a low-dielectric constant. A preparation method of the copper-clad plate with a low-dielectric constant comprises the following steps of 1, mixing hollow glass microballoons, one or more solvents, a coupling agent, a surfactant, an epoxy resin, a curing agent and an accelerating agent by stirring to obtain a mixed solution, 2, dipping an electronic grade glass fiber fabric, roasting, and cooling to obtain prepregs, 3, carrying overlap of more than one of the prepregs, and coating two copper foil layers respectively on two surfaces of the overlapped prepregs to obtain a sheet material, 4, overlapping stainless steel plates on the two surface of the sheet material, feeding the sheet material with the stainless steel plates into an overlap-type compressor to carry out compacting, and carrying out thermal insulation, 5, disconnecting the compacted sheet material from the stainless steel plates, and 6, carrying out an edge cutting process on the sheet material separated from the stainless steel plates to obtain the copper-clad plate with a low-dielectric constant. The copper-clad plate with a low-dielectric constant has the advantages of low-dielectric constant, high strength, good smoothness, small thermal expansion coefficient, stable performances, high cost performance, stable thermal properties, high mechanical strength, low cost, and simple production process.
Description
Technical field
The present invention relates to a kind of dielectric materials, be specifically related to a kind of copper-clad plate of hollow glass micro-ball modification.
Background technology
The develop rapidly of semiconductor integrated circuit technology has promoted the continuous progress of new material, new technology, also makes the semi-conductor industry to grow into the very important strength of industrial quarters.Along with the continuous lifting of constantly the reducing of live width, transistor density, increasing people has invested the application of advanced low-k materials in super large-scale integration to sight.Work as Intel, IBM, AMD, Motorola, Infineon, when company such as TSMC and UMC announces to use advanced low-k materials in 0.13mm and following technology thereof in succession, to advanced low-k materials and the integrated research of technology thereof, just become the another important branch of semiconductor integrated circuit technique gradually.
In integrated circuit technology, the silica that fabulous heat endurance, moisture resistance are arranged is the main insulating materials that uses between the metal interconnection circuit always.Metallic aluminium then is the main material of circuit interconnects lead in the chip.Yet, along with the progress of integrated circuit technique, have high-speed, high device density, low-power consumption and cheaply chip more and more become the major product that super large-scale integration is made.At this moment, the wire density in the chip constantly increases, and conductor width and spacing constantly reduce, and the ghost effect that the resistance in interconnected and electric capacity produce is more and more obvious.
After device size is less than 0.25mm, overcome and disturb between signal propagation delays that capacitance-resistance sluggishness (RC Delay) causes, line and power dissipation etc., just become integrated circuit processing technique and develop unavoidable problem.The resistivity of metallic copper (~ 1.7mWcm) than the resistivity of metallic aluminium (～2.7mWcm) low about 40%.Thereby substitute the inevitable direction that traditional aluminum steel just becomes the integrated circuit technology development with copper cash.Nowadays, copper cash technology has developed into the key areas of integrated circuit technology.Meanwhile, advanced low-k materials substitutes the another inevitable choice that traditional insulating materials silica also just becomes the integrated circuit technology development.
Reduce dielectric constant and mainly contain following three kinds of approach: the one, utilize the low k characteristic of organic matter or inorganic matter itself, but its shortcoming is general organic matter non-refractory, not enough with the metal adhesive force, thereby limited their application in integrated circuit; The 2nd, mix impurity and reach the method that reduces material self polarity, adopt generally that the doped with fluorine element forms the silica that the FSG(fluorine mixes in silica) reduce the dielectric constant of material.Fluorine is to have strong electronegative element, after it is doped in the silica, can reduce electronics and ionic polarization in the material, thereby the dielectric constant of material is reduced to about 3.6 from 4.2.For further reducing the dielectric constant of material, people have introduced carbon in silica: namely the low polarity network that utilizes formation Si-C and C-C key to be unified into reduces the dielectric constant of material.The for example research of amorphous c film, the dielectric constant of its material can be reduced to below 3.0, but this kind method complex process, cost height, and this material do not have enough adhesions to metal line, so be difficult in practice be used; The 3rd, inject the method that the hole reduces density of material, the first adopts the method for chemical vapor deposition (CVD) to introduce methyl (CH3) in the process of growth silica, thereby form loose SiOC:H film, also claim the silica that CDO(carbon mixes), its dielectric constant is about 3.0.It two is to adopt spin-on process (spin-on) that organic polymer is used for integrated circuit technology as insulating materials.This method has been taken into account and has been formed low polarity network and high-voidage density two big characteristics, thereby its dielectric constant can drop to below 2.6.But fatal shortcoming is bad mechanical strength, and heat endurance also has much room for improvement.The low dielectric material of broad research mostly is to obtain by these three kinds of approach at present.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide a kind of prescription simple, directly hybrid process and have that dielectric constant is low, cost is low, the hollow glass micro-ball epoxy resin-matrix copper-clad plate that stable performance is good.
Another object of the present invention is to provide a kind of preparation method who prepares the epoxy resin copper-clad plate of above-mentioned hollow glass micro-ball modification.This method is applied to existing epoxy resin-matrix copper-clad plate field with hollow glass microballoon, and operating process is simple, industrialization feasibility height.
Above-mentioned purpose of the present invention is achieved by following technical solution:
A kind of low dielectric copper-clad plate is got by following method preparation:
1) hollow glass micro-ball, solvent, coupling agent, surfactant, epoxy resin, curing agent, promoter are got mixed liquor by weight 5～30:35～60:0.5～3.0:0.05～0.1:125:2.5～35.0:0.05～0.50 high-speed stirred mixing;
2) place mixed liquor to flood electronic-grade glass fiber cloth, under 150 ℃～230 ℃ temperature, toast then, obtain prepreg through cooling again;
3) the above prepreg of a slice is carried out stacked, and the prepreg two sides after stacked respectively is covered with one deck Copper Foil, and sheet material;
4) with the superimposed corrosion resistant plate of going up of stacked good sheet material two sides difference, send the superposed type press then to, suppress between 100 ℃-220 ℃, the compacting compressive load per unit area is 1Mpa-4Mpa; The compacting back is incubated at 180 ℃-220 ℃, and temperature retention time is at 40min-90min, and the holding stage compressive load per unit area is 2Mpa-4Mpa;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Glass microsphere is that a class density is little, dielectric constant low (1.2 ~ 2.0), moderate cost, the filling inorganic material that light weight has high dimension stability, shock resistance, hear resistance, resistance to abrasion and is easy to process.And its spherical structure, can avoid being enhanced the mixing inequality that material produces in process, blanking is built bridge and the problem excessive to the wearing and tearing of equipment.Epoxy resin composite material has that quality is light, intensity is high, modulus is big, good corrosion resistance, electrical property excellence, raw material sources are extensive, machine-shaping is easy, production efficiency is high, combination property is best, characteristics such as cost performance height, and have material designability and some other property, become the important materials that can't replace in national economy, national defense construction and the development in science and technology.Therefore, coming the epoxy resin-matrix copper-clad plate of modification with hollow glass micro-ball is to reduce one of feasible way of material dielectric constant, by exploitation hollow glass micro-ball epoxy resin-matrix copper-clad plate product, it is low to make the epoxy resin copper-clad plate have a dielectric constant, Heat stability is good, the mechanical strength height with advantages such as metal line, various film or components and parts adhesion are good, makes product be applied in high frequency, super large-scale integration field.
Preferably, in the step 1), with 5～30 parts by weight in hollow glass micro-ball, solvent, coupling agent, surfactant: 10～30 parts: 0.5～3.0 part: 0.05～0.1 part join that the high speed dispersor high speed stirs and solution; Form epoxy resin adhesive liquid by 125 parts of weight portion epoxy resin, 2.5～35.0 parts in curing agent, 0.05～0.50 part of promoter, 25.0～30.0 parts of mixed preparing of solvent; Epoxy resin adhesive liquid is joined in the hollow glass micro-ball solution of above-mentioned high-speed stirred and mix, be mixed with mixed liquor.The main purpose of in the step 1) epoxy resin adhesive liquid being added in the glass microsphere solution of high-speed stirred is the dispersion that is more conducive to glass microsphere, and fully dispersion can balling in resin to make glass microsphere.Stir in the middle of can certainly be directly adding glass microsphere and auxiliary material to epoxy resin adhesive liquid, the dispersion effect of Jiao Baning does not have the former good like this.
Preferably, described hollow glass micro-ball particle diameter is 300 ~ 1200 orders, and density is at 0.3 ~ 0.4g/cm3.If the glass microsphere particle diameter is too little, on the market stay in grade seldom and particle diameter little hollowness also little density is just big generally; If particle diameter is too big then occur hydro-planing easily, be difficult to form mixed liquor relatively uniformly.
How many direct dielectric properties of the final sheet material of influence that described hollow glass micro-ball adds umber, weight and intensity, add umber too much then the intensity severe dielectric properties that descend change not quite.
Preferably, described coupling agent is silane coupler.The compatibility of glass microsphere and solution and glass cloth can be better behind the interpolation coupling agent, can promote certain adhesion.
Preferably, described surfactant is fluorocarbon surfactant.Fluorocarbon chain molecule in the fluorocarbon surfactant can greatly reduce the surface tension of water, has certain water and oil-resistant and can improve stain resistance simultaneously.Add the abundant wetting glass microsphere in back and be beneficial to its dispersion in resin, improved the adhesive force of glass microsphere to a certain extent.
Preferably, described solvent is one or more in acetone or butanone or the dimethyl formamide.
Preferably, the stir speed (S.S.) of described high-speed stirred is 800 ~ 1500 commentaries on classics/min.Stir speed (S.S.) is too fast, and the poor quality glass microsphere is broken easily, and is too slow and that mixed liquor is mixed is irregular, so this speed interval is proper.
Among the present invention, the common model of electronic-grade glass fiber cloth has standard cloth or imitative cloth such as 1080,2116,7628,1506.Imitative cloth is as imitative 7628 cloth, imitative 2116 cloth etc.
Preferably, described epoxy resin is bisphenol A type epoxy resin or bisphenol f type epoxy resin or brominated epoxy resin or phosphorous epoxy resin, described curing agent is selected from one or more in dicyandiamide, phenolic aldehyde, DADPS, the diamino-diphenylamine, and described promoter is methylimidazole or diethyl tetramethyl imidazoles.
Again preferably, described curing agent is resting form electron level dicy-curing agent.Adopting dicyandiamide mainly is that the resin solidification action pane is wide with the existing manufacturing technique comparison match, and process controllability is strong.
The glue gel time of the prepreg that makes preferably, described step 2) is 200-300 second, and flowability is 15%-23%, and resin content is 36%-54%.Gel time described above, fluidity, resin content all are the TM650 method of testing tests according to industry standard IPC4101B correspondence.Above-mentioned technological parameter is the key that guarantees the sheet material quality, has higher yields.
The present invention has adopted epoxy resin, curing agent, promoter, solvent, hollow glass micro-ball and auxiliary material mixed preparing to form glue, after reinforcing material places the oven dry of glue dipping to handle, the low dielectric copper-clad plate that suppresses, dielectric constant is low, the intensity height, little, the stable performance of thermal coefficient of expansion.
The low dielectric copper-clad plate technological process that the present invention obtains is simple, the production efficiency height, and equipment drops into little, and the place takies few, has good chemical proofing; Dielectric constant is low simultaneously, intensity is high, planarization good, thermal coefficient of expansion is little, stable performance, and the cost performance height replaces traditional low dielectric copper-clad plate, and hot property is stablized, reduced cost when mechanical strength is high, has simplified technology.
Description of drawings
Fig. 1 is technological process of production figure of the present invention.
The specific embodiment
The present invention is further detailed explanation below in conjunction with specific embodiment, but be not limiting the scope of the invention.
Each raw material that manufacture method of the present invention relates to all can obtain by commercial sources.
Embodiment 1:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
1.1) be that 900 purpose hollow glass micro-balls, 10kg dimethyl formamide, 0.5kg silane coupler, 0.05kg fluorocarbon surfactant join the high speed dispersor high speed and stir with the 5kg particle diameter;
1.2) bisphenol A type epoxy resin 125kg, electron level dicyandiamide 3.1kg, methylimidazole 0.1kg, dimethyl formamide 28kg are deployed into gel time is 210～215 seconds glue;
1.3) with step 1.2) and in glue join step 1.1) the hollow glass micro-ball solution high speed that stirs of high speed mixes, and is configured to mixed liquor;
2) putting into temperature after 2116 cloth are flooded through squeeze into the mixed liquor in the glue basin with pump in is that 150 ℃～230 ℃ baking ovens toast, obtaining resin flow through cooling again is 22%～23%, content is 48.4%～49.4% 2116 cloth prepregs, and 2116 cloth prepregs are cut into needed size;
3) 8 prepregs are carried out stacked, and one deck Copper Foil is respectively covered on the prepreg two sides after stacked and sheet material;
4) send the superposed type press to behind each the superimposed last corrosion resistant plate of two sides with sheet material, between 100 ℃～220 ℃, suppress, compacting compressive load per unit area position 1～4Mpa, the holding temperature scope of compacting is 180 ℃～185 ℃, temperature retention time 70 minutes, holding stage compacting compressive load per unit area is 4Mpa, fully flows even in this stage resin;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Embodiment 2:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
1.1) be that 300 purpose hollow glass micro-balls, 22kg dimethyl formamide, 0.6kg silane coupler, 0.05kg fluorocarbon surfactant join the high speed dispersor high speed and stir with the 10kg particle diameter;
1.2) bisphenol A type epoxy resin 125kg, electron level dicyandiamide 2.8kg, methylimidazole 0.055kg, dimethyl formamide 28kg are deployed into gel time is 245～250 seconds glue;
1.3) with step 1.2) and in glue join step 1.1) the hollow glass micro-ball solution high speed that stirs of high speed mixes, and is configured to mixed liquor;
2) putting into temperature after 1506 cloth are flooded through squeeze into the mixed liquor in the glue basin with pump in is that 150 ℃～230 ℃ baking ovens toast, obtaining resin flow through cooling again is 18%～19%, content is 42.3%～42.7% 1506 cloth prepregs, and 1506 cloth prepregs are cut into needed size;
3) 6 prepregs are carried out stacked, and one deck Copper Foil is respectively covered on the prepreg two sides after stacked and sheet material;
4) send the superposed type press to behind each the superimposed last corrosion resistant plate of two sides with sheet material, between 100 ℃～220 ℃, suppress, compacting compressive load per unit area position 1～4Mpa, the holding temperature scope of compacting is 185 ℃～190 ℃, temperature retention time 65 minutes, holding stage compacting compressive load per unit area is 3Mpa, fully flows even in this stage resin;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Embodiment 3:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
1.1) be that 1200 purpose hollow glass micro-balls, 20kg dimethyl formamide, 1kg silane coupler, 0.07kg fluorocarbon surfactant join the high speed dispersor high speed and stir with the 15kg particle diameter;
1.2) bisphenol A type epoxy resin 125kg, electron level dicyandiamide 2.5kg, methylimidazole 0.050kg, dimethyl formamide 26kg are deployed into gel time is 260～270 seconds glue;
1.3) with step 1.2) and in glue join step 1.1) the hollow glass micro-ball solution high speed that stirs of high speed mixes, and is configured to mixed liquor;
2) putting into temperature after 2116 cloth are flooded through squeeze into the mixed liquor in the glue basin with pump in is that 150 ℃～230 ℃ baking ovens toast, obtaining resin flow through cooling again is 20%～21%, content is 46.5%～47.3% 2116 cloth prepregs, and 2116 cloth prepregs are cut into needed size;
3) 7 prepregs are carried out stacked, and one deck Copper Foil is respectively covered on the prepreg two sides after stacked and sheet material;
4) send the superposed type press to behind each the superimposed last corrosion resistant plate of two sides with sheet material, between 100 ℃～220 ℃, suppress, compacting compressive load per unit area position 1～4Mpa, the holding temperature scope of compacting is 185-190 ℃, temperature retention time 70 minutes, holding stage compacting compressive load per unit area is 2.5Mpa, fully flows even in this stage resin;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Embodiment 4:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
1.1) be that 600 purpose hollow glass micro-balls, 20kg dimethyl formamide, 1.1kg silane coupler, 0.07kg fluorocarbon surfactant join the high speed dispersor high speed and stir with the 20kg particle diameter;
1.2) bisphenol A type epoxy resin 125kg, electron level dicyandiamide 2.8kg, methylimidazole 0.050kg, dimethyl formamide 29kg are deployed into gel time is 290～300 seconds glue;
1.3) with step 1.2) and in glue join step 1.1) the hollow glass micro-ball solution high speed that stirs of high speed mixes, and is configured to mixed liquor;
2) putting into temperature after 1506 cloth are flooded through squeeze into the mixed liquor in the glue basin with pump in is that 150 ℃～230 ℃ baking ovens toast, obtaining resin flow through cooling again is 18%～19%, content is 38.2%～38.9% 1506 cloth prepregs, and 1506 cloth prepregs are cut into needed size;
3) 5 prepregs are carried out stacked, and one deck Copper Foil is respectively covered on the prepreg two sides after stacked and sheet material;
4) send the superposed type press to behind each the superimposed last corrosion resistant plate of two sides with sheet material, between 100 ℃～220 ℃, suppress, compacting compressive load per unit area position 1～4Mpa, the holding temperature scope of compacting is 180 ℃～185 ℃, temperature retention time 75 minutes, holding stage compacting compressive load per unit area is 3.0Mpa, fully flows even in this stage resin;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Embodiment 5:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
1.1) be that 900 purpose hollow glass micro-balls, 20kg dimethyl formamide and 5kg acetone, 2kg silane coupler, 0.09kg fluorocarbon surfactant join the high speed dispersor high speed and stir with the 25kg particle diameter;
1.2) with bisphenol f type epoxy resin 125kg, DADPS 35kg, methylimidazole 0.5kg, dimethyl formamide 20kg and acetone 10 kg, be deployed into gel time and be 280～390 seconds glue;
1.3) with step 1.2) and in glue join step 1.1) the hollow glass micro-ball solution high speed that stirs of high speed mixes, and is configured to mixed liquor;
2) putting into temperature after 2116 cloth are flooded through squeeze into the mixed liquor in the glue basin with pump in is that 150 ℃～230 ℃ baking ovens toast, obtaining resin flow through cooling again is 17%～18%, content is 45.1%～45.7% 2116 cloth prepregs, and 2116 cloth prepregs are cut into needed size;
3) 9 prepregs are carried out stacked, and one deck Copper Foil is respectively covered on the prepreg two sides after stacked and sheet material;
4) send the superposed type press to behind each the superimposed last corrosion resistant plate of two sides with sheet material, between 100 ℃～220 ℃, suppress, compacting compressive load per unit area position 1～4Mpa, the holding temperature scope of compacting is 215 ℃～220 ℃, temperature retention time 90 minutes, holding stage compacting compressive load per unit area is 2.5Mpa, fully flows even in this stage resin;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Embodiment 6:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
1.1) be that 700 purpose hollow glass micro-balls, 8kg butanone, 20kg dimethyl formamide and 2kg acetone, 3kg silane coupler, 0.1kg fluorocarbon surfactant join the high speed dispersor high speed and stir with the 30kg particle diameter;
1.2) with bisphenol f type epoxy resin 125kg, DADPS 22kg, diamino-diphenylamine 6kg, methylimidazole 0.2kg, dimethyl formamide 25kg and acetone 5 kg, be deployed into gel time and be 260～270 seconds glue;
1.3) with step 1.2) and in glue join step 1.1) the hollow glass micro-ball solution high speed that stirs of high speed mixes, and is configured to mixed liquor;
2) putting into temperature after 2116 cloth are flooded through squeeze into the mixed liquor in the glue basin with pump in is that 150 ℃～230 ℃ baking ovens toast, obtaining resin flow through cooling again is 22%～23%, content is 48.1%～48.7% 2116 cloth prepregs, and 2116 cloth prepregs are cut into needed size;
3) 5 prepregs are carried out stacked, and one deck Copper Foil is respectively covered on the prepreg two sides after stacked and sheet material;
4) send the superposed type press to behind each the superimposed last corrosion resistant plate of two sides with sheet material, between 100 ℃～220 ℃, suppress, compacting compressive load per unit area position 1～4Mpa, the holding temperature scope of compacting is 200 ℃～205 ℃, temperature retention time 80 minutes, holding stage compacting compressive load per unit area is 2Mpa, fully flows even in this stage resin;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Embodiment 7:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
1.1) be that 800 purpose hollow glass micro-balls, 8kg butanone, 15kg dimethyl formamide and 7kg acetone, 1kg silane coupler, 0.08kg fluorocarbon surfactant join the high speed dispersor high speed and stir with the 30kg particle diameter;
1.2) with brominated epoxy resin 125kg, DADPS 10kg, dicyandiamide 1.5kg, methylimidazole 0.2kg, dimethyl formamide 20kg and acetone 8 kg, be deployed into gel time and be 200～210 seconds glue;
1.3) with step 1.2) and in glue join step 1.1) the hollow glass micro-ball solution high speed that stirs of high speed mixes, and is configured to mixed liquor;
2) putting into temperature after 7628 cloth are flooded through squeeze into the mixed liquor in the glue basin with pump in is that 150 ℃～230 ℃ baking ovens toast, obtaining resin flow through cooling again is 15%～16%, content is 36%～37% 7628 cloth prepregs, and 7628 cloth prepregs are cut into needed size;
3) 4 prepregs are carried out stacked, and one deck Copper Foil is respectively covered on the prepreg two sides after stacked and sheet material;
4) send the superposed type press to behind each the superimposed last corrosion resistant plate of two sides with sheet material, between 100 ℃～220 ℃, suppress, compacting compressive load per unit area position 1～4Mpa, the holding temperature scope of compacting is 215 ℃～220 ℃, temperature retention time 45 minutes, holding stage compacting compressive load per unit area is 2.5Mpa, fully flows even in this stage resin;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Embodiment 8:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
1.1) be that 800 purpose hollow glass micro-balls, 23kg butanone, 7kg acetone, 2kg silane coupler, 0.09kg fluorocarbon surfactant join the high speed dispersor high speed and stir with the 30kg particle diameter;
1.2) with phosphorous epoxy resin 125kg, linear phenolic curing agent 34kg, methylimidazole 0.15kg, diethyl tetramethyl imidazoles 0.2kg, butanone 20kg and acetone 10 kg, be deployed into gel time and be 290～295 seconds glue;
1.3) with step 1.2) and in glue join step 1.1) the hollow glass micro-ball solution high speed that stirs of high speed mixes, and is configured to mixed liquor;
2) putting into temperature after 1080 cloth are flooded through squeeze into the mixed liquor in the glue basin with pump in is that 150 ℃～230 ℃ baking ovens toast, obtaining resin flow through cooling again is 20%～21%, content is 53%～54% 1080 cloth prepregs, and 1080 cloth prepregs are cut into needed size;
3) 10 prepregs are carried out stacked, and one deck Copper Foil is respectively covered on the prepreg two sides after stacked and sheet material;
4) send the superposed type press to behind each the superimposed last corrosion resistant plate of two sides with sheet material, between 100 ℃～220 ℃, suppress, compacting compressive load per unit area position 1～4Mpa, the holding temperature scope of compacting is 195 ℃～200 ℃, temperature retention time 80 minutes, holding stage compacting compressive load per unit area is 3Mpa, fully flows even in this stage resin;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
Embodiment 9:
With reference to Fig. 1, a kind of low dielectric copper-clad plate, adopt following method preparation:
Basic identical with product and implementation column 1 step that the imitative cloth 2116 of electronic-grade glass is made, timber intensity is more lower slightly than mark cloth, permittivity ratio mark Bu Lvegao, and warpage is than mark cloth product height, and other performances are similar substantially to standard cloth product.
The test example
Dielectric constant is carried out in low dielectric copper-clad plate and ordinary epoxy resin copper-clad plate that embodiment 1-9 prepares, flexural strength, dimensional stability, its result is as shown in table 1 for peel strength and thermal performance test.
Table 1 hangs down dielectric copper-clad plate performance (copper-clad plate of contrast ordinary epoxy resin)
| Embodiment | Dielectric constant 1GHz | Bending strength MPa | 288 ℃ of not stratified foamings of thermal stress S() | Dimensional stability PPM | Peel strength N/mm(1oz Copper Foil) |
| 1 | 4.55 | 470 | 190 | 23 | 1.60 |
| 2 | 4.23 | 450 | 180 | 22 | 1.59 |
| 3 | 3.56 | 430 | 200 | 18 | 1.65 |
| 4 | 3.27 | 410 | 170 | 19 | 1.61 |
| 5 | 2.89 | 380 | 185 | 20 | 1.67 |
| 6 | 2.73 | 350 | 175 | 16 | 1.70 |
| 7 | 2.92 | 360 | 195 | 19 | 1.62 |
| 8 | 2.67 | 340 | 165 | 17 | 1.68 |
| 9 | 4.70 | 460 | 160 | 24 | 1.58 |
| Common epoxy copper-clad plate | 5.05 | 500 | 120 | 25 | 1.57 |
The dimensional stability here is change value of thickness and the ratio that heats preceding thickness after the product by heating.
The common epoxy copper-clad plate here is not for containing the conventional glass fiber reinforced epoxy resin copper-clad plate (8 layers of prepreg add the Copper Foil lamination) of glass microsphere.
Above-mentioned dielectric constant, bending strength, thermal stress, the peel strength performance test is all tested according to the TM650 method of testing of IPC4101B correspondence.
The dielectric constant of the low dielectric copper-clad plate of several embodiment is all low than common epoxy composite copper-clad plate as can be seen from Table 1, and wherein embodiment 8 minimums reach 2.67.Although the bending strength value of each embodiment is all little than common epoxy copper-clad plate, but all satisfy the requirement of industry standard IPC4101B, and heat endurance, peel strength and dimensional stability are all slightly excellent than epoxy resin copper-clad plate performance, also satisfy the performance of conventional copper-clad plate when having reached low dielectric.Cost is slightly little by little higher than common copper-clad plate, is more or less the same, but many (price are generally several times of common copper-clad plate) lower than the existing dielectric materials of industry.
The low dielectric copper-clad plate of said method production also has following advantage:
1. stable performance and have good chemical proofing;
2. machine-shaping is easy, guarantees that material has reduced the density of material when hanging down dielectric, realize the lightweight of product;
3. material caking property is good, the intensity height;
4. technology is simple, operation and serialization production easily, and the production efficiency height, calculating a vertical superposed type press in one day 24 hours can 5000 low dielectric copper-clad plate of volume production;
5. equipment less investment, place take few;
6. thermal coefficient of expansion is little, working stability under the middle temperature;
7. high performance-price ratio makes product be with a wide range of applications in high-frequency electronic material field;
Claims (10)
1. one kind low dielectric copper-clad plate is characterized in that being got by following method preparation:
1) with hollow glass micro-ball, solvent, coupling agent, surfactant, epoxy resin, curing agent, promoter by weight (5～30): (35～60): (0.5～3.0): (0.05～0.1): 125:(2.5～35.0): (0.05～0.50) high-speed stirred mix and mixed liquor;
2) place mixed liquor to flood electronic-grade glass fiber cloth, under 150 ℃～230 ℃ temperature, toast then, obtain prepreg through cooling again;
3) the above prepreg of a slice is carried out stacked, and the prepreg two sides after stacked respectively is covered with one deck Copper Foil, and sheet material;
4) with the superimposed corrosion resistant plate of going up of stacked good sheet material two sides difference, send the superposed type press then to, suppress between 100 ℃-220 ℃, the compacting compressive load per unit area is 1Mpa-4Mpa; The compacting back is incubated at 180 ℃-220 ℃, and temperature retention time is at 40min-90min, and the holding stage compressive load per unit area is 2Mpa-4Mpa;
5) sheet material and the corrosion resistant plate that suppress are disassembled out;
6) the sheet material cutting edge that will separate with steel plate and must hang down the dielectric copper-clad plate.
2. low dielectric copper-clad plate according to claim 1, it is characterized in that: in the step 1), with 5～30 parts by weight in hollow glass micro-ball, solvent, coupling agent, surfactant: 10～30 parts: 0.5～3.0 part: 0.05～0.1 part join that the high speed dispersor high speed stirs and solution; Form epoxy resin adhesive liquid by 125 parts of weight portion epoxy resin, 2.5～35.0 parts in curing agent, 0.05～0.50 part of promoter, 25.0～30.0 parts of mixed preparing of solvent; Epoxy resin adhesive liquid is joined in the hollow glass micro-ball solution of above-mentioned high-speed stirred and mix, be mixed with mixed liquor.
3. low dielectric copper-clad plate according to claim 1, it is characterized in that: described hollow glass micro-ball particle diameter is 300～1200 orders, and density is at 0.3～0.4g/cm
3
4. low dielectric copper-clad plate according to claim 1, it is characterized in that: described coupling agent is silane coupler.
5. low dielectric copper-clad plate according to claim 1, it is characterized in that: described surfactant is fluorocarbon surfactant.
6. low dielectric copper-clad plate according to claim 1 is characterized in that: described solvent is one or more in acetone or butanone or the dimethyl formamide.
7. low dielectric copper-clad plate according to claim 1, it is characterized in that: the stir speed (S.S.) of described high-speed stirred is 800～1500 commentaries on classics/min.
8. low dielectric copper-clad plate according to claim 1 is characterized in that: described epoxy resin is bisphenol A type epoxy resin or bisphenol f type epoxy resin or brominated epoxy resin or phosphorous epoxy resin; Described curing agent is selected from one or more in dicyandiamide, phenolic aldehyde, DADPS, the diamino-diphenylamine; Described promoter is methylimidazole or diethyl tetramethyl imidazoles.
9. low dielectric copper-clad plate according to claim 8 is characterized in that: described curing agent is resting form electron level dicy-curing agent.
10. low dielectric copper-clad plate according to claim 1 is characterized in that: the glue gel time of the prepreg that makes described step 2) is 200-300 second, and flowability is 15%-23%, and resin content is 36%-54%.
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| CN103160229B (en) * | 2013-01-28 | 2014-12-17 | 金安国纪科技股份有限公司 | Glue liquor for environment-friendly light laminated board, laminated board and preparation method of glue liquor |
| CN103287032B (en) * | 2013-06-08 | 2016-05-18 | 浙江华正新材料股份有限公司 | The application of laminated material and preparation method thereof and hollow glass micro-ball |
| CN104947358A (en) * | 2015-03-27 | 2015-09-30 | 安徽丹凤电子材料股份有限公司 | Electronic fabric surface treatment technology |
| CN105150662A (en) * | 2015-08-06 | 2015-12-16 | 忠信(太仓)绝缘材料有限公司 | Manufacturing method of epoxy glass-cloth-matrix copper clad laminate |
| CN105128497A (en) * | 2015-08-06 | 2015-12-09 | 忠信(太仓)绝缘材料有限公司 | CEM-3 type copper-clad laminated plate base paper manufacturing method |
| CN105273362B (en) * | 2015-11-12 | 2017-08-29 | 广东生益科技股份有限公司 | A kind of composition epoxy resin and its application |
| CN106589820B (en) * | 2016-12-13 | 2019-01-08 | 桂林电子科技大学 | A kind of multiphase composite material with high dielectric constant and preparation method thereof with isolation structure |
| CN109852002B (en) * | 2019-01-02 | 2021-06-08 | 浙江华正新材料股份有限公司 | Preparation method of light high-strength laminated composite board |
| CN114670512B (en) * | 2022-04-27 | 2023-06-23 | 中山新高电子材料股份有限公司 | Polytetrafluoroethylene flexible copper-clad plate containing glass fibre cloth and its preparation method |
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| CN101220160A (en) * | 2007-12-07 | 2008-07-16 | 广东生益科技股份有限公司 | A kind of prepreg applied to printed circuit multilayer board |
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Denomination of invention: A low dielectric copper clad plate Effective date of registration: 20231128 Granted publication date: 20130814 Pledgee: Agricultural Bank of China Limited Hangzhou Yuhang Branch Pledgor: ZHEJIANG HUAZHENG NEW MATERIAL GROUP Co.,Ltd. Registration number: Y2023980067733 |