CN103360621A - Packing in metal-clad foil plate with low thermal expansion coefficient and preparation method of packing - Google Patents
Packing in metal-clad foil plate with low thermal expansion coefficient and preparation method of packing Download PDFInfo
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- CN103360621A CN103360621A CN2013102757079A CN201310275707A CN103360621A CN 103360621 A CN103360621 A CN 103360621A CN 2013102757079 A CN2013102757079 A CN 2013102757079A CN 201310275707 A CN201310275707 A CN 201310275707A CN 103360621 A CN103360621 A CN 103360621A
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Abstract
The invention relates to composite silica amorphous eutectic powder packing in a metal-clad foil plate. The packing comprises the following components in percentage by weight: 57-70 percent of silica, 15-35 percent of aluminum oxide, less than or equal to 40 percent of magnesium oxide and calcium oxide, and less than or equal to 2 percent of sodium oxide and lithium oxide. According to the provided packing, the processability of an electronic substrate is improved, and the prepared metal-clad foil plate has a low thermal expansion coefficient.
Description
Technical field
The present invention relates to filler in a kind of clad with metal foil plate and preparation method thereof, relate in particular to amorphous eutectic powder stuffing of composite silicon dioxide in a kind of clad with metal foil plate and preparation method thereof.
Background technology
When using filler in the clad with metal foil plate (for example CEM-3), adopt aluminium hydroxide and magnesium hydroxide more in the past.But more than 200 degree centigrade in aluminium hydroxide just begins to decompose, thermo-labile impact, and 230 ℃, 300 ℃, 530 ℃ of three phases discharge crystal water, cause easily plate material lamination to bubble, so, heat-treat; And the magnesium hydroxide price is partially expensive.
Silicon-dioxide (SiO
2) then have excellent physical property, as have high-insulativity, high thermal conductivity, high thermal stability, resistance to acids and bases, wear resistance, low thermal expansivity, low-k etc., and lower price advantage, value of exploiting and utilizing is arranged very much.Improvement along with silicon-dioxide self surface treatment condition, improved the consistency of it and resin system, so the filler silicon powder of making as major ingredient with silicon-dioxide is applied in the clad with metal foil plate, not only can reduce cost, can also improve some performance (such as thermal expansivity, flexural strength, dimensional stability etc.) of clad with metal foil plate, so promise well.
Silicon powder is by natural quartz (SiO
2) or fused quartz (natural quartz is through high-temperature fusion, cooled amorphous Si O
2) micro mist that forms through multiple tracks processes such as broken, ball milling (or vibration, airflow milling), flotation, pickling purification, high purity water processing.
Electron trade is unleaded to have promoted the application of silicon powder filler at the clad with metal foil plate.In the past lead solder Sn-Pb(37%Pb arranged) lead welding material lowest total of the melting point be 183 ℃, the lowest total of the melting point of at present representative unleaded and enforceable scolder Sn-Ag-Cu system etc. is 217 ℃.The lifting of welding temperature has proposed higher thermotolerance and reliability requirement to various components and parts, printed circuit board (pcb) base material etc.The PCB leadless process requires sheet material to have low thermal expansivity (CTE), and for the clad with metal foil plate, improving stable on heating main approach is the CTE that reduces sheet material.To reduce at present most economical, the effective means of CTE and add filler.Reducing the most general method of sheet material CTE at present is to introduce inorganic powder material in the clad with metal foil plate.The thermal expansivity of Resins, epoxy is (30-50) ppm/ ℃, and the thermal expansivity of silicon-dioxide is (0.5-9) ppm/ ℃.In Resins, epoxy, add a large amount of silicon powders, so just can reduce the thermal expansivity of sheet material, reduce simultaneously water-intake rate, internal stress, shrinking percentage, thereby make the requirement of clad with metal foil plate adapted to leadless welding.
Silicon-dioxide is because its excellent chemical stability, low thermal expansivity are to use at present maximum fillers in the clad with metal foil board industry.But it is high that the shortcoming of silicon-dioxide is hardness, and Mohs' hardness is 7, and is large to equipment attrition.Especially affecting large is the obvious raising of the tooling cost of downstream PCB producer, such as boring, the raising of milling plate cost and press tool cost.In order to improve the processibility of powder, change the powder composition and become one of method of consideration.
Silicon is released than section and is improved the G2-C product of processibility, and has applied for the invention CN102088820A that this powder is used at copper clad laminate.The filler of this disclosure of the Invention is by silicon-dioxide 50-62wt%, and aluminium sesquioxide 11-19wt%, boron trioxide 4-13wt%, calcium oxide 6-27wt%, magnesium oxide<6wt%, strontium oxide<1.5wt% and barium oxide<0.1wt% are total to the amorphism reticulated structure that consists of.Although the filler that wherein adds has lower hardness, thermal expansivity is larger.
Summary of the invention
The object of the invention is to for behind the present use silicon powder filler making clad with metal foil plate, the problem that thermal expansivity is larger provides a kind of composite silicon dioxide amorphous eutectic powder stuffing.Filler composite silicon dioxide eutectic powder provided by the invention not only improve the processibility of electric substrate, make simultaneously the clad with metal foil plate that makes have lower thermal expansivity.
In order to achieve the above object, the present invention has adopted following technical scheme:
The amorphous eutectic powder stuffing of composite silicon dioxide in a kind of clad with metal foil plate, contain by weight percentage following component: silicon-dioxide 57~70wt%, for example be 58wt%, 61wt%, 64wt%, 68wt%, 69wt% etc., aluminium sesquioxide 15~35wt%, for example be 16wt%, 19wt%, 22wt%, 26wt%, 29wt%, 32wt%, 34wt% etc., magnesium oxide+calcium oxide≤40wt%, for example be 6wt%, 8wt%, 10wt%, 14wt%, 16wt%, 18wt%, 22wt%, 26wt%, 29wt%, 32wt%, 34wt% etc., sodium oxide+potassium oxide+Lithium Oxide 98min≤2wt% for example is 0.1wt%, 0.5wt%, 0.8wt%, 1.1wt%, 1.3wt%, 1.6wt%, 1.8wt%, 1.95wt% etc.
As optimal technical scheme, filler of the present invention contains following component: silicon-dioxide 60~66wt%, aluminium sesquioxide 23~28wt%, magnesium oxide+calcium oxide≤30wt%, sodium oxide+potassium oxide+Lithium Oxide 98min≤1wt% by weight percentage.
Silicon-dioxide forms the skeleton structure of eutectic, if its content less than 57wt%, the thermal expansivity of eutectic powder is high.If its content is higher than 70wt%, then filler hardness enlarges markedly, and affects the processibility of PCB.Therefore, it is 57~70wt% that the present invention selects dioxide-containing silica, is preferably 60~66wt%.
If the aluminium sesquioxide content in the eutectic powder is less than 15wt%, the water tolerance of eutectic powder is not good, if be higher than 35wt%, then the thermal expansivity of fusant powder is high.Therefore, it is 15~35wt% that the present invention selects aluminium sesquioxide content, is preferably 23~28wt%.
Contain under calcium oxide, the magnesian filler moisture conditions and separate out easily calcium ion, magnesium ion, affect CAF performance (anti-ion migration performance), thus the insulativity of the sheet material of impact preparation.Therefore, its content sum is defined as≤40wt%, is preferably≤30wt%.Calcium oxide can also have fluxing action in the preparation process of filler of the present invention on the other hand.
Sodium oxide+potassium oxide in the eutectic powder+Lithium Oxide 98min water soluble, the precipitating metal ion, the insulating property of the copper-clad plate of impact preparation, if its content is higher than 2wt%, then the copper-clad plate insulating property of the preparation of fusant powder worsen.Therefore, the present invention is defined as its content≤2wt%, is preferably≤1wt%.
As optimal technical scheme, filler of the present invention, contain by weight percentage ferric oxide≤0.6wt%, such as be 0.05wt%, 0.11wt%, 0.15wt%, 0.18wt%, 0.22wt%, 0.25wt%, 0.28wt%, 0.33wt%, 0.36wt%, 0.39wt%,, 0.44wt%, 0.51wt%, 0.58wt% etc., be preferably≤0.2wt%, more preferably≤0.1wt%.But ferric oxide is conducting material, and it is limited in the specific content range, can solve powder that prior art provides after making substrate, the problem of insulating property deficiency.
Stain is the black impurity in the composite silicon dioxide eutectic powder, and by analysis, but the stain major part is the black conducting material, and therefore, stain not only can affect the apparent of base material, and more affects the insulativity of base material.Therefore, the present invention with the stain number of the amorphous eutectic powder of described composite silicon dioxide less than 20/300g, such as being 3/300g, 5/300g, 8/300g, 11/300g, 14/300g, 16/300g, 18/300g etc., preferably less than 15/300g, further preferably less than 10/300g.
As optimal technical scheme, the specific conductivity of filler of the present invention≤200 μ s/cm, such as being 5 μ s/cm, 10 μ s/cm, 15 μ s/cm, 20 μ s/cm, 26 μ s/cm, 34 μ s/cm, 39 μ s/cm, 45 μ s/cm, 55 μ s/cm, 60 μ s/cm, 68 μ s/cm, 76 μ s/cm, 88 μ s/cm, 105 μ s/cm, 124 μ s/cm, 136 μ s/cm, 145 μ s/cm, 157 μ s/cm, 165 μ s/cm, 174 μ s/cm, 186 μ s/cm, 198 μ s/cm etc., be preferably≤100 μ s/cm.Specific conductivity is the conductivity of powder, and the insulating property of the higher sheet material of specific conductivity are poorer, in order to guarantee the insulating property of sheet material, the specific conductivity of filler is defined as≤200 μ s/cm.
As optimal technical scheme, filler of the present invention is through surface treatment.Because the powder stuffing described in the present invention is inorganic materials, and is bad with organic resin matrix consistency, therefore, need to do surface treatment to it with surface treatment agent, to increase the consistency of itself and matrix.
Preferably, the surface treatment agent that described surface treatment is used is the one kind or two or more mixture in silane coupling agent, titanate ester treatment agent, aluminate, zirconate, cationic surfactant, aniorfic surfactant, amphoterics, neutral surface active agent, stearic acid, oleic acid, lauric acid and their metallic salt, resol, organic silicone oil, hexamethyldisilazane, the polyoxyethylene glycol, is preferably the one kind or two or more mixture in silane coupling agent, titanate ester treatment agent, organic silicone oil, the hexamethyldisilazane.
As optimal technical scheme, the median size of filler of the present invention is 1-20 μ m, such as being 2 μ m, 4 μ m, 6 μ m, 7 μ m, 9 μ m, 12 μ m, 15 μ m, 17 μ m, 19 μ m etc., maximum particle diameter≤35 μ m; Being preferably median size is 1-6 μ m, maximum particle diameter≤25 μ m.
One of purpose of the present invention also is to provide the preparation method of described filler, comprises the steps:
The mineral that (a) will comprise quartz sand, kaolin, bauxitic clay, Wingdale mix by proportioning raw materials;
(b) with the mixture high temperature melting of step (a), obtain the amorphous eutectic of composite silicon dioxide;
(c) eutectic with step (b) is described filler through grinding the amorphous eutectic powder of acquisition composite silicon dioxide;
Optional carry out (d) carries out surface treatment with the eutectic powder of step (c).
As optimal technical scheme, high temperature melting temperature described in described preparation method's step (b) is 1000-2500 ℃, such as being 1050 ℃, 1110 ℃, 1150 ℃, 1180 ℃, 1250 ℃, 1360 ℃, 1420 ℃, 1490 ℃, 1560 ℃, 1700 ℃, 1950 ℃, 2050 ℃, 2100 ℃, 2200 ℃, 2350 ℃, 2460 ℃, 2490 ℃ etc., be preferably 1300-1600 ℃.
As optimal technical scheme, the median size of the eutectic powder described in described preparation method's step (c) is 1-20 μ m, such as being 1.5 μ m, 2.2 μ m, 3 μ m, 5 μ m, 7 μ m, 9 μ m, 11 μ m, 14 μ m, 16 μ m, 19 μ m etc., maximum particle diameter≤35 μ m; Being preferably median size is 1-6 μ m, maximum particle diameter≤25 μ m.
Preferably, the surface treatment agent that the described surface treatment of step (d) is used is silane coupling agent, the titanate ester treatment agent, aluminate, zirconate, cationic surfactant, aniorfic surfactant, amphoterics, the neutral surface active agent, stearic acid, oleic acid, lauric acid and their metallic salt, resol, organic silicone oil, hexamethyldisilazane, one kind or two or more mixture in the polyoxyethylene glycol is preferably silane coupling agent, the titanate ester treatment agent, organic silicone oil, one kind or two or more mixture in the hexamethyldisilazane.
The amorphous eutectic powder of composite silicon dioxide is as the special quartzy silicon powder of a class performance, adopt in the composition alkali metal oxide content less than 2%, aluminoborosilicate quartz-like mixture carries out the serial deep processings such as extra-fine grinding, fine grading, being prepared into median size is 1~20 μ m, is a kind of novel green electronic powder material that can be applied to the large-scale integrated circuit substrate.Powder stuffing provided by the present invention not only has the high-performances such as high heat-resisting, high moisture-proof that the traditional silicon micro mist possesses, high filler loading capacity, low bulk, low-stress, low-friction coefficient, and compares with common composite silicon dioxide filler and to have lower thermal expansivity.Can increase substantially the over-all properties of large-scale integrated circuit substrate with the powder filled large-scale circuit substrate of the amorphous eutectic of composite silicon dioxide.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand that described embodiment only is used for helping to understand the present invention, should not be considered as concrete restriction of the present invention.
Specify such as nothing, various raw materials of the present invention all can obtain by commercially available; Or prepare according to the ordinary method of this area.Unless otherwise defined or explanation, same meanings of being familiar with of all specialties used herein and scientific words and those skilled in the art.Any method similar or impartial to described content and material all can be applicable in the inventive method in addition.
The experimental technique of unreceipted actual conditions in the following example is measured according to national standard usually.If there is not corresponding national standard, then carry out according to general international standard, normal condition or according to the condition that manufacturer advises.Unless otherwise indicated, otherwise all umbers are weight part, and all per-cents are weight percentage.
The preparation of embodiment 1 filler A1-A4
Get different proportioning raw materials batch mixings by the component concentration of filler of the present invention, utilize preparation method provided by the invention to make filler A1-A4, its composition and quality percentage composition see Table 1.
Comparative example: its composition and quality percentage composition see Table 1 filler B.
Table 1
Form | Filler A1 | Filler A2 | Filler A3 | Filler A4 | Filler B |
Silicon-dioxide | 64 | 61 | 70 | 57 | 55 |
Aluminium sesquioxide | 29 | 11 | 18 | 23 | 14 |
Calcium oxide+magnesium oxide | 4 | 26 | 11 | 18 | 6 |
Boron trioxide | -- | -- | -- | -- | 10 |
Sodium oxide+potassium oxide+Lithium Oxide 98min | 1.8 | 0.1 | 0.5 | -- | -- |
Ferric oxide | 0.6 | 0.3 | -- | 0.05 | -- |
The appraisal procedure of the filler of the filler of the invention described above and Comparative Examples being carried out stain and specific conductivity is as follows.
1, the assessment of powder stuffing stain
A) take by weighing sample 300g, put into the clean beaker of 1000mL;
B) with cleaned by ultrasonic vibration 400 eye mesh screens, clean with pure water rinsing again;
C) sample in the beaker is slowly poured in the off-the-shelf clean test sieve, added in the pure water dilution flushing beaker again and remain sample, vibration is rocked and is all poured into a residue sample in the test sieve gently;
D) to pouring the test sieve pure water rinsing of sample into, then screenings is poured in the clean beaker with pure water and observe, number stain number.
2, the assessment of powder specific conductivity
The 10g powder adds fully stirring in the 100ml water, tests electrical conductivity of water with conductivity measurement.
The stain of filler and the assessment result of specific conductivity see Table 2.
Table 2
The preparation of embodiment 2 resin combinations
The filler that the embodiment of the invention 1 and comparative example are made utilizes butanone to be modulated into the used resin adhesive liquid of copper coated foil plate, and wherein solids component accounts for 65%, and its component and content see Table 3.
Table 3
Material and composition thereof used among the embodiment are as follows:
Thermosetting resin A is the bisphenol A type epoxy resin that DOW Chemical is produced, and commodity are called DER530, epoxy equivalent (weight) 435g/eq.
Thermosetting resin B is the novolac epoxy that Hexion Specialty Chemicals company (former U.S. Bowden chemical company and German Berlet company) produces, and commodity are called EPR627-MEK80, and its epoxy equivalent (weight) is between 160~250g/eq.
Solidifying agent is the resol stiffening agent that Hexion Specialty Chemicals company produces, and commodity are called PHL6635M65.
Promotor is that Japanese four countries change into the 2MI that company produces.
The filler that embodiment 3 utilizes filler that the present invention makes and Comparative Examples to make prepares copper coated foil plate
(1) glue: solvent is added in the proportion container, stir the lower solution that adds respectively thermosetting resin, curing agent solution and curing catalyst; Stir after 2 hours, add filler, continue to stir after 4-8 hour, the gel time of sampling and testing glue (170 ℃ of constant temperature hot plates) is 200~300 seconds.
(2) impregnation: will soak the layers of reinforcement of glue by vertical or horizontal type impregnation machine, by conditions such as control extruding wheel speed, linear speed, wind-warm syndrome and furnace temperature, specifically take vertical impregnation machine demonstration example as extruding wheel speed :-1.3~-2.5 ± 0.1M/min; Main line speed: 4~18m/min; Wind-warm syndrome: 120~170 ℃; Furnace temperature: 130~220 ℃, make prepreg.
(3) compacting: after will reducing good prepreg and combining with Copper Foil, put into vacuum hotpressing machine, press certain temperature, time and pressure also finally make copper coated foil plate.
1.6mm the concrete demonstration example of thick veneer sheet compacting is:
Temperature formula: 130 ℃/30min+155 ℃/30min+190 ℃/90min+220 ℃/60min;
The pressure formula:
25Kgf.cm-2/30min+50Kgf.cm-2/30min+90Kgf.cm-2/120min+30Kgf.cm-2/90min;
Vacuum formula: 30mmHg/130min+800mmHg/130min.
Under these conditions, the prepreg that to adopt 8 thickness be 0.2mm is stacked layer by layer between the thick Copper Foil of 35 μ m, can make the thick copper-clad laminate of 1.6mm after hot pressing.
4 pairs of copper-clad laminates of embodiment carry out performance test
The assessment of thermal expansion size changing rate: utilize etching solution to remove the Copper Foil of substrate, cut into the size of 5mm.Use TMA device (TA company) to heat up with 10 ℃/min, measure sample 50-260 ℃ thickness direction rate of expansion.Table 4 contrasts with the plate property that the filler that utilizes Comparative Examples makes for utilizing the present invention to make filler.
Table 4
As can be seen from Table 4, compare and add the copper coated foil plate that common dioxide composite silicon powder makes, the composite silicon dioxide eutectic powder stuffing that the present invention is made adds the copper coated foil plate of making in the glue to and has lower thermal expansivity.
The above, it only is preferred embodiment of the present invention, be not that content to composition of the present invention imposes any restrictions, for the person of ordinary skill of the art, can make other various corresponding changes and distortion according to technical scheme of the present invention and technical conceive, every foundation technical spirit of the present invention or composition composition or content all belong in the scope of technical solution of the present invention any trickle modification, equivalent variations and modification that above embodiment does.
Claims (10)
1. the amorphous eutectic powder stuffing of composite silicon dioxide in the clad with metal foil plate, it is characterized in that, contain by weight percentage following component: silicon-dioxide 57~70wt%, aluminium sesquioxide 15~35wt%, magnesium oxide+calcium oxide≤40wt%, sodium oxide+potassium oxide+Lithium Oxide 98min≤2wt%.
2. filler according to claim 1 is characterized in that, contains by weight percentage following component: silicon-dioxide 60~66wt%, aluminium sesquioxide 23~28wt%, magnesium oxide+calcium oxide≤30wt%, sodium oxide+potassium oxide+Lithium Oxide 98min≤1wt%.
3. filler according to claim 1 and 2 is characterized in that, contains by weight percentage ferric oxide≤0.6wt%, be preferably≤0.2wt%, more preferably≤0.1wt%.
4. each described filler is characterized in that according to claim 1-3, and the stain number of described filler is less than 20/300g, preferably less than 15/300g, further preferably less than 10/300g.
5. each described filler is characterized in that according to claim 1-4, and the specific conductivity of described filler is≤200 μ s/cm, is preferably≤100 μ s/cm.
6. each described filler is characterized in that according to claim 1-5, and described filler is through surface treatment.
7. filler according to claim 6, it is characterized in that, the surface treatment agent that described surface treatment is used is silane coupling agent, the titanate ester treatment agent, aluminate, zirconate, cationic surfactant, aniorfic surfactant, amphoterics, the neutral surface active agent, stearic acid, oleic acid, lauric acid and their metallic salt, resol, organic silicone oil, hexamethyldisilazane, one kind or two or more mixture in the polyoxyethylene glycol is preferably silane coupling agent, the titanate ester treatment agent, organic silicone oil, one kind or two or more mixture in the hexamethyldisilazane.
8. each described filler is characterized in that according to claim 1-7, and the median size of described filler is 1-20 μ m, maximum particle diameter≤35 μ m; Being preferably median size is 1-6 μ m, maximum particle diameter≤25 μ m.
9. the preparation method of each described filler of claim 1-8 comprises the steps:
The mineral that (a) will comprise quartz sand, kaolin, bauxitic clay, Wingdale mix by proportioning raw materials;
(b) with the mixture high temperature melting of step (a), obtain the amorphous eutectic of composite silicon dioxide;
(c) eutectic with step (b) is described filler through grinding the amorphous eutectic powder of acquisition composite silicon dioxide;
Optional carry out (d) carries out surface treatment with the eutectic powder of step (c).
10. preparation method according to claim 9 is characterized in that, the high temperature melting temperature described in the step (b) is 1000-2500 ℃, is preferably 1300-1600 ℃;
Preferably, the median size of the eutectic powder described in the step (c) is 1-20 μ m, maximum particle diameter≤35 μ m; Being preferably median size is 1-6 μ m, maximum particle diameter≤25 μ m;
Preferably, the surface treatment agent that the described surface treatment of step (d) is used is silane coupling agent, the titanate ester treatment agent, aluminate, zirconate, cationic surfactant, aniorfic surfactant, amphoterics, the neutral surface active agent, stearic acid, oleic acid, lauric acid and their metallic salt, resol, organic silicone oil, hexamethyldisilazane, one kind or two or more mixture in the polyoxyethylene glycol,, be preferably silane coupling agent, the titanate ester treatment agent, organic silicone oil, one kind or two or more mixture in the hexamethyldisilazane.
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CN105802186A (en) * | 2016-03-18 | 2016-07-27 | 重庆市锦艺硅材料开发有限公司苏州分公司 | Packing and resin composition for copper-clad laminate and application of packing and resin composition in copper-clad laminate |
CN105968713A (en) * | 2015-11-23 | 2016-09-28 | 重庆市锦艺硅材料开发有限公司苏州分公司 | Preparation method of filling material used for copper-clad plate, resin composition used for copper-clad plate and copper-clad plate thereof |
CN108164151A (en) * | 2017-12-23 | 2018-06-15 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of ic substrate micro-scale surface modified glass powder |
CN113754979A (en) * | 2020-06-05 | 2021-12-07 | 浙江华正新材料股份有限公司 | Prepreg composition, prepreg, circuit board and printed circuit board |
CN114526595A (en) * | 2022-03-17 | 2022-05-24 | 湖南亿胜新材料有限公司 | Preparation device and preparation method of low-dielectric-constant silicon micro powder |
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CN105968713A (en) * | 2015-11-23 | 2016-09-28 | 重庆市锦艺硅材料开发有限公司苏州分公司 | Preparation method of filling material used for copper-clad plate, resin composition used for copper-clad plate and copper-clad plate thereof |
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CN108164151A (en) * | 2017-12-23 | 2018-06-15 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of ic substrate micro-scale surface modified glass powder |
CN113754979A (en) * | 2020-06-05 | 2021-12-07 | 浙江华正新材料股份有限公司 | Prepreg composition, prepreg, circuit board and printed circuit board |
CN114526595A (en) * | 2022-03-17 | 2022-05-24 | 湖南亿胜新材料有限公司 | Preparation device and preparation method of low-dielectric-constant silicon micro powder |
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