CN103359944B - Soft glass micro powder and preparation method thereof - Google Patents
Soft glass micro powder and preparation method thereof Download PDFInfo
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- CN103359944B CN103359944B CN201210081369.0A CN201210081369A CN103359944B CN 103359944 B CN103359944 B CN 103359944B CN 201210081369 A CN201210081369 A CN 201210081369A CN 103359944 B CN103359944 B CN 103359944B
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- 239000011521 glass Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000000843 powder Substances 0.000 title abstract description 24
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 19
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000292 calcium oxide Substances 0.000 claims abstract description 16
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 16
- 239000003595 mist Substances 0.000 claims description 37
- 239000000463 material Substances 0.000 claims description 26
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 17
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000945 filler Substances 0.000 description 9
- 230000006872 improvement Effects 0.000 description 8
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000007499 fusion processing Methods 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 230000008676 import Effects 0.000 description 5
- 239000011863 silicon-based powder Substances 0.000 description 5
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 3
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 3
- 229910001950 potassium oxide Inorganic materials 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- 229910001948 sodium oxide Inorganic materials 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000012764 mineral filler Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 238000009156 water cure Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Abstract
The invention relates to soft glass micro powder. The soft glass micro powder is characterized by comprising the following components in percent by weight: 35-54% of silicon oxide, 23-35% of aluminium oxide, 13-40% of calcium oxide and 0.1-4% of boron oxide, or 35-54% of silicon oxide, 1-11% of aluminium oxide, 13-40% of calcium oxide and 13-30% of boron oxide, or 66-75% of silicon oxide, 1-11% of aluminium oxide, 1-3% of calcium oxide and 13-30% of boron oxide, or 66-75% of silicon oxide, 1-11% of aluminium oxide, 13-40% of calcium oxide and 13-30% of boron oxide, or 66-75% of silicon oxide, 1-11% of aluminium oxide, 13-40% of calcium oxide and 0.1-4% of boron oxide. The soft glass micro powder has the beneficial effects that the soft glass micro powder is added with boron oxide, hardness of the soft glass micro powder is low, and mechanical property and electrical property of a copper-clad plate can be improved when the soft glass micro powder is applied to the copper-clad plate.
Description
Technical field
The present invention relates to a kind of glass micro mist, particularly relate to a kind of manufacturing that can be applicable to copper-clad plate to improve the soft glass micro mist of copper-clad plate performance.
Background technology
As everyone knows, in copper-clad plate resin glue, add the common practice that inorganic powder is copper-clad plate industry, add inorganic powder and improve the mechanical property of material after resin solidification, dimensional performance and electric property.As United States Patent (USP) 5264056 is pointed out, the dimensional stability adding the copper-clad plate after can improving Resin adhesive water cure of mineral filler, dimensional stability is an extremely important index in the rear road complete processing of copper-clad plate.Meanwhile, No. 222950, Japanese Patent, No. 97633 point out, inorganic powder add the mobility weakening resin glue, improve punching performance.In addition, add the good Alumina Inorganic powder of heat conductivility, improve the thermal conductivity of copper-clad plate in resin glue, high thermal conductivity is important indicators in some high-end copper-clad plates.
Along with the enforcement of electron trade lead-free and halogen-free standard, under copper-clad plate ensures the prerequisite of dimensional stabilizing in the processing in rear road, must can bear higher temperature.High glass-transition temperature, low-expansion copper-clad plate usage quantity increases sharply.Resin after this kind of copper-clad plate solidification is more crisp, and the stripping strength of Copper Foil is lower, and after adding common silica powder, hardness increases.Cause occurring white edge phenomenon in rear road machining, tool wear is accelerated simultaneously, and production cost significantly rises.The inorganic micro powder used in copper-clad plate industry respectively has relative merits: as alumina powder good heat conductivity, but hardness is high, and difficulty of processing is large; Ultrafine Mica hardness is low, but peel strength of copper foil is low.Aluminium hydroxide flame-retardant is excellent, but poor heat resistance.
Summary of the invention
For the deficiencies in the prior art, the technical problem that the present invention solves is to provide and a kind ofly reduces copper-clad plate cost, improves the soft glass micro mist of its mechanical property and electric property and the preparation method of this soft glass micro mist.
For solving the problems of the technologies described above, technical scheme of the present invention is achieved in that a kind of soft glass micro mist, and described soft glass micro mist comprises by weight percentage:
The silicon oxide of 35% ~ 54%, the aluminum oxide of 23% ~ 35%, the calcium oxide of 13% ~ 40%, the boron oxide of 0.1% ~ 4%;
Or the silicon oxide of 35% ~ 54%, the aluminum oxide of 1% ~ 11%, the calcium oxide of 13% ~ 40%, the boron oxide of 13% ~ 30%;
Or the silicon oxide of 66% ~ 75%, the aluminum oxide of 1% ~ 11%, the calcium oxide of 1% ~ 3%, the boron oxide of 13% ~ 30%;
Or the silicon oxide of 66% ~ 75%, the aluminum oxide of 1% ~ 11%, the calcium oxide of 13% ~ 40%, the boron oxide of 13% ~ 30%;
Or the silicon oxide of 66% ~ 75%, the aluminum oxide of 1% ~ 11%, the calcium oxide of 13% ~ 40%, the boron oxide of 0.1% ~ 4%.
As a further improvement on the present invention, described soft glass micro mist also comprises other oxide compounds, and other oxide compounds described comprise potassium oxide, sodium oxide or barium oxide.
As a further improvement on the present invention, described soft glass micro mist maximum particle diameter is less than or equal to 40 microns, and described soft glass micro mist median size is less than or equal to 10 microns.
As a further improvement on the present invention, described soft glass micro mist median size is 2 ~ 3 microns.
As a further improvement on the present invention, described soft glass micro mist surface is processed by silane coupling agent.
Technical scheme of the present invention can also realize like this:
A preparation method for above-mentioned soft glass micro mist, comprises the following steps:
(1) supply raw materials, described raw material takes by the proportioning of claim 1;
(2) melting in High Temperature Furnaces Heating Apparatus after being mixed by step (1) Raw, forms glass state material after complete reaction, and is incubated specific duration;
(3) glass state material in step (2) is carried out Quench, and then form soft glass micro mist by ball mill pulverizing and fine grading.
As a further improvement on the present invention, the melt temperature of described High Temperature Furnaces Heating Apparatus is 1400 DEG C ~ 1600 DEG C.
As a further improvement on the present invention, the specific duration in described step (2) is 6 ~ 12 hours.
As a further improvement on the present invention, the Mohs' hardness of described soft glass micro mist is between 4.5 ~ 5.5.
As a further improvement on the present invention, the pure water of described soft glass micro mist dissolves ion content at below 100ppm.
Compared with prior art, the invention has the beneficial effects as follows: the soft glass micro mist being added with boron oxide, its hardness is low, when for copper-clad plate, can improve mechanical property and the electric property of copper-clad plate.
Accompanying drawing explanation
Figure 1 shows that the preparation method of the soft glass micro mist of the present invention.
Embodiment
Below in conjunction with each embodiment shown in the drawings, the present invention is described in detail; but should be noted that; these embodiments are not limitation of the present invention; those of ordinary skill in the art are according to these embodiment institute work energy, method or structural equivalent transformations or substitute, and all belong within protection scope of the present invention.
Below by specific embodiment, the present invention is further elaborated (ginseng Fig. 1):
Embodiment one:
1) take soft glass powder material, raw material takes as following weight percent: silicon oxide 50%, aluminum oxide 24%, calcium oxide 24%, boron oxide 2%;
2) melting in High Temperature Furnaces Heating Apparatus after soft glass powder material being mixed, complete reaction in 1400 DEG C ~ 1600 DEG C high-temperature fusion processes, forms glass state material, and is incubated 6 ~ 12 hours;
3) high temp glass state material is after Quench, and by ball mill pulverizing and fine grading, form largest particle diameter and be not more than 40 microns, median size (D50) the glass micro mist that is less than 10 microns, median size is good with 2 ~ 3 microns.
Embodiment two:
1) take soft glass powder material, raw material takes as following weight percent: silicon oxide 54%, aluminum oxide 10%, calcium oxide 22%, boron oxide 13%;
2) melting in High Temperature Furnaces Heating Apparatus after soft glass powder material being mixed, complete reaction in 1400 DEG C ~ 1600 DEG C high-temperature fusion processes, forms glass state material, and is incubated 6 ~ 12 hours;
3) high temp glass state material is after Quench, and by ball mill pulverizing and fine grading, form largest particle diameter and be not more than 40 microns, median size (D50) the glass micro mist that is less than 10 microns, median size is good with 2 ~ 3 microns.
Embodiment three:
1) take soft glass powder material, raw material takes as following weight percent: silicon oxide 68%, aluminum oxide 5%, calcium oxide 3%, boron oxide 15%;
2) melting in High Temperature Furnaces Heating Apparatus after soft glass powder material being mixed, complete reaction in 1400 DEG C ~ 1600 DEG C high-temperature fusion processes, forms glass state material, and is incubated 6 ~ 12 hours;
3) high temp glass state material is after Quench, and by ball mill pulverizing and fine grading, form largest particle diameter and be not more than 40 microns, median size (D50) the glass micro mist that is less than 10 microns, median size is good with 2 ~ 3 microns.
Embodiment four:
1) take soft glass powder material, raw material takes as following weight percent: silicon oxide 66%, aluminum oxide 8%, calcium oxide 15%, boron oxide 20%, barium oxide 12%;
2) melting in High Temperature Furnaces Heating Apparatus after soft glass powder material being mixed, complete reaction in 1400 DEG C ~ 1600 DEG C high-temperature fusion processes, forms glass state material, and is incubated 6 ~ 12 hours;
3) high temp glass state material is after Quench, and by ball mill pulverizing and fine grading, form largest particle diameter and be not more than 40 microns, median size (D50) the glass micro mist that is less than 10 microns, median size is good with 2 ~ 3 microns.
Embodiment five:
1) take soft glass powder material, raw material takes as following weight percent: silicon oxide 66%, aluminum oxide 5%, calcium oxide 28%, boron oxide 2%;
2) melting in High Temperature Furnaces Heating Apparatus after soft glass powder material being mixed, complete reaction in 1400 DEG C ~ 1600 DEG C high-temperature fusion processes, forms glass state material, and is incubated 6 ~ 12 hours;
3) high temp glass state material is after Quench, and by ball mill pulverizing and fine grading, form largest particle diameter and be not more than 40 microns, median size (D50) the glass micro mist that is less than 10 microns, median size is good with 2 ~ 3 microns.
In above-described embodiment, other oxide compounds such as a small amount of potassium oxide, sodium oxide can also be added, to reduce fusing point.Certainly, in other embodiments, also itself may be mixed into other oxide compounds such as potassium oxide, sodium oxide in raw material, this oxide compound exists with Impure forms, and proportion is very little.
The performance of the soft glass micro mist of the present invention is described below in conjunction with the testing method of " adding the copper-clad plate drill test of various filler " and experimental data:
One, experiment purpose and method:
Under same experimental conditions, select different boring apparatus and different drill bits, the copper-clad plate of import 925 silicon powder of interpolation same ratio, soft glass micropowder filler of the present invention, aluminium hydroxide three kinds of fillers is carried out boring experiment, compare bit wear.
Two, the collection of experimental data:
Gather and embody the most important tread of bit wear, little Jiao, unfilled corner three groups of data, carry out intersection and compare, analyze wear pattern.Tread value is larger, illustrates that wearing and tearing are less; Little angle value is less, illustrates that wearing and tearing are less; Unfilled corner value is less, illustrates that wearing and tearing are less.
Three, experiment content
Scheme: the contrast of import 925 silicon powder and soft glass micropowder filler
1. experiment material: 1.6mm thickness glass fiber reinforcements copper-clad plate one deck
2. filler adding proportion: filler: resin=40:100
3. boring apparatus: pine forest MT CNC 2600 drilling machine
A) rotating speed: 105,000RPM
B) feed several times: 320CM/MIN
C) withdrawing speed: 1500CM/MIN
4. drill bit: brand-new HP TET(Hua Weina) 0.3MM drill bit
5. surveying instrument: MACHVISION POINTGAUGE
6. detect data
7. detect data analysis and conclusion
With the drill bit of 0.3mm, the copper-clad plate of the extraordinary soft-filler of import 925 silicon powder and bright and beautiful skill adding same ratio is bored 500 holes, 1,000 hole, 2,000 hole, and the tread of drill bit, little angle and unfilled corner data are deteriorated successively.
It is suitable that the bit wear that 500 holes and the copper-clad plate adding soft glass micropowder filler bore 2,000 hole is bored in the copper-clad plate adding import 925 silicon powder.
Four, experiment conclusion
Above data show, the bit wear of processing interpolation soft glass micropowder filler copper-clad plate is the 1/3-1/4 of import 925 silicon powder.
In addition, the present invention's soft glass micro mist also has following beneficial effect:
Soft glass micro mist prepared by the present invention, owing to being added with boron oxide, its Mohs' hardness, between 4.5 ~ 5.5, greatly reduces the abrasion loss of copper-clad plate cutter in rear road cutting process.
Soft glass micro mist prepared by the present invention, its pure water dissolves ion content at below 100ppm.
Prepared by the present invention, soft glass micro mist adds in the glue of copper-clad plate, greatly improves the dimensional stability of copper-clad plate after solidification, and the stripping strength of its Copper Foil does not also obviously reduce.
Prepared by the present invention, soft glass micro mist, adds in the glue of copper-clad plate, and after solidification, the electric property of copper-clad plate does not obviously reduce.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.Any Reference numeral in claim should be considered as the claim involved by limiting.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (2)
1. a soft glass micro mist, is characterized in that, described soft glass micro mist comprises by weight percentage: the silicon oxide of 50%, the aluminum oxide of 24%, the calcium oxide of 24% and the boron oxide of 2%; Described soft glass micro mist maximum particle diameter is less than or equal to 40 microns, and described soft glass micro mist median size is 2 ~ 3 microns.
2. the preparation method of a kind of soft glass micro mist as claimed in claim 1, is characterized in that, comprise the following steps:
(1) supply raw materials, described raw material takes by the proportioning of claim 1;
(2) melting in High Temperature Furnaces Heating Apparatus after being mixed by step (1) Raw, forms glass state material after complete reaction, and is incubated specific duration;
(3) glass state material in step (2) is carried out Quench, and then form soft glass micro mist by ball mill pulverizing and fine grading;
Wherein,
Described High Temperature Furnaces Heating Apparatus melt temperature is 1400 DEG C to 1600 DEG C, specific duration in described step (2) is 6 to 12 hours, the Mohs' hardness of described soft glass micro mist is between 4.5 to 5.5, and the pure water of described soft glass micro mist dissolves ion content at below 100ppm.
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| CN201210081369.0A CN103359944B (en) | 2012-03-26 | 2012-03-26 | Soft glass micro powder and preparation method thereof |
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| CN103359944B true CN103359944B (en) | 2015-07-22 |
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| CN105968713B (en) * | 2015-11-23 | 2018-01-23 | 苏州海旭新材料科技有限公司 | A kind of preparation method of copper-clad plate filler, copper-clad plate resin combination and copper-clad plate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962760A (en) * | 2005-11-11 | 2007-05-16 | 旭玻璃纤维股份有限公司 | Glass filler for polycarbonate resin, and polycarbonate resin composition |
| CN101094818A (en) * | 2004-05-29 | 2007-12-26 | 肖特股份公司 | Nano glass powder and use thereof, particularly multicomponent glass powder with a mean particle size of less than 1 [mu]m |
| CN101547558A (en) * | 2009-04-21 | 2009-09-30 | 无锡宏仁电子材料科技有限公司 | Copper clad base plate and preparation method thereof |
| CN102088820A (en) * | 2009-12-03 | 2011-06-08 | 新加坡商矽比科亚洲有限公司 | Copper clad laminate and impregnation liquid for making same |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0791086B2 (en) * | 1989-04-26 | 1995-10-04 | 日東紡績株式会社 | Glass powder for thermosetting resin moldings |
| JPH05155638A (en) * | 1991-12-06 | 1993-06-22 | Nippon Electric Glass Co Ltd | Glass composition |
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2012
- 2012-03-26 CN CN201210081369.0A patent/CN103359944B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101094818A (en) * | 2004-05-29 | 2007-12-26 | 肖特股份公司 | Nano glass powder and use thereof, particularly multicomponent glass powder with a mean particle size of less than 1 [mu]m |
| CN1962760A (en) * | 2005-11-11 | 2007-05-16 | 旭玻璃纤维股份有限公司 | Glass filler for polycarbonate resin, and polycarbonate resin composition |
| CN101547558A (en) * | 2009-04-21 | 2009-09-30 | 无锡宏仁电子材料科技有限公司 | Copper clad base plate and preparation method thereof |
| CN102088820A (en) * | 2009-12-03 | 2011-06-08 | 新加坡商矽比科亚洲有限公司 | Copper clad laminate and impregnation liquid for making same |
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