CN103450499B - Filler in a kind of metal-clad foil plate of the insulativity had and preparation method thereof - Google Patents
Filler in a kind of metal-clad foil plate of the insulativity had and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to the amorphous eutectic powder stuffing of composite silicon dioxide in a kind of metal-clad foil plate, by weight percentage containing following component: silicon-dioxide 50 ~ 70wt%, aluminium sesquioxide 5 ~ 25wt%, boron trioxide 3 ~ 20wt%, calcium oxide≤5wt%, magnesium oxide≤4wt%.Filler provided by the present invention not only improves the processibility of electric substrate, makes the metal-clad foil plate obtained have good insulativity simultaneously.
Description
Technical field
The present invention relates to filler in a kind of metal-clad foil plate and preparation method thereof, particularly relate to amorphous eutectic powder stuffing of composite silicon dioxide in a kind of metal-clad foil plate and preparation method thereof.
Background technology
When using filler in metal-clad foil plate (such as CEM-3) in the past, many employing aluminium hydroxide and magnesium hydroxide.But more than 200 degree Celsius, aluminium hydroxide just starts to decompose, thermo-labile impact, and 230 DEG C, 300 DEG C, 530 DEG C of three phases discharge crystal water, easily cause plate material lamination to bubble, so, heat-treat; And magnesium hydroxide price is partially expensive.
Silicon-dioxide (SiO
2) then there is excellent physical property, as having 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, there is value of exploiting and utilizing very much.Along with the improvement of silicon-dioxide its own face treatment condition, improve the consistency of it and resin system, so the filler silicon powder made as major ingredient with silicon-dioxide is applied in metal-clad foil plate, not only can reduce costs, some performance (as thermal expansivity, flexural strength, dimensional stability etc.) of metal-clad foil plate can also be improved, therefore 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) through the micro mist of the multiple tracks processes such as broken, ball milling (or vibration, airflow milling), flotation, pickling purification, high purity water process.Silicon powder is a kind of nontoxic, tasteless, free of contamination ceramic.Due to it possess that temperature tolerance is good, the excellent performance such as acid-alkali-corrosive-resisting, poor thermal conductivity, high insulation, low bulk, stable chemical performance, hardness are large, be widely used in the fields such as chemical industry, electronics, unicircuit (IC), electrical equipment, plastics, coating, senior paint, rubber, national defence.
The leadless environment-friendly requirement of electron trade, has promoted the application of silicon powder in clad with metal foil board industry.At the initial stage of application, in order to pursue high thermotolerance and reduce costs, a lot of metal-clad foil plate producer adds the dihedral silicon-dioxide of mineral fragmentation in a large number.The use of this dihedral silicon-dioxide brings the problem of a series of production and processing, as the impact of dispersing technology, and the wearing and tearing etc. of glue application device; What have the greatest impact is make significantly improving of the tooling cost of downstream printed circuit board (pcb) producer, as boring, and the raising of milling plate cost and press tool cost.In order to improve the processibility of powder, change one of powder composition method becoming consideration.
Silicon releases the G2-C product improving processibility than section, and has applied for the invention CN102088820A that this powder is applied on copper clad laminate.The filler of this disclosure of the invention is by silicon-dioxide 50-62wt%, aluminium sesquioxide 11-19wt%, boron trioxide 4-13wt%, calcium oxide 6-27wt%, the amorphism reticulated structure that magnesium oxide < 6wt%, strontium oxide < 1.5wt% and barium oxide < 0.1wt% is formed altogether.Wuxi Hongren Electron Material Science Co., Ltd has applied for invention CN101547558A, this disclosure of the invention using method of mineral filler in copper-clad plate, wherein mineral filler is compound silica powder, by 55%-65% silicon-dioxide, 15%-35% aluminium sesquioxide, other oxide compound composition of the melting of 5%-15% boron trioxide and 0%-10%, other oxide compound refers to calcium oxide, sodium oxide or potassium oxide.Elite Material Co. and silicon are combined than section and have been applied for the application invention CN101857735A of comprehensive silicon micro mist in copper-clad plate.The composition of this disclosure of the invention silicon dioxide eutectic thing and preparation method, wherein eutectic is composed as follows: silicon-dioxide, its weight percent is 55 ~ 65wt%; Aluminium sesquioxide, its weight percent is 12 ~ 22wt%; Boron trioxide, its weight percent is 5 ~ 15wt%; Calcium oxide, its weight percent is 4 ~ 12wt%; Magnesium oxide, its weight percent is 0 ~ 6wt%; And a mixed metal oxide, being made up of sodium oxide, potassium oxide and ferric oxide, its weight percent is less than 1wt%.
As the filler used in electronic material substrate except considering except the impact of processibility, also need the factor on affecting powder insulativity, as alkalimetal oxide, especially the content of calcium oxide, magnesium oxide, potassium oxide, sodium oxide and the content of the stain and ferric oxide that affect insulating property have restriction, and foregoing invention can not meet the requirement of electronic circuit board to powder insulativity completely to the restriction of these materials.
Summary of the invention
The object of the invention is to for after the metal-clad foil plate of use silicon powder filler making at present, the problem of insulating property deficiency, provides a kind of composite silicon dioxide amorphous eutectic powder stuffing.Filler provided by the invention adopts suboxide calcium, low ferric oxide, low stain content composition composite silicon dioxide eutectic powder, and this powder not only improves the processibility of electric substrate, makes the metal-clad foil plate obtained have good insulativity simultaneously.
In order to achieve the above object, present invention employs following technical scheme:
The amorphous eutectic powder stuffing of composite silicon dioxide in a kind of metal-clad foil plate, by weight percentage containing following component: silicon-dioxide 50 ~ 70wt%, be such as 51wt%, 54wt%, 56wt%, 59wt%, 61wt%, 64wt%, 66wt%, 69wt% etc., aluminium sesquioxide 5 ~ 25wt%, be such as 6wt%, 8wt%, 9wt%, 12wt%, 16wt%, 19wt%, 21wt%, 23wt%, 24wt% etc., boron trioxide 3 ~ 20wt%, be such as 4wt%, 6wt%, 9wt%, 12wt%, 16wt%, 18wt%, 19wt% etc., calcium oxide≤5wt%, be such as 0.4wt%, 0.8wt%, 1wt%, 1.6wt%, 2.2wt%, 3wt%, 3.4wt%, 3.9wt%, 4.5wt%, 4.9wt% etc., magnesium oxide≤4wt%, be such as 0.2wt%, 0.6wt%, 1.1wt%, 1.6wt%, 2.1wt%, 2.4wt%, 2.8wt%, 3.3wt%, 3.7wt%, 3.9wt% etc.
As optimal technical scheme, filler of the present invention, by weight percentage containing following component: silicon-dioxide 55 ~ 65wt%, aluminium sesquioxide 10 ~ 20wt%, boron trioxide 5 ~ 14wt%, calcium oxide≤4wt%, magnesium oxide≤2wt%.
Metal oxide boron trioxide, calcium oxide, magnesian content directly affects the insulativity of the sheet material prepared with filler of the present invention, especially the filler containing calcium oxide easily separates out calcium ion under moisture conditions, form conductive path, thus the insulativity of the sheet material of impact preparation.Therefore, the content of calcium oxide is defined as≤5wt% by the present invention, is preferably≤4wt%, is particularly preferably≤3wt%.
As optimal technical scheme, filler of the present invention, by weight percentage containing ferric oxide≤0.6wt%, be such as 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%.Ferric oxide is can conducting material, is limited in 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 composite silicon dioxide eutectic powder, by analysis, stain major part for black can conducting material, therefore, stain not only can affect the apparent of base material, and more affects the insulativity of base material.Therefore, the stain number of amorphous for described composite silicon dioxide eutectic powder is less than 20/300g by the present invention, be such as 3/300g, 5/300g, 8/300g, 11/300g, 14/300g, 16/300g, 18/300g etc., preferably be less than 15/300g, be preferably less than 10/300g further.
As optimal technical scheme, the specific conductivity of filler of the present invention is≤200 μ s/cm, be such as 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 ensure 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, bad with organic resin matrix consistency, therefore, need to do surface treatment with surface treatment agent to it, to increase the consistency of itself and matrix.
Preferably, the surface treatment agent that the surface treatment stated uses is 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, one kind or two or more mixture in polyoxyethylene glycol, be preferably the one kind or two or more mixture in silane coupling agent, titanate ester treatment agent, organic silicone oil, hexamethyldisilazane.
As optimal technical scheme, the median size of filler of the present invention is 1-20 μm, such as, be 2 μm, 4 μm, 6 μm, 7 μm, 9 μm, 12 μm, 15 μm, 17 μm, 19 μm etc., maximum particle diameter≤35 μm; Being preferably median size is 1-6 μm, maximum particle diameter≤25 μm.
An object of the present invention is also the preparation method providing described filler, comprises the steps:
(a) by comprise quartz sand, kaolin, bauxitic clay, Wingdale, boron magnesium ore deposit mineral mix by proportioning raw materials;
B (), by the mixture high temperature melting of step (a), obtains the amorphous eutectic of composite silicon dioxide;
C the eutectic of step (b) is obtained composite silicon dioxide amorphous eutectic powder through grinding and is described filler by ();
Optionally carry out (d) and the eutectic powder of step (c) is carried out surface treatment.
As optimal technical scheme, high temperature melting temperature described in described preparation method's step (b) is 1000-2500 DEG C, be such as 1050 DEG C, 1110 DEG C, 1150 DEG C, 1180 DEG C, 1250 DEG C, 1360 DEG C, 1420 DEG C, 1490 DEG C, 1560 DEG C, 1700 DEG C, 1950 DEG C, 2050 DEG C, 2100 DEG C, 2200 DEG C, 2350 DEG C, 2460 DEG C, 2490 DEG C etc., be preferably 1300-1600 DEG C.
As optimal technical scheme, the median size of the eutectic powder described in described preparation method's step (c) is 1-20 μm, be such as 1.5 μm, 2.2 μm, 3 μm, 5 μm, 7 μm, 9 μm, 11 μm, 14 μm, 16 μm, 19 μm etc., maximum particle diameter≤35 μm; Being preferably median size is 1-6 μm, maximum particle diameter≤25 μm.
Preferably, the surface treatment agent that surface treatment described in step (d) uses is 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, one kind or two or more mixture in polyoxyethylene glycol, be preferably silane coupling agent, titanate ester treatment agent, organic silicone oil, one kind or two or more mixture in hexamethyldisilazane.
Composite silicon dioxide amorphous eutectic powder is as the special quartzy silicon powder of a class performance, adopt and the serial deep processing such as extra-fine grinding, fine grading is carried out to aluminoborosilicate quartz-like mixture, being prepared into median size is 1 ~ 20 μm, is a kind of novel green electronic powder material that can be applied to large-scale integrated circuit substrate.This powder not only has the high-performance such as heat-resisting, the high moisture-proof of height, high filler loading capacity, low bulk, low-stress, low-friction coefficient that traditional silicon micro mist possesses, and with substrate framework material (mainly alkali-free glass cloth), there is splendid consistency, Mohs' hardness is far below Conventional filling material.The over-all properties of large-scale integrated circuit substrate can be increased substantially 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, described embodiment only understands the present invention for helping, and should not be considered as concrete restriction of the present invention.
As no specific instructions, various raw material of the present invention all can be obtained by commercially available; Or prepare according to the ordinary method of this area.Unless otherwise defined or described herein, all specialties used herein and scientific words and those skilled in the art the same meaning be familiar with.In addition any method similar or impartial to described content and material all can be applicable in the inventive method.
The experimental technique of unreceipted actual conditions in the following example, measures according to national standard usually.If there is no corresponding national standard, then according to general international standard, normal condition or carry out according to the condition that manufacturer advises.Unless otherwise indicated, otherwise all numbers are weight part, and all per-cent is 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 obtain filler A1-A4, its composition and mass percentage are in table 1.
Comparative example: its composition and mass percentage are in filler B, C, D, E of table 1.
Table 1
Filler C is the preferred embodiment of CN101857735A.
The appraisal procedure of the filler of the invention described above and the filler of comparative example being carried out to stain and specific conductivity is as follows.
1, the assessment of powder stuffing stain
A) take sample 300g, put into the clean beaker of 1000mL;
B) with cleaned by ultrasonic vibration 400 eye mesh screen, cleaner by pure water rinsing;
C) slowly poured in off-the-shelf clean test sieve by sample in beaker, then add pure water dilution and rinse in beaker and remain sample, vibration is rocked and a residue sample is all poured in test sieve gently;
D) to the test sieve pure water rinsing pouring sample into, then screenings pure water is poured in clean beaker and observe, number stain number.
2, the assessment of powder specific conductivity
10g powder adds in 100ml water and fully stirs, and tests electrical conductivity of water with conductivity measurement.
The stain of filler and the assessment result of specific conductivity are in table 2.
Table 2
The preparation of embodiment 2 resin combination
Utilized by the filler that the embodiment of the present invention 1 and comparative example obtain butanone to be modulated into copper coated foil plate resin adhesive liquid used, wherein solids component accounts for 65%, and its component and content are in table 3.
Table 3
Material used in embodiment and composition 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 (Bowden chemical company of the former U.S. 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 phenolic resin hardener that Hexion Specialty Chemicals company produces, and commodity are called PHL6635M65.
Promotor is the 2MI that Japanese four countries change into company's production.
Copper coated foil plate prepared by the filler that embodiment 3 utilizes the present invention to obtain and the filler that comparative example obtains
(1) glue: added by solvent in proportion container, adds the solution of thermosetting resin, curing agent solution and curing catalyst respectively under stirring; Stir after 2 hours, add filler, continue to stir after 4-8 hour, the gel time (170 DEG C of constant temperature hot plates) of sampling and testing glue is 200 ~ 300 seconds.
(2) impregnation: by the layers of reinforcement of dipped glue by vertical or horizontal type impregnation machine, by controlling the conditions such as extruding wheel speed, linear speed, wind-warm syndrome and furnace temperature, with vertical impregnation machine demonstration example is specifically: extruding wheel speed :-1.3 ~-2.5 ± 0.1M/min; Main line speed: 4 ~ 18m/min; Wind-warm syndrome: 120 ~ 170 DEG C; Furnace temperature: 130 ~ 220 DEG C, obtained prepreg.
(3) suppress: after the prepreg reduced and Copper Foil being combined, put into vacuum hotpressing machine, by certain temperature, time and pressure is final obtained copper coated foil plate also.
The concrete demonstration example of the veneer sheet compacting that 1.6mm is thick is:
Temperature formula: 130 DEG C/30min+155 DEG C/30min+190 DEG C/90min+220 DEG C/60min;
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, adopt 8 thickness to be that the prepreg of 0.2mm is stacked layer by layer between 35 μm of thick Copper Foils, the thick copper-clad laminate of 1.6mm can be obtained after hot pressing.
Embodiment 4 pairs of copper-clad laminates carry out performance test
Volume resistance: test by standard GB/T4722-92 the 7th chapter.
Resistance to electric arc: test by standard Q/GDSY6050-20122.5.1.
Test result is in table 4.
Table 4
As can be seen from Table 4, compare and add the obtained copper coated foil plate of common dioxide composite silicon powder, composite silicon dioxide eutectic powder stuffing the present invention obtained adds the copper coated foil plate made in glue to and has better insulating property.Contrasted by embodiment 2 and comparative example 2, can obviously find out, calcium oxide ratio is lower, obviously can improve the insulating property of the sheet material of preparation.
The above, be only preferred embodiment of the present invention, not the content of composition of the present invention is imposed any restrictions, for the person of ordinary skill of the art, other various corresponding change and distortion can be made according to technical scheme of the present invention and technical conceive, every above embodiment is done according to technical spirit of the present invention or composition composition or content any trickle amendment, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (17)
1. the amorphous eutectic powder stuffing of the composite silicon dioxide in metal-clad foil plate, is characterized in that, by weight percentage containing following component: silicon-dioxide 50 ~ 70wt%, aluminium sesquioxide 5 ~ 25wt%, boron trioxide 3 ~ 20wt%, calcium oxide≤3wt%, magnesium oxide≤4wt%;
Wherein, the stain number of described filler is less than 20/300g, and the specific conductivity of described filler is≤200 μ s/cm;
The median size of described filler is 1-20 μm, maximum particle diameter≤35 μm.
2. filler according to claim 1, is characterized in that, by weight percentage containing following component: silicon-dioxide 55 ~ 65wt%, aluminium sesquioxide 10 ~ 20wt%, boron trioxide 5 ~ 14wt%, calcium oxide≤3wt%, magnesium oxide≤2wt%.
3. filler according to claim 1 and 2, is characterized in that, by weight percentage containing ferric oxide≤0.6wt%.
4. filler according to claim 1 and 2, is characterized in that, the stain number of described filler is less than 15/300g.
5. filler according to claim 1 and 2, is characterized in that, the specific conductivity of described filler is≤100 μ s/cm.
6. filler according to claim 1 and 2, is characterized in that, 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 uses is silane coupling agent, titanate ester treatment agent, aluminate, zirconate, cationic surfactant, aniorfic surfactant, amphoterics, neutral surface active agent, resol, organic silicone oil, one kind or two or more mixture in hexamethyldisilazane.
8. filler according to claim 6, is characterized in that, the surface treatment agent that described surface treatment uses is stearic acid, oleic acid, lauric acid and their metallic salt, one kind or two or more mixture in polyoxyethylene glycol.
9. filler according to claim 7, is characterized in that, the surface treatment agent that described surface treatment uses is silane coupling agent, one kind or two or more mixture in titanate ester treatment agent, organic silicone oil, hexamethyldisilazane.
10. filler according to claim 1, is characterized in that, the median size of described filler is 1-6 μm, maximum particle diameter≤25 μm.
Described in 11. 1 kinds of any one of claim 1-10, the preparation method of filler, comprises the steps:
(a) by comprise quartz sand, kaolin, bauxitic clay, Wingdale, boron magnesium ore deposit mineral mix by proportioning raw materials;
B (), by the mixture high temperature melting of step (a), obtains the amorphous eutectic of composite silicon dioxide;
C the eutectic of step (b) is obtained composite silicon dioxide amorphous eutectic powder through grinding and is described filler by ();
Optionally carry out (d) and the eutectic powder of step (c) is carried out surface treatment.
12. preparation methods according to claim 11, is characterized in that, the high temperature melting temperature described in step (b) is 1000-2500 DEG C.
13. preparation methods according to claim 11, is characterized in that, the median size of the eutectic powder described in step (c) is 1-20 μm, maximum particle diameter≤35 μm.
14. preparation methods according to claim 13, is characterized in that, the median size of described eutectic powder is 1-6 μm, maximum particle diameter≤25 μm.
15. preparation methods according to claim 11, it is characterized in that, the surface treatment agent that surface treatment described in step (d) uses is silane coupling agent, titanate ester treatment agent, aluminate, zirconate, cationic surfactant, aniorfic surfactant, amphoterics, neutral surface active agent, resol, organic silicone oil, one kind or two or more mixture in hexamethyldisilazane.
16. preparation methods according to claim 11, is characterized in that, the surface treatment agent that described surface treatment uses is stearic acid, oleic acid, lauric acid and their metallic salt, one kind or two or more mixture in polyoxyethylene glycol.
17. preparation methods according to claim 15, is characterized in that, the surface treatment agent that described surface treatment uses is silane coupling agent, one kind or two or more mixture in titanate ester treatment agent, organic silicone oil, hexamethyldisilazane.
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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 |
| CN114526595B (en) * | 2022-03-17 | 2022-10-04 | 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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| CN101857735B (en) * | 2009-04-07 | 2012-12-12 | 台光电子材料股份有限公司 | Silicon dioxide eutectic filling material and preparation method of laminate |
| CN101547558B (en) * | 2009-04-21 | 2011-04-13 | 无锡宏仁电子材料科技有限公司 | Copper clad base plate and preparation method thereof |
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Address after: 222000, No. 6, Sinpo Economic Development Zone, Haizhou District, Jiangsu, Lianyungang, Zhujianglu Road Applicant after: JIANGSU LIANRUI NEW MATERIAL CO., LTD. Address before: 222000 No. 6, Sinpo Economic Development Zone, Lianyungang, Jiangsu, Zhujianglu Road Applicant before: JIANGSU LIANRUI NEW MATERIAL CO., LTD. |
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