CN108359394A - A kind of processing method for copper coated foil plate nano silicon micronization - Google Patents
A kind of processing method for copper coated foil plate nano silicon micronization Download PDFInfo
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- C08K3/20—Oxides; Hydroxides
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- C08K2003/222—Magnesia, i.e. magnesium oxide
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Abstract
The invention belongs to nano silicon micronization processing technique fields, and in particular to a kind of processing method for copper coated foil plate nano silicon micronization, including raw material compounding, intermediate powder prepare and prepared by nano silicon micronization.The present invention has the following advantages compared with prior art：The content of silica and calcium oxide is reduced in the present invention, increase the content of aluminium oxide and boron oxide, while a variety of assisted oxidation objects being used cooperatively, through under mist projection granulating and laser irradiation matching requirements, obtain the compound reconstruct particle for having cavity between particle, obtain ground dielectric constant, soft new powder, performance stablizes, and heat resistance is strong, for copper coated foil plate, electric property can be avoided to be deteriorated, light easy assembling improves the stability of copper coated foil plate.
Description
Technical field
The invention belongs to nano silicon micronization processing technique fields, and in particular to a kind of for copper coated foil plate nano silicon micronization
Processing method.
Background technology
Nano silicon micronization (or nano silicon dioxide) has many unique properties, as quantum size, quantum tunneling are imitated
It answers, special optical and electrical properties and high Magnetoresistance Phenomena, high-strength, high-ductility, high stability under nonlinear resistance phenomenon and high temperature
Make it that there is anti-ultraviolet optical property Deng, these properties, intensity, elasticity, ageing resistance and the chemically-resistant of material can be improved
Property, have the function of adsorpting pigment ion, reduce pigment decaying, therefore, nano silicon micronization can be widely applied to catalyst carrier,
Polymer composite, electronic package material, high technology ceramics material, rubber, papermaking, plastics, binder, coating, optical fiber,
In the products such as hot investment casting, almost it is related to all industries using silicon powder, wherein as preparing the bases integrated circuit PCB material
The copper coated foil plate of material adds inorganic particle to improve its dielectric constant and hardness with glue, and Mohs' hardness is 5.5 or so, is passed through
Changing the content of silica and calcium oxide improves its performance, dielectric constant（1MZ）It is 4.57, dielectric loss（1MZ）For
0.014, as the requirement to its copper coated foil plate is higher and higher, need to further change the performance of nano silicon micronization.
Invention content
The purpose of the present invention is for existing problem, provide a kind of processing side for copper coated foil plate nano silicon micronization
Method.
The present invention is achieved by the following technical solutions：A kind of processing method for copper coated foil plate nano silicon micronization,
Include the following steps：
（1）Raw material compounds, by weight, including 43-47 parts of silica, 16-20 parts of calcium oxide, 22-26 parts of aluminium oxide, oxygen
Change 14-18 parts of boron, 1-3 parts of antimony oxide, 2-6 parts of copper oxide, 1-3 parts of magnesia, 0.2-0.8 parts of tin oxide, carbon nanotube 1-3
Part；
（2）Above-mentioned raw materials are milled to grain size and are less than after 2 μm the ultrasonic disperse in the ethanol solution that mass concentration is 10-18%, Gu
Liquid mass ratio is 3-5:1, the polyvinyl alcohol for being equivalent to ethanol solution weight 0.6-0.8% is added；
（3）Spray drying, rotating speed are 7500-8500 revs/min, and heat treatment temperature is 350-450 DEG C, processing time 2-3h,
200 mesh sieve is crossed, intermediate powder is obtained；
（4）It is 2.4 × 10 by the intermediate powder power density17-3.2×1019W/cm2 laser irradiate 2-4 minutes to get.
As further improvement of these options, ball milling, rotational speed of ball-mill are the mechanical milling process under nitrogen atmosphere
400-600 revs/min.
As further improvement of these options, the single-layer carbon nano-tube of 55-65wt% is included in the carbon nanotube.
As further improvement of these options, the step（2）The middle ultrasonic disperse time is no less than 40 minutes.
As further improvement of these options, the step（2）The time of middle ultrasonic disperse is 60-80 minutes.
As further improvement of these options, the step（4）Middle laser output wavelength is 800nm, pulsewidth 35fs.
The present invention has the following advantages compared with prior art：The content that silica and calcium oxide are reduced in the present invention, increases
Add the content of aluminium oxide and boron oxide, while a variety of assisted oxidation objects being used cooperatively, through mist projection granulating and laser irradiation cooperation
Under the conditions of, obtain the compound reconstruct particle for having cavity between particle, obtain ground dielectric constant, soft new powder, performance stablizes,
Heat resistance is strong, is used for copper coated foil plate, electric property can be avoided to be deteriorated, light easy assembling improves the stability of copper coated foil plate.
Specific implementation mode
Embodiment 1
A kind of processing method for copper coated foil plate nano silicon micronization includes the following steps：
（1）Raw material compound, by weight, including 45 parts of silica, 18 parts of calcium oxide, 24 parts of aluminium oxide, 16 parts of boron oxide,
2 parts of antimony oxide, 4 parts of copper oxide, 2 parts of magnesia, 0.5 part of tin oxide, 2 parts of carbon nanotube；
（2）Above-mentioned raw materials are milled to grain size and are less than after 2 μm ultrasonic disperse, solid-liquid in the ethanol solution that mass concentration is 14%
Mass ratio is 4:1, the polyvinyl alcohol for being equivalent to ethanol solution weight 0.7% is added；
（3）Spray drying, rotating speed are 8000 revs/min, and heat treatment temperature is 400 DEG C, processing time 2.5h, cross 200 mesh sieve,
Obtain intermediate powder；
（4）It is 5.8 × 10 by the intermediate powder power density18W/cm2 laser irradiate 3 minutes to get.
Wherein, ball milling, rotational speed of ball-mill are 500 revs/min to the mechanical milling process under nitrogen atmosphere；In the carbon nanotube
Include the single-layer carbon nano-tube of 60wt%；The step（2）The time of middle ultrasonic disperse is 70 minutes；The step（4）Middle laser
Output wavelength is 800nm, pulsewidth 35fs.
It being handled through 288 DEG C of wickings, heat-resistant time reaches 12 minutes or more, water absorption rate 0.47%, Mohs' hardness 3.4,
Dielectric constant（1MZ）It is 2.28, dielectric loss（1MZ）It is 0.006.
Embodiment 2
A kind of processing method for copper coated foil plate nano silicon micronization includes the following steps：
（1）Raw material compound, by weight, including 43 parts of silica, 20 parts of calcium oxide, 26 parts of aluminium oxide, 14 parts of boron oxide,
1 part of antimony oxide, 2 parts of copper oxide, 3 parts of magnesia, 0.2 part of tin oxide, 3 parts of carbon nanotube；
（2）Above-mentioned raw materials are milled to grain size and are less than after 2 μm ultrasonic disperse, solid-liquid in the ethanol solution that mass concentration is 18%
Mass ratio is 3:1, the polyvinyl alcohol for being equivalent to ethanol solution weight 0.6% is added；
（3）Spray drying, rotating speed are 8500 revs/min, and heat treatment temperature is 450 DEG C, processing time 2h, cross 200 mesh sieve, obtain
To intermediate powder；
（4）It is 3.2 × 10 by the intermediate powder power density19W/cm2 laser irradiate 2 minutes to get.
Wherein, ball milling, rotational speed of ball-mill are 600 revs/min to the mechanical milling process under nitrogen atmosphere；In the carbon nanotube
Include the single-layer carbon nano-tube of 65wt%；The step（2）The time of middle ultrasonic disperse is 80 minutes；The step（4）Middle laser
Output wavelength is 800nm, pulsewidth 35fs.
It being handled through 288 DEG C of wickings, heat-resistant time reaches 12 minutes or more, water absorption rate 0.46%, Mohs' hardness 3.3,
Dielectric constant（1MZ）It is 2.26, dielectric loss（1MZ）It is 0.005.
Embodiment 3
A kind of processing method for copper coated foil plate nano silicon micronization includes the following steps：
（1）Raw material compound, by weight, including 47 parts of silica, 16 parts of calcium oxide, 22 parts of aluminium oxide, 18 parts of boron oxide,
3 parts of antimony oxide, 6 parts of copper oxide, 1 part of magnesia, 0.8 part of tin oxide, 1 part of carbon nanotube；
（2）Above-mentioned raw materials are milled to grain size and are less than after 2 μm ultrasonic disperse, solid-liquid in the ethanol solution that mass concentration is 10%
Mass ratio is 5:1, the polyvinyl alcohol for being equivalent to ethanol solution weight 0.8% is added；
（3）Spray drying, rotating speed are 7500 revs/min, and heat treatment temperature is 350 DEG C, processing time 3h, cross 200 mesh sieve, obtain
To intermediate powder；
（4）It is 2.4 × 10 by the intermediate powder power density17W/cm2 laser irradiate 4 minutes to get.
Wherein, ball milling, rotational speed of ball-mill are 400 revs/min to the mechanical milling process under nitrogen atmosphere；In the carbon nanotube
Include the single-layer carbon nano-tube of 55wt%；The step（2）The time of middle ultrasonic disperse is 60 minutes；The step（4）Middle laser
Output wavelength is 800nm, pulsewidth 35fs.
It being handled through 288 DEG C of wickings, heat-resistant time reaches 12 minutes or more, water absorption rate 0.45%, Mohs' hardness 3.5,
Dielectric constant（1MZ）It is 2.32, dielectric loss（1MZ）It is 0.008.
Control group 1 is set, carbon nanotube in embodiment 1 is removed, remaining content is constant；It is handled through 288 DEG C of wickings, it is resistance to
The hot time reaches 20 seconds 9 minutes, water absorption rate 0.44%, Mohs' hardness 3.7, dielectric constant（1MZ）It is 2.45, dielectric loss
（1MZ）It is 0.013.
Control group 2 is set, magnesia in embodiment 1 is removed, remaining content is constant；It is handled through 288 DEG C of wickings, it is heat-resisting
Time reaches 40 seconds 10 minutes, water absorption rate 0.43%, Mohs' hardness 3.5, dielectric constant（1MZ）It is 2.37, dielectric loss
（1MZ）It is 0.013.
It can be seen that carbon nanotube and magnesia mating reaction are affected to the heat resistance of nano silicon micronization.
Control group 3 is set, by step in embodiment 1（4）Remove, remaining content is constant；It is handled through 288 DEG C of wickings, it is resistance to
The hot time reaches 12 minutes or more, water absorption rate 0.45%, Mohs' hardness 3.6, dielectric constant（1MZ）It is 2.87, dielectric loss
（1MZ）It is 0.016, illustrates that laser emission is affected to dielectric properties.
Claims (6)
1. a kind of processing method for copper coated foil plate nano silicon micronization, which is characterized in that include the following steps：
（1）Raw material compounds, by weight, including 43-47 parts of silica, 16-20 parts of calcium oxide, 22-26 parts of aluminium oxide, oxygen
Change 14-18 parts of boron, 1-3 parts of antimony oxide, 2-6 parts of copper oxide, 1-3 parts of magnesia, 0.2-0.8 parts of tin oxide, carbon nanotube 1-3
Part；
（2）Above-mentioned raw materials are milled to grain size and are less than after 2 μm the ultrasonic disperse in the ethanol solution that mass concentration is 10-18%, Gu
Liquid mass ratio is 3-5:1, the polyvinyl alcohol for being equivalent to ethanol solution weight 0.6-0.8% is added；
（3）Spray drying, rotating speed are 7500-8500 revs/min, and heat treatment temperature is 350-450 DEG C, processing time 2-3h,
200 mesh sieve is crossed, intermediate powder is obtained；
（4）It is 2.4 × 10 by the intermediate powder power density17-3.2×1019W/cm2 laser irradiate 2-4 minutes to get.
2. a kind of processing method for copper coated foil plate nano silicon micronization as described in claim 1, which is characterized in that the ball milling
Ball milling, rotational speed of ball-mill are 400-600 revs/min to process under nitrogen atmosphere.
3. a kind of processing method for copper coated foil plate nano silicon micronization as described in claim 1, which is characterized in that the carbon is received
Include the single-layer carbon nano-tube of 55-65wt% in mitron.
4. a kind of processing method for copper coated foil plate nano silicon micronization as described in claim 1, which is characterized in that the step
（2）The middle ultrasonic disperse time is no less than 40 minutes.
5. a kind of processing method for copper coated foil plate nano silicon micronization as claimed in claim 4, which is characterized in that the step
（2）The time of middle ultrasonic disperse is 60-80 minutes.
6. a kind of processing method for copper coated foil plate nano silicon micronization as described in claim 1, which is characterized in that the step
（4）Middle laser output wavelength is 800nm, pulsewidth 35fs.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1460657A (en) * | 2003-07-04 | 2003-12-10 | 北京工业大学 | Continuously adjustable and controllable power laser preparation method by using high dielectric constant Ta2O5 base ceramics |
| CN101752235A (en) * | 2008-12-08 | 2010-06-23 | 中芯国际集成电路制造(上海)有限公司 | Method for forming and processing high-K gate dielectric layer and method for forming transistor |
| CN103419439A (en) * | 2013-08-19 | 2013-12-04 | 陕西生益科技有限公司 | Manufacturing method of low-dielectric-constant CEM-3 copper-clad plate |
| CN103950940A (en) * | 2014-04-10 | 2014-07-30 | 周雨 | Preparation method for low-dielectric-constant fine silicon powder |
| CN105084373A (en) * | 2015-07-24 | 2015-11-25 | 陈林 | Method for preparing low-dielectric-constant silica powder |
-
2017
- 2017-12-30 CN CN201711489205.0A patent/CN108359394A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1460657A (en) * | 2003-07-04 | 2003-12-10 | 北京工业大学 | Continuously adjustable and controllable power laser preparation method by using high dielectric constant Ta2O5 base ceramics |
| CN101752235A (en) * | 2008-12-08 | 2010-06-23 | 中芯国际集成电路制造(上海)有限公司 | Method for forming and processing high-K gate dielectric layer and method for forming transistor |
| CN103419439A (en) * | 2013-08-19 | 2013-12-04 | 陕西生益科技有限公司 | Manufacturing method of low-dielectric-constant CEM-3 copper-clad plate |
| CN103950940A (en) * | 2014-04-10 | 2014-07-30 | 周雨 | Preparation method for low-dielectric-constant fine silicon powder |
| CN105084373A (en) * | 2015-07-24 | 2015-11-25 | 陈林 | Method for preparing low-dielectric-constant silica powder |
Non-Patent Citations (1)
| Title |
|---|
| 高祀建等: ""γ-射线辐照对电熔石英玻璃介电性质的影响"", 《物理学报》 * |
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Application publication date: 20180803 |