CN106219561A - A kind of preparation method of fillet silicon metal micropowder - Google Patents
A kind of preparation method of fillet silicon metal micropowder Download PDFInfo
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- CN106219561A CN106219561A CN201610610504.4A CN201610610504A CN106219561A CN 106219561 A CN106219561 A CN 106219561A CN 201610610504 A CN201610610504 A CN 201610610504A CN 106219561 A CN106219561 A CN 106219561A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The present invention is the preparation method of a kind of fillet silicon metal micropowder, and the method comprises the steps: to join in fillet processing equipment D50 at the dihedral silicon metal micropowder of 10 60 μm, starts equipment agitating function, adds deionized water while stirring；Regulate pressure, heating-up temperature and milling time after adding deionized water, start to grind；Described grinding divides 3 stages to carry out, and grinds after terminating, again regulates pressure, heating-up temperature and drying time, and the silicon powder after grinding is dried；In drying course, pressure is set to 0 MPa, and heating-up temperature is set to 100 110 DEG C, and drying time is 1 3h.Silicon powder after drying removes ferrum through screening machine screening with tramp iron separator, obtains fillet silicon metal micropowder.Fillet micropowder good fluidity, loading that the inventive method prepares, thermal conductivity is high, technique is simple and convenient to operate, preparation process environmental protection.
Description
Technical field
The present invention relates to the preparation method of a kind of fine silica powder, particularly to the preparation of a kind of fillet silicon metal micropowder
Method.
Background technology
Along with developing rapidly of microelectronic packaging technology, also drive currently as main electronic package material epoxy mould
The fast development of plastics.In epoxy molding plastic, the content of filler is up to 60% one 90%, so the selection scheme of filler and property thereof
The performance of epoxy molding plastic can there be is the very important topmost fine silica powder of filler affecting epoxy molding plastic, though
So silicon powder has different classification, but they are as filling, have common feature, it is simply that can improve certain seed ginseng of EMC
Number and characteristic, such as: contraction can be reduced, increase intensity, enhancing wearability, raising thermal distorsion temperature, raising thermal conductivity, reduction
Thermal coefficient of expansion, reduction cost, etc..They have general character, there is individual character too, such as: ball-shaped silicon micro powder is than dihedral silicon
Micropowder has bigger loading, has good mobility, crack resistance etc.；Molten silicon micropowder has low heat conductivity and low line is swollen
Swollen coefficient；Silicon metal micropowder has higher thermal conductivity.Although ball-shaped silicon micro powder excellent performance, there is good mobility, but
The shortcomings such as ball-shaped silicon micro powder cost is high, thermal conductivity is low to a certain degree limit its application, so occurring in that a kind of fillet on market
Silicon metal micropowder, also known as obtuse angle silicon powder, class ball-shaped silicon micro powder.Compared to common dihedral silicon metal micropowder, fillet silicon powder
Grain does not has sharp-pointed corner angle, mobility and loading the highest, can be micro-in conjunction with ball-shaped silicon micro powder good fluidity and silicon metal
The advantage that powder thermal conductivity is high, applies in requiring good fluidity and the high moulding compound of thermal conductivity.Compared to ball-shaped silicon micro powder, due to
Production technology is different, and the cost of fillet silicon powder is less, and mobility is preferable, so existing market large usage quantity, to this environmental protection,
The fillet silicon powder product demand that high heat conduction, height are filled is in rising trend, and this type of production technology is substantially by abroad
Business monopoly, associated production technology is urgently to be resolved hurrily.
In prior art: the Chinese patent document of Application No. 201410286355.1, it is with waste and old silica crucible
For raw material, finally obtain melted obtuse angle quartz sand through overpickling, melted, broken, magnetic separation.Application No. 201210070479.7
China's patent document, with quartz sand as raw material, through magnetic separation, melt, crush, sort, the technique such as grinding produces obtuse angle
Molten silicon micropowder.Although this two patents product is obtuse angle powder, but being molten state, production process needs high-temperature fusion, energy consumption
Height, molten state thermal conductivity is the lowest, and the spent acid produced in first patent production process pollutes environment, is unsatisfactory for environmental protection and wants
Ask.The Chinese patent document of Application No. 201010000299.2, is with natural powdery quartz as raw material, adds in Ultrafine Grinding
Enter mineral acid to be ground, add reducing agent and chelating agent, be washed out, dry, obtain the silicon powder that class is spherical.This invention
Not only can product spent acid, and also have other chemical agents, serious environment pollution, grind also cannot guarantee to obtain the spherical silicon of class
Micropowder.
Summary of the invention
The technical problem to be solved is for the deficiencies in the prior art, it is provided that a kind of production technology is simple, behaviour
Make convenient, the preparation method of production process free of contamination fillet silicon metal micropowder.
The technical problem to be solved is to be achieved through the following technical solutions.The present invention is a kind of fillet crystallization
The preparation method of silicon powder, is characterized in, the method comprises the steps:
(1) D50 is joined in fillet processing equipment at the dihedral silicon metal micropowder of 10-60 μm, start equipment agitating function, limit
Stirring limit adds deionized water；Regulate pressure, heating-up temperature and milling time after adding deionized water, start to grind；Described
Grinding point 3 stages, the 1st stage amount of water is the 3%-15% of dihedral silicon metal micropowder quality, and pressure is set to 0.3-0.6MPa,
Heating-up temperature is set to 40-80 DEG C, and milling time is set to 0.5-2.5h；2nd stage amount of water is dihedral silicon metal micropowder matter
The 1%-3% of amount, pressure is set to 0.2-0.5MPa, and heating-up temperature is constant, and milling time is set to 1-2.5h；3rd stage added water
Amount is the 1%-3% of dihedral silicon metal micropowder quality, and pressure is set to 0.1-0.4MPa, and heating-up temperature is constant, and milling time is arranged
For 0.5-2h；
(2) after grinding terminates, again regulating pressure, heating-up temperature and drying time, the silicon powder after grinding is dried；Dry
During Gan, pressure is set to 0 MPa, and heating-up temperature is set to 100-110 DEG C, and drying time is 1-3h.
(3) silicon powder after drying removes ferrum through screening machine screening with tramp iron separator, obtains fillet silicon metal micropowder.
The preparation method of fillet silicon metal micropowder of the present invention, its further preferred technical scheme is: step (1)
In, the 1st stage amount of water is the 6%-12% of dihedral silicon metal micropowder quality, and pressure is set to 0.4-0.5MPa, and heating-up temperature sets
Being set to 50-70 DEG C, milling time is set to 1-2h；2nd stage amount of water is the 1.5%-2.5% of dihedral silicon metal micropowder quality,
Pressure is set to 0.3-0.4MPa, and heating-up temperature is constant, and milling time is set to 1-2h；3rd stage amount of water is dihedral crystallization
The 1.5%-2.5% of silicon powder quality, pressure is set to 0.2-0.3MPa, and heating-up temperature is constant, and milling time is set to 0.8-
1.5h。
The preparation method of fillet silicon metal micropowder of the present invention, further preferably technical scheme is: step (1)
In, the 1st stage amount of water is the 10% of dihedral silicon metal micropowder quality, and pressure is set to 0.45MPa, and heating-up temperature is set to 60
DEG C, milling time is set to 1.5h；2nd stage amount of water is the 2% of dihedral silicon metal micropowder quality, and pressure is set to
0.35MPa, heating-up temperature is constant, and milling time is set to 1.5h；3rd stage amount of water is dihedral silicon metal micropowder quality
2%, pressure is set to 0.25MPa, and heating-up temperature is constant, and milling time is set to 1.2h.
The preparation method of fillet silicon metal micropowder of the present invention, its further preferred technical scheme is: step (2)
Described heating-up temperature is set to 102-108 DEG C, milling time 1.5-2.5h.
The preparation method of fillet silicon metal micropowder of the present invention, its further preferred technical scheme is: step (2)
Described heating-up temperature is set to 105 DEG C, milling time 2h.
Compared with prior art, the inventive method prepares fillet micropowder good fluidity, loading, thermal conductivity are high, technique
Be simple and convenient to operate, preparation process environmental protection.
Detailed description of the invention
The concrete technical scheme of the present invention described further below, in order to those skilled in the art is further understood that
The present invention, and do not constitute the restriction to its right.
Embodiment 1, the preparation method of a kind of fillet silicon metal micropowder, the method comprises the steps:
(1) D50 is joined in fillet processing equipment at the dihedral silicon metal micropowder of 10-60 μm, start equipment agitating function, limit
Stirring limit adds deionized water；Regulate pressure, heating-up temperature and milling time after adding deionized water, start to grind；Described
Grinding point 3 stages, the 1st stage amount of water is the 3% of dihedral silicon metal micropowder quality, and pressure is set to 0.3MPa, heating-up temperature
Being set to 40 DEG C, milling time is set to 0.5h；2nd stage amount of water is the 1% of dihedral silicon metal micropowder quality, and pressure is arranged
For 0.2MPa, heating-up temperature is constant, and milling time is set to 1h；3rd stage amount of water is the 1% of dihedral silicon metal micropowder quality,
Pressure is set to 0.1MPa, and heating-up temperature is constant, and milling time is set to 0.5h；
(2) after grinding terminates, again regulating pressure, heating-up temperature and drying time, the silicon powder after grinding is dried；Dry
During Gan, pressure is set to 0 MPa, and heating-up temperature is set to 100 DEG C, and drying time is 1h.
(3) silicon powder after drying removes ferrum through screening machine screening with tramp iron separator, obtains fillet silicon metal micropowder.
Embodiment 2, the preparation method of a kind of fillet silicon metal micropowder, the method comprises the steps:
(1) D50 is joined in fillet processing equipment at the dihedral silicon metal micropowder of 10-60 μm, start equipment agitating function, limit
Stirring limit adds deionized water；Regulate pressure, heating-up temperature and milling time after adding deionized water, start to grind；Described
Grinding point 3 stages, the 1st stage amount of water is the 15% of dihedral silicon metal micropowder quality, and pressure is set to 0.6MPa, heating temperature
Degree is set to 80 DEG C, and milling time is set to 2.5h；2nd stage amount of water is the 3% of dihedral silicon metal micropowder quality, and pressure sets
Being set to 0.5MPa, heating-up temperature is constant, and milling time is set to 2.5h；3rd stage amount of water is dihedral silicon metal micropowder quality
3%, pressure is set to 0.4MPa, and heating-up temperature is constant, and milling time is set to 2h；
(2) after grinding terminates, again regulating pressure, heating-up temperature and drying time, the silicon powder after grinding is dried；Dry
During Gan, pressure is set to 0 MPa, and heating-up temperature is set to 110 DEG C, and drying time is 3h.
(3) silicon powder after drying removes ferrum through screening machine screening with tramp iron separator, obtains fillet silicon metal micropowder.
Embodiment 3, the preparation method of a kind of fillet silicon metal micropowder, the method comprises the steps:
(1) D50 is joined in fillet processing equipment at the dihedral silicon metal micropowder of 10-60 μm, start equipment agitating function, limit
Stirring limit adds deionized water；Regulate pressure, heating-up temperature and milling time after adding deionized water, start to grind；1st stage
Amount of water is the 6% of dihedral silicon metal micropowder quality, and pressure is set to 0.4MPa, and heating-up temperature is set to 50 DEG C, and milling time sets
It is set to 1h；2nd stage amount of water is the 1.5% of dihedral silicon metal micropowder quality, and pressure is set to 0.3MPa, and heating-up temperature is constant,
Milling time is set to 1h；3rd stage amount of water is the 1.5% of dihedral silicon metal micropowder quality, and pressure is set to 0.2MPa, adds
Heat is temperature-resistant, and milling time is set to 0.8h.
(2) after grinding terminates, again regulating pressure, heating-up temperature and drying time, the silicon powder after grinding dries
Dry；In drying course, pressure is set to 0 MPa, and described heating-up temperature is set to 102 DEG C, drying time 1.5h.
(3) silicon powder after drying removes ferrum through screening machine screening with tramp iron separator, obtains fillet silicon metal micropowder.
Embodiment 4, the preparation method of a kind of fillet silicon metal micropowder, the method comprises the steps:
(1) D50 is joined in fillet processing equipment at the dihedral silicon metal micropowder of 10-60 μm, start equipment agitating function, limit
Stirring limit adds deionized water；Regulate pressure, heating-up temperature and milling time after adding deionized water, start to grind；1st stage
Amount of water is the 12% of dihedral silicon metal micropowder quality, and pressure is set to 0.5MPa, and heating-up temperature is set to 70 DEG C, milling time
It is set to 2h；2nd stage amount of water is the 2.5% of dihedral silicon metal micropowder quality, and pressure is set to 0.4MPa, and heating-up temperature is not
Becoming, milling time is set to 2h；3rd stage amount of water is the 2.5% of dihedral silicon metal micropowder quality, and pressure is set to 0.3MPa,
Heating-up temperature is constant, and milling time is set to 1.5h.
(2) after grinding terminates, again regulating pressure, heating-up temperature and drying time, the silicon powder after grinding dries
Dry；In drying course, pressure is set to 0 MPa, and described heating-up temperature is set to 108 DEG C, drying time 2.5h.
(3) silicon powder after drying removes ferrum through screening machine screening with tramp iron separator, obtains fillet silicon metal micropowder.
Embodiment 5, the preparation method of a kind of fillet silicon metal micropowder, the method comprises the steps:
(1) D50 is joined in fillet processing equipment at the dihedral silicon metal micropowder of 10-60 μm, start equipment agitating function, limit
Stirring limit adds deionized water；Regulate pressure, heating-up temperature and milling time after adding deionized water, start to grind；1st stage
Amount of water is the 10% of dihedral silicon metal micropowder quality, and pressure is set to 0.45MPa, and heating-up temperature is set to 60 DEG C, milling time
It is set to 1.5h；2nd stage amount of water is the 2% of dihedral silicon metal micropowder quality, and pressure is set to 0.35MPa, and heating-up temperature is not
Becoming, milling time is set to 1.5h；3rd stage amount of water is the 2% of dihedral silicon metal micropowder quality, and pressure is set to
0.25MPa, heating-up temperature is constant, and milling time is set to 1.2h.
(2) after grinding terminates, again regulating pressure, heating-up temperature and drying time, the silicon powder after grinding dries
Dry；In drying course, pressure is set to 0 MPa, and described heating-up temperature is set to 105 DEG C, milling time 2h.
(3) silicon powder after drying removes ferrum through screening machine screening with tramp iron separator, obtains fillet silicon metal micropowder.
Claims (5)
1. the preparation method of a fillet silicon metal micropowder, it is characterised in that the method comprises the steps:
(1) D50 is joined in fillet processing equipment at the dihedral silicon metal micropowder of 10-60 μm, start equipment agitating function, limit
Stirring limit adds deionized water；Regulate pressure, heating-up temperature and milling time after adding deionized water, start to grind；Described
Grinding point 3 stages, the 1st stage amount of water is the 3%-15% of dihedral silicon metal micropowder quality, and pressure is set to 0.3-0.6MPa,
Heating-up temperature is set to 40-80 DEG C, and milling time is set to 0.5-2.5h；2nd stage amount of water is dihedral silicon metal micropowder matter
The 1%-3% of amount, pressure is set to 0.2-0.5MPa, and heating-up temperature is constant, and milling time is set to 1-2.5h；3rd stage added water
Amount is the 1%-3% of dihedral silicon metal micropowder quality, and pressure is set to 0.1-0.4MPa, and heating-up temperature is constant, and milling time is arranged
For 0.5-2h；
(2) after grinding terminates, again regulating pressure, heating-up temperature and drying time, the silicon powder after grinding is dried；Dry
During Gan, pressure is set to 0 MPa, and heating-up temperature is set to 100-110 DEG C, and drying time is 1-3h；
(3) silicon powder after drying removes ferrum through screening machine screening with tramp iron separator, obtains fillet silicon metal micropowder.
Preparation method the most according to claim 1, it is characterised in that: in step (1), the 1st stage amount of water is dihedral knot
The 6%-12% of crystal silicon micropowder quality, pressure is set to 0.4-0.5MPa, and heating-up temperature is set to 50-70 DEG C, and milling time is arranged
For 1-2h；2nd stage amount of water is the 1.5%-2.5% of dihedral silicon metal micropowder quality, and pressure is set to 0.3-0.4MPa, heating
Temperature-resistant, milling time is set to 1-2h；3rd stage amount of water is the 1.5%-2.5% of dihedral silicon metal micropowder quality, pressure
Being set to 0.2-0.3MPa, heating-up temperature is constant, and milling time is set to 0.8-1.5h.
Preparation method the most according to claim 1, it is characterised in that: in step (1), the 1st stage amount of water is dihedral knot
The 10% of crystal silicon micropowder quality, pressure is set to 0.45MPa, and heating-up temperature is set to 60 DEG C, and milling time is set to 1.5h；2nd
Stage amount of water is the 2% of dihedral silicon metal micropowder quality, and pressure is set to 0.35MPa, and heating-up temperature is constant, and milling time sets
It is set to 1.5h；3rd stage amount of water is the 2% of dihedral silicon metal micropowder quality, and pressure is set to 0.25MPa, and heating-up temperature is not
Becoming, milling time is set to 1.2h.
Preparation method the most according to claim 1, it is characterised in that: the heating-up temperature described in step (2) is set to 102-
108 DEG C, milling time 1.5-2.5h.
Preparation method the most according to claim 1, it is characterised in that: the heating-up temperature described in step (2) is set to 105
DEG C, milling time 2h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003382A (en) * | 2017-12-28 | 2018-05-08 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order |
| CN111153631A (en) * | 2020-02-25 | 2020-05-15 | 长兴电子材料（昆山）有限公司 | High-thermal-conductivity and high-reliability epoxy resin composition and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130015806A (en) * | 2011-08-05 | 2013-02-14 | 전자부품연구원 | Manufacturing method of sio2 nano-particle |
| CN103466645A (en) * | 2013-09-27 | 2013-12-25 | 上海冠旗电子新材料股份有限公司 | Method for preparing nano-silica by wet grinding |
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2016
- 2016-07-29 CN CN201610610504.4A patent/CN106219561B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130015806A (en) * | 2011-08-05 | 2013-02-14 | 전자부품연구원 | Manufacturing method of sio2 nano-particle |
| CN103466645A (en) * | 2013-09-27 | 2013-12-25 | 上海冠旗电子新材料股份有限公司 | Method for preparing nano-silica by wet grinding |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003382A (en) * | 2017-12-28 | 2018-05-08 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order |
| CN111153631A (en) * | 2020-02-25 | 2020-05-15 | 长兴电子材料（昆山）有限公司 | High-thermal-conductivity and high-reliability epoxy resin composition and application thereof |
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