CN108003382A - A kind of preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order - Google Patents

A kind of preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order Download PDF

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Publication number
CN108003382A
CN108003382A CN201711454356.2A CN201711454356A CN108003382A CN 108003382 A CN108003382 A CN 108003382A CN 201711454356 A CN201711454356 A CN 201711454356A CN 108003382 A CN108003382 A CN 108003382A
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China
Prior art keywords
mpa
silicon powder
grinding
roller pressure
micron order
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CN201711454356.2A
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Chinese (zh)
Inventor
吕福发
王松宪
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JIANGSU LIANRUI NEW MATERIAL Co Ltd
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JIANGSU LIANRUI NEW MATERIAL Co Ltd
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Priority to CN201711454356.2A priority Critical patent/CN108003382A/en
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
    • C09C1/3018—Grinding
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

Abstract

The present invention is a kind of preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order, its step is as follows:High purity crystalline type fine silica powder is added in grinder and is ground three times, roller pressure is set for the first time as the Mpa of 1.0 Mpa~1.5, second set roller pressure set roller pressure as 0.3Mpa for the Mpa of 0.5 Mpa~1.0, grinding third time, three times the obtained component A of discharging after grinding；Component A is delivered to cyclone separator by air-flow and removes fine powder, obtained silicon powder cleans by screening, up to product.The present invention carries out sphericalization using secondary granulation to powdered quartz micro mist, so as to lift powdered quartz filling rate, improves electronic component thermal conductivity, while improve the reliability of electronic component.In addition preparation method generation processing step provided by the invention is simple, product quality is controllable, is produced suitable for industrialization.

Description

A kind of preparation of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order Method
Technical field
The present invention relates to a kind of preparation method of silicon powder, particularly a kind of high-power total incapsulation transistor micron order class The preparation method of spheroidal crystal silicon powder.
Background technology
With developing rapidly for 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 its property There can be very important influence on the performance of epoxy molding plastic, it is micro- that the filler of epoxy molding plastic is most importantly silica Powder.Although silicon powder has different classification, they have the characteristics of common, are to improvement EMC certain as filling Kind parameter and characteristic, such as：Can reduce contraction, increase intensity, enhancing wearability, improve thermal distorsion temperature, improve thermal conductivity, Reduce thermal coefficient of expansion, reduce cost, etc..They have general character, similarly there are individual character, powdered quartz micro mist 12.6 W/K.m of pyroconductivity, is a kind of electronics packing material, but because powdered quartz micro powder granule shape is more well Low for irregular shape filling rate, thermal conduction effect is had a greatly reduced quality.Preparing spherical SiO 2 micro mist has filling rate height, but spherical Fine silica powder is fusion, poor thermal conductivity, allows powdered quartz micro mist sphericalization, you can improves filling rate and again may be used To ensure that pyroconductivity is preferred plan, electronics integrates, electronic component power increases, electronic component generates heat etc. can be solved Problem.
The content of the invention
The technical problems to be solved by the invention are in view of the deficiencies of the prior art, there is provided one kind lifting crystal type titanium dioxide Silicon filling rate, improves electronic component thermal conductivity, while improves the high-power total incapsulation transistor of the reliability of electronic component With the preparation method of the spherical crystallization silicon powder of micron order.
The technical problems to be solved by the invention are realized by following technical solution, and the present invention is a kind of big work( The preparation method of the spherical crystallization silicon powder of rate total incapsulation transistor micron order, its main feature is that, its step is as follows:
(1) raw material prepares：High purity crystalline type fine silica powder, SiO2Content >=99.8%, Fe2O3≤ 0.015%, Cl ions ≤ 5ppm, Na ions≤5ppm, pH value 5~7, granularity requirements：≤ 100 mesh；
(2) grinding is granulated：
High purity crystalline type fine silica powder is added in grinder and is ground three times, sets roller pressure as 1.0 for the first time The Mpa of Mpa~1.5, grinds 0.5h~1h；Second set roller pressure as 0.5 Mpa~1.0 Mpa, grinding 0.5h~1h； Third time sets roller pressure as 0.3Mpa, grinds 0.5h~1h；By the shearing force that is produced between high pressing roller and raw material not Disconnected grinding removes particle wedge angle and reaches sphericalization, discharges after grinding three times and component A is made；
It is as follows to produce technological parameter：
(3) filtering is collected in shaping：
By component A with 8500 ± 500M3/ h absorbing quantities are delivered to the fine powder of less than 3 microns of cyclone separator removal by air-flow, Obtained silicon powder cleans by vibrating screen screening with magnetic separator, that is, obtains the spherical crystallization silicon powder of micron order.
Less than 3 microns of fine powder is the tip-angled shape particle ground, because fine powder specific surface area is big, absorbs resin It is more, used in encapsulation system as filler when viscosity it is big, therefore be not suitable for use.
In the preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order of the present invention, step Suddenly（2）In, set roller pressure for the first time as the Mpa of 1.2 Mpa~1.4, grinding 0.6h~0.8h；Second of setting roller pressure Power is the Mpa of 0.6 Mpa~0.8, grinds 0.6h~0.8h；Third time sets roller pressure as 0.3Mpa, and grinding 0.5h~ 0.6h。
In the preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order of the present invention, step Suddenly（3）Middle silicon powder is sieved by 100 mesh vibrating screens, by 10000Gs magnetic separators, removes metal impurities.
In the preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order of the present invention, step Suddenly（2）In, high purity crystalline type fine silica powder addition is 500kg~1000kg.
Compared with prior art, the present invention carries out sphericalization using secondary granulation to powdered quartz micro mist, from And powdered quartz filling rate is lifted, improve electronic component thermal conductivity, while improve the reliability of electronic component.Separately Outer preparation method generation processing step provided by the invention is simple, product quality is controllable, is produced suitable for industrialization.
Embodiment
Concrete technical scheme of the invention described further below, in order to which those skilled in the art is further understood that The present invention, without forming the limitation to its right.
Embodiment 1, a kind of preparation method of the high-power spherical crystallization silicon powder of total incapsulation transistor micron order, it is walked It is rapid as follows：
(1) raw material prepares：High purity crystalline type fine silica powder, SiO2Content >=99.8%, Fe2O3≤ 0.015%, Cl ions ≤ 5ppm, Na ions≤5ppm, pH value 5~7, granularity requirements：≤ 100 mesh；
(2) grinding is granulated：
High purity crystalline type fine silica powder 500kg is added in grinder and is ground three times, sets roller pressure for the first time For 1.0 Mpa, 0.5h is ground；Roller pressure is set as 1.0 Mpa for the second time, grinds 1h；Third time set roller pressure as 0.3Mpa, grinds 0.5h；Removal particle wedge angle is constantly ground by the shearing force produced between high pressing roller and raw material and reaches class Spheroidization, discharges after grinding three times and component A is made；
(3) filtering is collected in shaping：
By component A with 8500 ± 500M3/ h absorbing quantities are delivered to the fine powder of less than 3 microns of cyclone separator removal by air-flow, Fine powder is the tip-angled shape particle ground, and obtained silicon powder passes through 100 mesh vibrating screens again, by 10000Gs magnetic separators, Metal impurities are removed, that is, obtain the spherical crystallization silicon powder of micron order.
Embodiment 2, a kind of preparation method of the high-power spherical crystallization silicon powder of total incapsulation transistor micron order, it is walked It is rapid as follows：
(1) raw material prepares：High purity crystalline type fine silica powder, SiO2Content >=99.8%, Fe2O3≤ 0.015%, Cl ions ≤ 5ppm, Na ions≤5ppm, pH value 5~7, granularity requirements：≤ 100 mesh；
(2) grinding is granulated：
High purity crystalline type fine silica powder 1000kg is added in grinder and is ground three times, sets roller pressure for the first time For 1.5 Mpa, 1h is ground；Roller pressure is set as 1.5 Mpa for the second time, grinds 0.5h；Third time set roller pressure as 0.3Mpa, grinds 1h；Removal particle wedge angle is constantly ground by the shearing force produced between high pressing roller and raw material and reaches class ball Shape, discharges after grinding three times and component A is made；
(3) filtering is collected in shaping：
By component A with 8500 ± 500M3/ h absorbing quantities are delivered to the fine powder of less than 3 microns of cyclone separator removal by air-flow, Fine powder is the tip-angled shape particle ground, and obtained silicon powder passes through 100 mesh vibrating screens again, by 10000Gs magnetic separators, Metal impurities are removed, that is, obtain the spherical crystallization silicon powder of micron order.
Embodiment 3, a kind of preparation method of the high-power spherical crystallization silicon powder of total incapsulation transistor micron order, it is walked It is rapid as follows：
(1) raw material prepares：High purity crystalline type fine silica powder, SiO2Content >=99.8%, Fe2O3≤ 0.015%, Cl ions ≤ 5ppm, Na ions≤5ppm, pH value 5~7, granularity requirements：≤ 100 mesh；
(2) grinding is granulated：
High purity crystalline type fine silica powder 800kg is added in grinder and is ground three times, sets roller pressure for the first time For 1.2 Mpa, 0.8h is ground；Roller pressure is set as 1.2 Mpa for the second time, grinds 0.6h；Third time set roller pressure as 0.3Mpa, grinds 0.7h；Removal particle wedge angle is constantly ground by the shearing force produced between high pressing roller and raw material and reaches class Spheroidization, discharges after grinding three times and component A is made；
(3) filtering is collected in shaping：
By component A with 8500 ± 500M3/ h absorbing quantities are delivered to the fine powder of less than 3 microns of cyclone separator removal by air-flow, Fine powder is the tip-angled shape particle ground, and obtained silicon powder passes through 100 mesh vibrating screens again, by 10000Gs magnetic separators, Metal impurities are removed, that is, obtain the spherical crystallization silicon powder of micron order.
Product made from embodiment 1 is detected and is detected with application performance, it is as a result as follows：
Product testing：
Application performance：
From the point of view of the result of experiment, spherical crystallization silicon powder is showed than the product of angle-style crystallization silicon powder in EMC performances It is more excellent, it is mainly reflected in filling rate height, length of flow length.
Conclusion：
The product is shown good by detecting and testing in the application process of high-power total incapsulation transistor epoxy molding plastic Mobility, also do very well in terms of flash.Especially protruded because height is filled in highly thermally conductive aspect of performance performance.

Claims (4)

  1. A kind of 1. preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order, it is characterised in that its Step is as follows：
    (1) raw material prepares：High purity crystalline type fine silica powder, SiO2Content >=99.8%, Fe2O3≤ 0.015%, Cl ions ≤ 5ppm, Na ions≤5ppm, pH value 5~7, granularity requirements：≤ 100 mesh；
    (2) grinding is granulated：
    High purity crystalline type fine silica powder is added in grinder and is ground three times, sets roller pressure as 1.0 for the first time The Mpa of Mpa~1.5, grinds 0.5h~1h；Second set roller pressure as 0.5 Mpa~1.0 Mpa, grinding 0.5h~1h； Third time sets roller pressure as 0.3Mpa, grinds 0.5h~1h；By the shearing force that is produced between high pressing roller and raw material not Disconnected grinding removes particle wedge angle and reaches sphericalization, discharges after grinding three times and component A is made；
    (3) filtering is collected in shaping：
    By component A with 8500 ± 500M3/ h absorbing quantities are delivered to the fine powder of less than 3 microns of cyclone separator removal by air-flow, obtain The silicon powder arrived cleans by vibrating screen screening with magnetic separator, that is, obtains the spherical crystallization silicon powder of micron order.
  2. 2. the preparation side of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order according to claim 1 Method, it is characterised in that：Step（2）In, set roller pressure for the first time as the Mpa of 1.2 Mpa~1.4, grinding 0.6h~0.8h； Second set roller pressure as 0.6 Mpa~0.8 Mpa, grinding 0.6h~0.8h；Third time set roller pressure as 0.3Mpa, grinds 0.5h~0.6h.
  3. 3. the preparation side of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order according to claim 1 Method, it is characterised in that：Step（3）Middle silicon powder is sieved by 100 mesh vibrating screens, and by 10000Gs magnetic separators, it is miscellaneous to remove metal Matter.
  4. 4. the preparation side of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order according to claim 1 Method, it is characterised in that：Step（2）In, high purity crystalline type fine silica powder addition is 500kg~1000kg.
CN201711454356.2A 2017-12-28 2017-12-28 A kind of preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order Pending CN108003382A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109135346A (en) * 2018-09-05 2019-01-04 中建材蚌埠玻璃工业设计研究院有限公司 Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof
CN111073350A (en) * 2019-12-25 2020-04-28 中建材蚌埠玻璃工业设计研究院有限公司 Preparation method of submicron active silica micropowder

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CN103627215A (en) * 2013-11-27 2014-03-12 连云港东海硅微粉有限责任公司 Preparation method of submicron silica powder
CN106219561A (en) * 2016-07-29 2016-12-14 江苏联瑞新材料股份有限公司 A kind of preparation method of fillet silicon metal micropowder
CN106939130A (en) * 2016-01-03 2017-07-11 新沂市宏润石英硅微粉有限公司 A kind of production method for crystallizing silicon powder

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Publication number Priority date Publication date Assignee Title
CN101733685A (en) * 2009-12-10 2010-06-16 洛阳轴研科技股份有限公司 Processing technique for ceramic balls
CN103627215A (en) * 2013-11-27 2014-03-12 连云港东海硅微粉有限责任公司 Preparation method of submicron silica powder
CN106939130A (en) * 2016-01-03 2017-07-11 新沂市宏润石英硅微粉有限公司 A kind of production method for crystallizing silicon powder
CN106219561A (en) * 2016-07-29 2016-12-14 江苏联瑞新材料股份有限公司 A kind of preparation method of fillet silicon metal micropowder

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109135346A (en) * 2018-09-05 2019-01-04 中建材蚌埠玻璃工业设计研究院有限公司 Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof
CN111073350A (en) * 2019-12-25 2020-04-28 中建材蚌埠玻璃工业设计研究院有限公司 Preparation method of submicron active silica micropowder

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Application publication date: 20180508