CN107827117A - A kind of preparation method of more peak shape distribution spherical fine silica powders - Google Patents
A kind of preparation method of more peak shape distribution spherical fine silica powders Download PDFInfo
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- CN107827117A CN107827117A CN201711176711.4A CN201711176711A CN107827117A CN 107827117 A CN107827117 A CN 107827117A CN 201711176711 A CN201711176711 A CN 201711176711A CN 107827117 A CN107827117 A CN 107827117A
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- 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
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- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The present invention is a kind of preparation method of more peak shape distribution spherical fine silica powders：It is more than 99.8% from purity, granularity is that 0.1 μm 60 μm of fine silica powder is raw material；The flame zone formed in balling furnace using natural gas and oxygen combustion is passed into spheroidized area nodularization as spheroidized area, by raw material and product A, product B, products C and product D is made；By product A and product B according to mass ratio 0.1 ~ 1：1, mixed by high efficient mixer, the product after being well mixed is designated as product AB；Product AB and products C and product D are mixed in mixer, 10 ~ 50min of incorporation time, and product is produced after well mixed.Preparing spherical SiO 2 micro mist prepared by this method at least contain three peaks, show filler the good fluidity of plastic packaging material product, loading greatly, low thermal coefficient of expansion and the features such as low warpage.
Description
Technical field
The present invention relates to a kind of preparation method of preparing spherical SiO 2 micro mist, particularly a kind of more peak shape distribution spherical dioxies
The preparation method of SiClx micro mist.
Background technology
Semicon industry in order to meet present consumer it is light to end product, it is small, thin etc. require, weight occurs for its packing forms
Big change, from packing forms such as leaded DIP, SIP, develop into the encapsulation shape such as surface-adhered type SOP, TSOP, SSOP and QFP
Formula, it is in progress now towards packing forms such as underfill.
Wherein, main flows of the SOP and QFP as middle and high-end market, it is competing under conditions of packaging technology and market reach its maturity
It is also increasingly fierce to strive, and on the one hand properties of product is proposed with higher requirement, a Key Performance Indicator is epoxy-plastic packaging among these
The Spiral flow of material, in general, the longer the better for Spiral flow.This performance indications and filler（Silicon powder）Close phase
Close, it may be said that suitable filler plays a decisive role to the mobility of epoxy-plastic packaging material.In order to meet these requirements, first, to filler
Carry out spheroidization, there is provided the loading and mobility of filler, second, preparing more peak shape distribution fillers.On the other hand, it is inexpensive
It is the key factor into market.Under the requirement of these conditions, prepare one kind and be used in middle and high end semiconductor packages low cost
High performance spherical fine silica powder product.
The A of patent No. CN 101743198, applicant Deuki Kagaku Kogyo Co., Ltd are utilized in fine silica powder raw material
It is middle to increase silicon metal powder to prepare more peak shape preparing spherical SiO 2s, the place of this preparation process Shortcomings.First, nodularization
Process because furnace temperature temperature is too high, easily reunite by micropowders（The patent No.：Unexamined Patent 2-296711, spherical silicon microparticle and its
Preparation method, when illustrating more than 1300 DEG C, nodularization process is easily melted, and causes to reunite, it is difficult to obtains ultra micro ball powder）, production technology control
Difficulty processed is big；Second, the content for the ultra tiny ball powder that different product needs is different, product can not be adjusted accurately after causing nodularization, no
The product of different demands can be prepared；Third, silicon metal powder has potential safety hazard, security incident is easily caused；Fourth, metallic silicon is
Conductive material, technology controlling and process is inaccurate, is easily accessible in product, causes downstream product electrical property to fail.
The B applicant Wuxi Chuangda Electronic Co., Ltd. of patent No. CN 103665775 is micro- using the spherical silicon of different-grain diameter
Powder, crystallization silicon powder, the melting gentle aerosil of silicon powder are prepared compared with high filler loading capacity to prepare more peak shape fillers, mobility compared with
Good plastic packaging material.Deficiency place be add aerosil because specific surface area is big, oil absorbency improve, cause plastic packaging material to glue
Degree sharply increases, it is impossible to is used in the encapsulating products such as SOP.
The A applicant Jiangsu Lian Rui new materials limited companies of patent No. CN 104194274 utilize two kinds of raw materials two
Secondary grinding prepares bimodal shape horn shape silicon powder, and the product for making to produce in this way is unable to reach peak value occurs at 0-1 μm.Can not
Meet the requirement of the encapsulating products such as SOP.
The content of the invention
The technical problems to be solved by the invention are the problem of presence for prior art, there is provided a kind of good fluidity, low
The preparation method of thermal coefficient of expansion and the preparing spherical SiO 2 micro mist of low warpage.
The technical problems to be solved by the invention are realized by following technical scheme, and the present invention is a kind of multimodal
The preparation method of shape distribution spherical fine silica powder, is characterized in：Its step is as follows：
（1）Raw material：It is more than 99.8% from purity, the fine silica powder that granularity is 0.1 μm -60 μm is raw material；
（2）Raw material is passed into spheroidized area ball by the flame zone formed in balling furnace using natural gas and oxygen combustion as spheroidized area
Change and be made：- 0.5 μm of D50=0.1 μm product A, -3.0 μm of D50=0.6 μm product B, D50=4 μm of -14 μm of products Cs and D50=15 μm -
60 μm of product D；
（3）By product A and product B according to mass ratio 0.1 ~ 1：1, mixed by high efficient mixer, incorporation time 3min
- 30min, the product after being well mixed are designated as product AB；
（4）Product AB and products C and product D are according to mass ratio 0.05-0.30：0.11-0.24：0.66-1.08 enters in mixer
Row mixing, 10 ~ 50min of incorporation time, product is produced after well mixed.
In the preparation method of more peak shape distribution spherical fine silica powders of the present invention：Above-mentioned high efficient mixer is gas
Streaming mixer or intensive mixer or planetary mixer or homogenizer.
In the preparation method of more peak shape distribution spherical fine silica powders of the present invention：The high efficient mixer is gas
During streaming mixer, compressed air pressure is in 0.3Mpa -2.0Mpa, load factor 0.3-0.5.
In the preparation method of more peak shape distribution spherical fine silica powders of the present invention：Described mixer is two dimension
Mixer, three-dimensional mixer, V-Mixer, bipyramid-type mixer, Agravicmixer, cone-type mixer or plough coulter type mixing
Machine.
In the preparation method of more peak shape distribution spherical fine silica powders of the present invention：Day described in the balling furnace
The dosage of right gas uses 0.5 m for per kilogram silicon powder3-2.5m3。
D50 refers to corresponding particle diameter when certain powder cumulative volume fraction is 50%.
Compared with prior art, the inventive method is simple, the product of different-grain diameter is made using the nodularization of flame spherical container shaping method, no
Product with particle diameter at least contains three peaks, table by being mixed to prepare this product, preparing spherical SiO 2 micro mist prepared by this method
Reveal filler in the good fluidity of plastic packaging material product, loading is big, low thermal coefficient of expansion and the features such as low warpage.
Brief description of the drawings
Fig. 1 is Granularity Distribution figure made from embodiment 4.
Fig. 2 is Granularity Distribution figure made from embodiment 5.
Fig. 3 is Granularity Distribution figure made from comparative example 1.
Fig. 4 is Granularity Distribution figure made from comparative example 2.
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 more peak shape distribution spherical fine silica powders, its step are as follows：
（1）Raw material：It is more than 99.8% from purity, the fine silica powder that granularity is 0.1 μm -60 μm is raw material；
（2）Raw material is passed into spheroidized area ball by the flame zone formed in balling furnace using natural gas and oxygen combustion as spheroidized area
Change and be made：- 0.5 μm of D50=0.1 μm product A, -3.0 μm of D50=0.6 μm product B, D50=4 μm of -14 μm of products Cs and D50=15 μm -
60 μm of product D；
（3）By product A and product B according to mass ratio 0.1 ~ 1：1, mixed by airflow mixer, incorporation time is
3min -30min, the compressed air pressure of airflow mixer are mixed in 0.3 Mpa -2.0Mpa, load factor 0.3-0.5
Product after closing uniformly is designated as product AB；
（4）Product AB and products C and product D are according to mass ratio 0.05-0.30：0.11-0.24：0.66-1.08 enters in mixer
Row mixing, 10 ~ 50min of incorporation time, product is produced after well mixed.
Embodiment 2, it is described mixed according in a kind of preparation method of more peak shape distribution spherical fine silica powders of embodiment 1
Conjunction machine be two-dimensional mixing machine, three-dimensional mixer, V-Mixer, bipyramid-type mixer, Agravicmixer, cone-type mixer or
Coulter type mixer.
Embodiment 3, according in a kind of preparation method of more peak shape distribution spherical fine silica powders of embodiment 1, the ball
The dosage for changing natural gas described in stove uses 0.5 m for per kilogram silicon powder3-2.5m3。
Embodiment 4, a kind of preparation method of more peak shape distribution spherical fine silica powders, it is more than 99.8% from purity,
The fine silica powder that granularity is 0.1 μm -60 μm is raw material；The flame zone formed in balling furnace with natural gas and oxygen combustion
For spheroidized area, raw material is passed into spheroidized area and is made by different spheroidizing process nodularizations：- 0.5 μm of D50=0.1 μm product A,
- 3.0 μm of D50=0.6 μm product B, D50=4 μm of -14 μm of products Cs and -60 μm of D50=15 μm product D；
Product A and product B is according to quality proportioning 0.2：1,10min, the sky of airflow mixer are mixed in airflow mixer
Atmospheric pressure is 1.2Mpa, load factor 0.4, and the product mixed is designated as product AB.Product AB, products C, product D are pressed into matter
Measure ratio 0.10:0.20:Mixed 15 minutes in 0.87 input two-dimensional mixing machine, the rotating speed of two-dimensional mixing machine is 12rpm, that is, production is made
Product.Particle size distribution figure refer to the attached drawing 1.Multimodal form is presented in this size distribution（Containing 4 peak values）.
Embodiment 5, a kind of preparation method of more peak shape distribution spherical fine silica powders, it is more than 99.8% from purity,
The fine silica powder that granularity is 0.1 μm -60 μm is raw material；The flame zone formed in balling furnace with natural gas and oxygen combustion
For spheroidized area, raw material is passed into spheroidized area and is made by different spheroidizing process nodularizations：- 0.5 μm of D50=0.1 μm product A,
- 3.0 μm of D50=0.6 μm product B, D50=4 μm of -14 μm of products Cs and -60 μm of D50=15 μm product D；
Product A and product B is according to quality proportioning 0.8：1,10min, the sky of airflow mixer are mixed in airflow mixer
Atmospheric pressure is 1.9Mpa, load factor 0.35, and the product mixed is designated as product AB.Product AB, products C, product D are pressed into matter
Measure ratio 0.08:0.23:Mixed 15 minutes in 0.72 input two-dimensional mixing machine, the rotating speed of two-dimensional mixing machine is 12rpm, that is, production is made
Product.Size distribution refer to the attached drawing 2, this size distribution equally contain 4 peak values.
Comparative example 1：
Product B and product D is made using the method for embodiment 4 or 5, by product B and product D in mass ratio 0.10:0.90, input
Being mixed 15 minutes in two-dimensional mixing machine, the rotating speed of mixer is 12rpm, and product is made, shown in Granularity Distribution figure accompanying drawing 3,
Bi-modal is presented in this size distribution.
Comparative example 2：
It is finished product that product D, product D, which is made, using the method for embodiment 4 or 5, this shown in Granularity Distribution figure accompanying drawing 4
Granularity Distribution only has a peak.
Granularity Distribution is detected using Beckman particle size analyzers.
Comparative example 1, comparative example 2 and embodiment 4 and the properties of product such as following table of embodiment 5：
α 1, α 2 are thermal coefficient of expansions.
From the point of view of data above, the general performance of embodiment 5 is best.That is more peak shape distribution spherical silica are micro-
Powder is than unimodal shape（Comparative example 2）（Or bimodal shape, comparative example 1）Performance it is more excellent, be mainly reflected in mobility length, loading
Greatly, linear expansion coefficient is small and the features such as high intensity.
Claims (5)
1. a kind of preparation method of more peak shape distribution spherical fine silica powders, it is characterised in that its step is as follows：
Raw material：It is more than 99.8% from purity, the fine silica powder that granularity is 0.1 μm -60 μm is raw material；
Raw material is passed into spheroidized area nodularization system by the flame zone formed in balling furnace using natural gas and oxygen combustion as spheroidized area
：- 0.5 μm of D50=0.1 μm product A, -3.0 μm of D50=0.6 μm product B, D50=4 μm of -14 μm of products Cs and -60 μm of D50=15 μm
Product D；
By product A and product B according to mass ratio 0.1 ~ 1：1, mixed by high efficient mixer, incorporation time be 3min-
30min, the product after being well mixed are designated as product AB；
Product AB and products C and product D are according to mass ratio 0.05-0.30：0.11-0.24：0.66-1.08 is mixed in mixer
Close, 10 ~ 50min of incorporation time, product is produced after well mixed.
2. preparation method according to claim 1, it is characterised in that：Step（3）In, the high efficient mixer is air-flowing type
Mixer or intensive mixer or planetary mixer or homogenizer.
3. preparation method according to claim 2, it is characterised in that：When high efficient mixer is airflow mixer, compression
Air pressure is in 0.3 Mpa -2.0Mpa, load factor 0.3-0.5.
4. preparation method according to claim 1, it is characterised in that：Step（4）In, described mixer mixes for two dimension
Machine, three-dimensional mixer, V-Mixer, bipyramid-type mixer, Agravicmixer, cone-type mixer or coulter type mixer.
5. preparation method according to claim 1, it is characterised in that：Step（2）In, natural gas described in the balling furnace
Dosage use 0.5 m for per kilogram silicon powder3-2.5m3。
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455726A (en) * | 2018-12-14 | 2019-03-12 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of ball-shaped silicon micro powder used for electronic packaging |
| CN109456620A (en) * | 2018-11-19 | 2019-03-12 | 江苏联瑞新材料股份有限公司 | A kind of low viscosity filler composition and preparation method thereof |
| WO2020019372A1 (en) * | 2018-07-27 | 2020-01-30 | 湖州五爻硅基材料研究院有限公司 | Preparation method for spherical powder filler, spherical powder filler obtained thereby and application thereof |
| CN112607756A (en) * | 2020-11-25 | 2021-04-06 | 江苏联瑞新材料股份有限公司 | Preparation method of spherical alumina for epoxy molding and packaging material |
| CN112978740A (en) * | 2021-03-23 | 2021-06-18 | 江苏联瑞新材料股份有限公司 | Preparation method of submicron spherical silicon dioxide micropowder |
| CN113308229A (en) * | 2021-05-21 | 2021-08-27 | 江苏联瑞新材料股份有限公司 | Preparation method of high-thermal-conductivity spherical powder for ball grid array packaging |
| CN113735149A (en) * | 2021-09-17 | 2021-12-03 | 江苏联瑞新材料股份有限公司 | Preparation method of spherical alumina powder for high-thermal-conductivity underfill |
| CN113881232A (en) * | 2021-11-04 | 2022-01-04 | 广东航迈新材料科技有限公司 | Ceramic organic silica gel material for medium-voltage fire-resistant cable and preparation method thereof |
| CN113929122A (en) * | 2021-11-12 | 2022-01-14 | 联瑞新材(连云港)有限公司 | Preparation method of multimodal distribution high heat conduction alpha phase spherical alumina |
| CN115368754A (en) * | 2022-08-12 | 2022-11-22 | 吉安豫顺新材料有限公司 | Spherical low-density silica filler |
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| CN105384177A (en) * | 2015-11-27 | 2016-03-09 | 江苏联瑞新材料股份有限公司 | Preparing method of submicrometer spherical silicon dioxide micropowder |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020019372A1 (en) * | 2018-07-27 | 2020-01-30 | 湖州五爻硅基材料研究院有限公司 | Preparation method for spherical powder filler, spherical powder filler obtained thereby and application thereof |
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| CN113881232A (en) * | 2021-11-04 | 2022-01-04 | 广东航迈新材料科技有限公司 | Ceramic organic silica gel material for medium-voltage fire-resistant cable and preparation method thereof |
| CN113929122A (en) * | 2021-11-12 | 2022-01-14 | 联瑞新材(连云港)有限公司 | Preparation method of multimodal distribution high heat conduction alpha phase spherical alumina |
| CN113929122B (en) * | 2021-11-12 | 2023-09-05 | 联瑞新材(连云港)有限公司 | Preparation method of multimodal distributed high-heat-conductivity alpha-phase spherical alumina |
| CN115368754A (en) * | 2022-08-12 | 2022-11-22 | 吉安豫顺新材料有限公司 | Spherical low-density silica filler |
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