JP7002519B2 - How to prepare spherical silicon fine powder for electronic packaging - Google Patents
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- 239000000843 powder Substances 0.000 title claims description 97
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 95
- 229910052710 silicon Inorganic materials 0.000 title claims description 95
- 239000010703 silicon Substances 0.000 title claims description 95
- 238000004100 electronic packaging Methods 0.000 title claims description 24
- 239000002245 particle Substances 0.000 claims description 49
- 239000011362 coarse particle Substances 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 30
- 239000010419 fine particle Substances 0.000 claims description 15
- 238000007873 sieving Methods 0.000 claims description 10
- 238000013329 compounding Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 238000009472 formulation Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 238000004806 packaging method and process Methods 0.000 description 10
- 238000009826 distribution Methods 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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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
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- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
- H01L21/563—Encapsulation of active face of flip-chip device, e.g. underfilling or underencapsulation of flip-chip, encapsulation preform on chip or mounting substrate
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- 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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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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Description
本発明は無機非金属材料の精密加工の技術分野に属し、特に電子パッケージング用の球状シリコン微粉末の調製方法に関する。 The present invention belongs to the technical field of precision processing of inorganic non-metal materials, and particularly relates to a method for preparing spherical silicon fine powder for electronic packaging.
マイクロエレクトロニクス産業の軽量化、Ｉ／Ｏポート数の増加、小型化、及び機能の多様化において発展している傾向に伴って、従来のワイヤボンディング相互接続技術は、高密度の要件を満たすことができず、製品のパッケージング要件を満たすために、多くの製品は、フリップチップパッケージング技術を施す必要がある。フリップチップパッケージングでは、毛管作用によりアンダーフィルをチップと基板との間の隙間に充填するため、アンダーフィルの重要な組成部として、球状シリコン微粉末の品質は、製品の充填効果に大きく影響する。チップと基板との間の隙間は非常に小さいため、パッケージング中に充填材の大粒子サイズ及び量に対していずれも厳しい要件を提案し、粗大粒子では、パッケージング中に接着剤注入口を塞ぐか又はパッケージング不良を回避し、パッケージングのスムーズな行いを保証するために、非常に低いレベルで制御する必要がある。 With the evolving trends in the microelectronics industry in weight reduction, increasing number of I / O ports, miniaturization, and diversification of functions, traditional wire bonding interconnect technologies can meet high density requirements. In order to meet the product packaging requirements, many products need to be flip-chip packaging technology. In flip-chip packaging, the underfill is filled in the gap between the chip and the substrate by capillary action, so the quality of spherical silicon fine powder has a great influence on the filling effect of the product as an important composition part of the underfill. .. Since the gap between the chip and the substrate is very small, we propose strict requirements for the size and amount of large particles of the filler during packaging, and for coarse particles, the adhesive inlet is provided during packaging. It needs to be controlled at a very low level to avoid blockages or packaging defects and to ensure smooth packaging.
材料充填中に、粗大粒子は、効果的に制御されることに加えて、パッケージング効果を改善する目的を達成するために、アンダーフィルがさらに低粘度、高流動性、優れたフラッシュ特性などの利点を有する必要がある。これらの性能の要件を満たすために、異なる粒度分布の球状シリコン微粉末は、合理的な粒度配合によって粘度を下げ、流動性を向上させ、フラッシュバリの発生を削減することができる。 During material filling, the coarse particles are effectively controlled, and in addition, the underfill has lower viscosity, higher fluidity, better flash properties, etc. to achieve the purpose of improving the packaging effect. You need to have an advantage. To meet these performance requirements, spherical silicon fine powders with different particle size distributions can reduce viscosity, improve fluidity and reduce the occurrence of flash burrs with rational particle size formulations.
特許文献１に記載の超音波湿式スクリーニング装置は、粒径が７５～１００μｍ以下である粒子の粒度分級プロセスの難しさを大幅に軽減するが、篩い分け後の製品における粗大粒子の制御レベルを詳しく分析せず、電子パッケージング技術の発展に伴い、粗大粒子の制御レベルは非常に重要な評価指標になり、より厳しいレベルに制御するために新しい方法を開発する必要がある。また、単一の気流分級、篩い分けなどの粗い分級プロセスによる、球状シリコン微粉末における粗大粒子に対する除去する効果は、製品の技術要件を満たすことができず、且つ、篩い分けプロセスでは、スクリーン開口が小さい場合、スムーズな篩い分けを実現しにくい。 The ultrasonic wet screening apparatus described in Patent Document 1 greatly reduces the difficulty of the particle size classification process for particles having a particle size of 75 to 100 μm or less, but details the control level of coarse particles in the product after sieving. Without analysis, with the development of electronic packaging technology, the control level of coarse particles has become a very important evaluation index, and new methods need to be developed to control to a stricter level. In addition, the effect of removing coarse particles in spherical silicon fine powder by a coarse classification process such as single airflow classification and sieving cannot meet the technical requirements of the product, and the screen opening in the sieving process. If is small, it is difficult to achieve smooth sieving.
本発明が解決しようとする技術的課題は、従来技術の欠陥に対して、設計が合理的で、粗大粒子を効果的に制御し、低粘度、高流動性であり、使用しやすい、電子パッケージング用の球状シリコン微粉末の調製方法を提供することである。 The technical problem to be solved by the present invention is that the design is rational for the defects of the prior art, the coarse particles are effectively controlled, the viscosity is low, the fluidity is high, and the electronic package is easy to use. It is an object of the present invention to provide a method for preparing a spherical silicon fine powder for an exfoliation.
本発明が解決しようとする技術的課題は、
（１）篩い分けようとする球状シリコン微粉末を粗い分級装置に入れて粗い分級を行い、粒度がＴｏｐ ｃｕｔ５５μｍ以上である粗粒度製品Ａと粒度がそれ以外の細粒度製品Ｂとを得る粗い分級ステップと、
（２）ステップ（１）で得られた細粒度製品Ｂを精密分級装置に入れて精密分級を行い、粗大粒子の数が低減された球状シリコン微粉末製品Ｃを得る精密分級ステップと、
（３）ステップ（２）で得られた球状シリコン微粉末製品Ｃを、気流分散下でミキサーに入れ、ステップ（１）で得られた粗粒度製品Ａの球状シリコン微粉末と混合させて粒度配合を行うことで、電子パッケージング用の球状シリコン微粉末を得る粒度配合ステップと、
を含む技術的解決手段によって実現できる。
The technical problem to be solved by the present invention is
(1) Spherical silicon fine powder to be sieved is placed in a coarse classification device and coarsely classified to obtain a coarse particle size product A having a particle size of Top cut 55 μm or more and a fine particle size product B having a particle size other than that. Steps and
(2) A precision classification step of putting the fine particle size product B obtained in step (1) into a precision classification device and performing precision classification to obtain a spherical silicon fine powder product C having a reduced number of coarse particles .
(3) The spherical silicon fine powder product C obtained in step (2) is placed in a mixer under air flow dispersion and mixed with the spherical silicon fine powder of the coarse particle size product A obtained in step (1) to mix the particle size . By performing the particle size compounding step to obtain spherical silicon fine powder for electronic packaging,
It can be realized by technical solutions including.
本発明が解決しようとする技術的課題はさらに、ステップ（１）に記載の粗い分級装置は、サイクロン分離器、渦分類器、振動スクリーン又は揺動スクリーンである技術的解決手段によって実現できる。 The technical problem to be solved by the present invention can be further realized by a technical solution means that the coarse classification device according to step (1) is a cyclone separator, a vortex classifier, a vibration screen or a swing screen.
本発明が解決しようとする技術的課題はさらに、ステップ（２）に記載の精密分級装置は、気流分級機、ボールトン振動ふるい機、超音波振動ふるい機、揺動振動ふるい機、リニア振動ふるい機、又は気流スクリーン機である技術的解決手段によって実現できる。 Further, the technical problem to be solved by the present invention is that the precision classification device described in step (2) includes an air flow classifier, a Bolton vibration sieve, an ultrasonic vibration sieve, a swing vibration sieve, and a linear vibration sieve. This can be achieved by a machine or a technical solution that is an airflow screen machine.
本発明が解決しようとする技術的課題はさらに、ステップ（３）で使用されるミキサーは、高撹拌機、二次元ミキサー、三次元ミキサー、ダブルコーンミキサー、Ｖ型ミキサー、無重力ミキサー、円錐ミキサー又はコールターミキサーである技術的解決手段によって実現できる。 Further, the technical problem to be solved by the present invention is that the mixer used in step (3) is a high stirrer, a two-dimensional mixer, a three-dimensional mixer, a double cone mixer, a V-type mixer, a gravity-free mixer, a conical mixer or This can be achieved by a technical solution that is a coalter mixer.
本発明が解決しようとする技術的課題はさらに、ステップ（３）に記載の粒度配合において、ステップ（２）に記載の球状シリコン微粉末製品Ｃとステップ（１）で得られた粗粒度製品Ａの球状シリコン微粉末との質量比が０．７０～０．７５：０．２５～０．３５である技術的解決手段によって実現できる。 Further, in the particle size compounding described in step (3), the technical problem to be solved by the present invention is the spherical silicon fine powder product C described in step (2) and the coarse particle size product A obtained in step (1). It can be realized by a technical solution in which the mass ratio of the above to the spherical silicon fine powder is 0.70 to 0.75: 0.25 to 0.35.
本発明が解決しようとする技術的課題はさらに、ステップ（１）に記載の球状シリコン微粉末は異なる粒径を有する多角形シリコン微粉末をガス燃焼炎法によって調製して得られる技術的解決手段によって実現できる。 Further, the technical problem to be solved by the present invention is a technical solution means obtained by preparing polygonal silicon fine powder having a different particle size from the spherical silicon fine powder according to step (1) by a gas combustion flame method. Can be achieved by.
本発明が解決しようとする技術的課題はさらに、多角形結晶シリコン微粉末の粒径をＤ５０：０．１～６０μｍに制御する技術的解決手段によって実現できる。 The technical problem to be solved by the present invention can be further realized by a technical solution means for controlling the particle size of the polygonal crystalline silicon fine powder to D50: 0.1 to 60 μm.
従来技術に比べて、本発明は、粗い分級及び精密分級プロセスにより球状シリコン微粉末から粗大粒子を除去することを実現し、充填材における粗大粒子を効果的に制御し、下流製品において使用されるときに粗大粒子がパッケージング接着剤注入口を詰ることやパッケージング不良を引き起こすことを回避し、粒度配合により、球状シリコン微粉末を使用するときに、システムの粘度、流動性への制御及び調整を実現し、製品の加工及び性能を向上させる。 Compared with the prior art, the present invention realizes the removal of coarse particles from spherical silicon fine powder by coarse classification and precision classification process, effectively controls the coarse particles in the filler, and is used in downstream products. Control and adjustment of system viscosity and fluidity when using spherical silicon fine powder, sometimes avoiding coarse particles clogging the packaging adhesive inlet and causing packaging defects, and particle size formulation And improve the processing and performance of the product.
当業者が本発明をさらに理解できるように、本発明の具体的な技術的解決手段についてさらに説明するが、その権利に対する制限を構成するものではない。 Specific technical solutions of the invention will be further described so that those skilled in the art can better understand the invention, but they do not constitute a limitation on their rights.
実施例１
電子パッケージング用の球状シリコン微粉末の調製方法であって、この方法では、篩い分けようとする球状シリコン微粉末から粗い分級及び精密分級によって粗大粒子を除去し、次に、粗い分級後に粗大粒子の制御の要件を満たす球状シリコン微粉末と、精密分級後の球状シリコン微粉末との粒度配合を行い、均一に混合させて電子パッケージング用の球状シリコン微粉末を調製して得た。
Example 1
A method for preparing spherical silicon fine powder for electronic packaging, in which coarse particles are removed from the spherical silicon fine powder to be sieved by coarse classification and precision classification, and then coarse particles are removed after coarse classification. Spherical silicon fine powder satisfying the control requirements of the above and spherical silicon fine powder after precision classification were mixed in particle size and mixed uniformly to prepare spherical silicon fine powder for electronic packaging.
実施例２
実施例１に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、
（１）篩い分けようとする球状シリコン微粉末を粗い分級装置に入れて粗い分級を行い、粗粒度製品Ａ及び細粒度製品Ｂを得る粗い分級ステップと、
（２）ステップ（１）で得られた細粒度製品Ｂを精密分級装置に入れて精密分級を行い、球状シリコン微粉末製品Ｃを得る精密分級ステップと、
（３）ステップ（２）で得られて球状シリコン微粉末製品Ｃを気流分散下でミキサーに入れ、ステップ（１）で得られた粗大粒子制御の要件を満たす球状シリコン微粉末と混合させ、電子パッケージング用の球状シリコン微粉末を得る粒度配合ステップとを含み、
粗粒度製品Ａとは、粒度がＴｏｐ ｃｕｔ５５μｍ以上である球状シリコン微粉末のことをいい、細粒度製品Ｂとは、粒度がＴｏｐ ｃｕｔ５５μｍ以下の球状シリコン微粉末のことをいい、細粒度製品Ｂの粒度は、Ｄ５０：０．１～３０μｍが好ましく、球状シリコン微粉末製品Ｃとは、粗大粒子の数を１０個以下に制御する球状シリコン微粉末のことをいい、球状シリコン微粉末製品Ｃの粒度は、Ｄ５０：６～４０μｍが好ましく、後続の精密分級の円滑性の要件を満たすために、粗い分級によって細粒度製品Ｂにおける粗大粒子の含有量を制御した。
Example 2
The method for preparing spherical silicon fine powder for electronic packaging according to Example 1.
(1) A coarse classification step of putting the spherical silicon fine powder to be sieved into a coarse classification device and performing coarse classification to obtain a coarse particle product A and a fine particle product B.
(2) In the precision classification step of putting the fine particle size product B obtained in step (1) into a precision classification device and performing precision classification to obtain a spherical silicon fine powder product C,
(3) The spherical silicon fine powder product C obtained in step (2) is placed in a mixer under airflow dispersion, mixed with the spherical silicon fine powder obtained in step (1) and satisfying the requirements for coarse particle control, and subjected to electrons. Including a particle size compounding step to obtain spherical silicon fine powder for packaging,
The coarse particle size product A means a spherical silicon fine powder having a particle size of Top cut 55 μm or more, and the fine particle size product B means a spherical silicon fine powder having a particle size of Top cut 55 μm or less. The particle size is preferably D50: 0.1 to 30 μm, and the spherical silicon fine powder product C refers to a spherical silicon fine powder that controls the number of coarse particles to 10 or less, and the particle size of the spherical silicon fine powder product C. D50: 6 to 40 μm, and the content of coarse particles in the fine particle size product B was controlled by coarse classification in order to satisfy the requirements for smoothness of subsequent precision classification.
実施例３
実施例２に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（１）における細粒度製品Ｂは、粒度がＴｏｐ ｃｕｔ５５μｍ以下の球状シリコン微粉末であった。
Example 3
In the method for preparing spherical silicon fine powder for electronic packaging according to Example 2, the fine particle size product B in step (1) was a spherical silicon fine powder having a particle size of Top cut 55 μm or less.
実施例４
実施例２～３に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（１）における粗い分級装置は、サイクロン分離器、渦分類器、振動スクリーン又は揺動スクリーンであった。
Example 4
The method for preparing spherical silicon fine powder for electronic packaging according to Examples 2 to 3, wherein the coarse classifier in step (1) is a cyclone separator, a vortex classifier, a vibration screen or a rocking screen. rice field.
実施例５
実施例２～４に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（２）における精密分級装置は、気流分級機、ボールトン振動ふるい機、超音波振動ふるい機、揺動振動ふるい機、リニア振動ふるい機、又は気流スクリーン機であった。
Example 5
The method for preparing spherical silicon fine powder for electronic packaging according to Examples 2 to 4, wherein the precision classification device in step (2) is an air flow classifier, a Vaulton vibrating sieve, an ultrasonic vibrating sieve, and the like. It was a oscillating vibration sieving machine, a linear oscillating sieving machine, or an air flow screen machine.
実施例６
実施例２～５に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（３）に記載の使用されるミキサーは、高撹拌機、二次元ミキサー、三次元ミキサー、ダブルコーンミキサー、Ｖ型ミキサー、無重力ミキサー、円錐ミキサー又はコールターミキサーであった。
Example 6
The method for preparing spherical silicon fine powder for electronic packaging according to Examples 2 to 5, wherein the mixer used in step (3) is a high stirrer, a two-dimensional mixer, a three-dimensional mixer, and a double. It was a cone mixer, a V-type mixer, a zero gravity mixer, a cone mixer or a coalter mixer.
実施例７
実施例２～６に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（３）で使用されるミキサーの負荷係数を０．３～０．５にした。
Example 7
In the method for preparing spherical silicon fine powder for electronic packaging according to Examples 2 to 6, the load coefficient of the mixer used in step (3) was set to 0.3 to 0.5.
実施例８
実施例２～７に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（３）に記載の粒度配合において、ステップ（２）に記載の球状シリコン微粉末製品Ｃと、ステップ（１）で得られて粗大粒子制御の要件を満たす球状シリコン微粉末との質量比は０．７０：０．２５であった。
Example 8
In the method for preparing spherical silicon fine powder for electronic packaging according to Examples 2 to 7, in the particle size formulation according to step (3), the spherical silicon fine powder product C according to step (2) and the spherical silicon fine powder product C according to step (2). The mass ratio with the spherical silicon fine powder obtained in step (1) and satisfying the requirements for controlling coarse particles was 0.70: 0.25.
実施例９
実施例２～７に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（３）に記載の粒度配合において、ステップ（２）に記載の球状シリコン微粉末製品Ｃと、ステップ（１）で得られて粗大粒子制御の要件を満たす球状シリコン微粉末との質量比は０．７５：０．３５であった。
Example 9
In the method for preparing spherical silicon fine powder for electronic packaging according to Examples 2 to 7, in the particle size formulation according to step (3), the spherical silicon fine powder product C according to step (2) and the spherical silicon fine powder product C according to step (2). The mass ratio with the spherical silicon fine powder obtained in step (1) and satisfying the requirements for coarse particle control was 0.75: 0.35.
実施例１０
実施例２～７に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（３）に記載の粒度配合において、ステップ（２）に記載の球状シリコン微粉末製品Ｃと、ステップ（１）で得られて粗大粒子制御の要件を満たす球状シリコン微粉末との質量比は０．７２：０．３０であった。
Example 10
In the method for preparing spherical silicon fine powder for electronic packaging according to Examples 2 to 7, in the particle size formulation according to step (3), the spherical silicon fine powder product C according to step (2) and the spherical silicon fine powder product C according to step (2). The mass ratio with the spherical silicon fine powder obtained in step (1) and satisfying the requirements for coarse particle control was 0.72: 0.30.
実施例１１
実施例２～８に記載の電子パッケージング用の球状シリコン微粉末の調製方法であって、ステップ（１）に記載の球状シリコン微粉末は異なる粒径の多角形であるシリコン微粉末をガス燃焼炎法によって調製して得られたものであって、多角形結晶シリコン微粉末の粒径をＤ５０：０．１～６０μｍにするように制御した。
Example 11
The method for preparing spherical silicon fine powder for electronic packaging according to Examples 2 to 8, wherein the spherical silicon fine powder according to step (1) gas-burns silicon fine powder having polygons having different particle sizes. It was prepared and obtained by a flame method, and the particle size of the polygonal crystalline silicon fine powder was controlled to be D50: 0.1 to 60 μm.
実施例１２
電子パッケージング用の球状シリコン微粉末の調製方法であって、
（１）粒径がＤ５０：０．１～６０μｍにするように制御された多角形であるシリコン微粉末を選択してガス燃焼炎法によって球状シリコン微粉末を調製して得る高温球状化処理ステップと、
（２）球状シリコン微粉末を粗い分級を行い、粗粒度製品Ａ及び細粒度製品Ｂを得る粗い分級ステップと、
（３）ステップ（１）で得られた細粒度製品Ｂを精密分級を行い、球状シリコン微粉末製品Ｃを得る精密分級ステップと、
（４）ステップ（３）で得られた球状シリコン微粉末製品Ｃとステップ（１）で得られて粗大粒子制御の要件を満たすシリコン微粉末を質量比０．７５：０．３５で混合させ、ミキサーの負荷係数を０．３にして、均一に混合させた後、完成品を得る粒度配合ステップとを含み、
実施例１２によって得られた完成品の粒度はＤ１０：１．８２μｍ、Ｄ５０：６．８８μｍ、Ｄ９０：１２．６μｍであり、粒度分布には二つのピークが現れて、比表面積は６．０ｍ２／ｇであり、粗大粒子を１０個以下にするように制御した。
Example 12
A method for preparing spherical silicon fine powder for electronic packaging.
(1) High-temperature spheroidizing treatment step obtained by selecting silicon fine powder having a polygon whose particle size is controlled to be D50: 0.1 to 60 μm and preparing spherical silicon fine powder by a gas combustion flame method. When,
(2) A coarse classification step of coarsely classifying spherical silicon fine powder to obtain a coarse particle size product A and a fine particle size product B.
(3) The fine particle size product B obtained in step (1) is subjected to precision classification to obtain a spherical silicon fine powder product C, and a precision classification step.
(4) The spherical silicon fine powder product C obtained in step (3) and the silicon fine powder obtained in step (1) and satisfying the requirements for coarse particle control are mixed at a mass ratio of 0.75: 0.35. Including a particle size compounding step of obtaining a finished product after uniformly mixing with a mixer load factor of 0.3.
The particle size of the finished product obtained in Example 12 was D10: 1.82 μm, D50: 6.88 μm, D90: 12.6 μm, two peaks appeared in the particle size distribution, and the specific surface area was 6.0 m 2 . It was / g, and the number of coarse particles was controlled to be 10 or less.
実施例１３
電子パッケージング用の球状シリコン微粉末の調製方法であって、
（１）粒径をＤ５０：０．１～６０μｍにするように制御した多角形であるシリコン微粉末を選択してガス燃焼炎法によって球状シリコン微粉末を調製して得る高温球状化処理ステップと、
（２）粗い分級：球状シリコン微粉末を粗い分級、粗粒度製品Ａ及び細粒度製品Ｂを得る粗い分級ステップと、
（３）精密分級：ステップ（１）で得られた細粒度製品Ｂを精密分級を行い、球状シリコン微粉末製品Ｃを得る精密分級ステップと、
（４）ステップ（３）で得られた球状シリコン微粉末製品Ｃとステップ（１）で得られて粗大粒子制御の要件を満たすシリコン微粉末とを質量比０．７０：０．３０で混合させ、ミキサーの負荷係数を０．４にし、均一に混合させた後、完成品を得る粒度配合ステップとを含み、
実施例１３によって得られた完成品の粒度はＤ１０：１．８５μｍ、Ｄ５０：７．００μｍ、Ｄ９０：１２．５９μｍであり、粒度分布には二つのピークが現れて、比表面積は５．５ｍ２／ｇであり、粗大粒子を１０個以下にするように制御した。
Example 13
A method for preparing spherical silicon fine powder for electronic packaging.
(1) A high-temperature spheroidizing treatment step obtained by selecting a polygonal silicon fine powder whose particle size is controlled to be D50: 0.1 to 60 μm and preparing spherical silicon fine powder by a gas combustion flame method. ,
(2) Coarse classification: Coarse classification of spherical silicon fine powder, coarse classification step to obtain coarse particle size product A and fine particle size product B, and
(3) Precision classification: A precision classification step of performing precision classification of the fine particle size product B obtained in step (1) to obtain a spherical silicon fine powder product C, and
(4) The spherical silicon fine powder product C obtained in step (3) and the silicon fine powder obtained in step (1) and satisfying the requirements for coarse particle control are mixed at a mass ratio of 0.70: 0.30. , Includes a particle size compounding step to obtain a finished product after setting the load factor of the mixer to 0.4 and mixing uniformly.
The particle size of the finished product obtained in Example 13 was D10: 1.85 μm, D50: 7.00 μm, D90: 12.59 μm, two peaks appeared in the particle size distribution, and the specific surface area was 5.5 m 2 . It was / g, and the number of coarse particles was controlled to be 10 or less.
比較例１
電子パッケージング用の球状シリコン微粉末の調製方法であって、
（１）粒径をＤ５０：０．１～６０μｍにするように制御した多角形であるシリコン微粉末を選択してガス燃焼炎法によって球状シリコン微粉末を調製して得る高温球状化処理ステップと、
（２）粗い分級：球状シリコン微粉末を、粗い分級を行い、粗粒度製品Ａ及び細粒度製品Ｂを得る粗い分級ステップと、
（３）精密分級：ステップ（１）で得られた細粒度製品Ｂを、精密分級を行い、球状シリコン微粉末製品Ｃを得る精密分級ステップと、
（４）ステップ（３）で得られた球状シリコン微粉末製品Ｃと、ステップ（１）で得られた粗大粒子制御の要件を満たすシリコン微粉末とを質量比０．７５：０．２５で混合させ、ミキサーの負荷係数を０．５にし、均一に混合させた後、完成品を得る粒度配合ステップとを含み、
比較例１によって得られた完成品の粒度はＤ１０：１．８８μｍ、Ｄ５０：７．１２μｍ、Ｄ９０：１２．６７μｍであり、粒度分布には二つのピークが現れ、比表面積は５．１ｍ2／ｇであり、粗大粒子は１０個以下に制御した。
Comparative Example 1
A method for preparing spherical silicon fine powder for electronic packaging.
(1) A high-temperature spheroidizing treatment step obtained by selecting a polygonal silicon fine powder whose particle size is controlled to be D50: 0.1 to 60 μm and preparing spherical silicon fine powder by a gas combustion flame method. ,
(2) Coarse classification: A coarse classification step of coarsely classifying spherical silicon fine powder to obtain a coarse particle size product A and a fine particle size product B.
(3) Precision classification: The fine particle size product B obtained in step (1) is subjected to precision classification to obtain a spherical silicon fine powder product C, and a precision classification step.
(4) The spherical silicon fine powder product C obtained in step (3) and the silicon fine powder obtained in step (1) that satisfy the requirements for coarse particle control are mixed at a mass ratio of 0.75: 0.25. Including a particle size compounding step to obtain a finished product after mixing, mixing the mixer to a load factor of 0.5 and mixing uniformly.
The particle size of the finished product obtained by Comparative Example 1 was D10: 1.88 μm, D50: 7.12 μm, D90: 12.67 μm, two peaks appeared in the particle size distribution, and the specific surface area was 5.1 m 2 /. It was g, and the number of coarse particles was controlled to 10 or less.
比較例２
ステップ（３）によって得られたシリコン微粉末製品Ｃを選択し、粒度配合を行わず、その粒度はＤ１０：３～５μｍ、Ｄ５０：６～９μｍ、Ｄ９０：１０～１５μｍであり、粒度分級は単一ピーク分布（Ｕｎｉｍｏｄａｌ ｄｉｓｔｒｉｂｕｔｉｏｎ）を示し、比表面積は約１ｍ2／ｇであり、粗大粒子を１０個以下にするように制御した。
Comparative Example 2
The silicon fine powder product C obtained in step (3) is selected, the particle size is not blended, the particle size is D10: 3 to 5 μm, D50: 6 to 9 μm, D90: 10 to 15 μm, and the particle size classification is simple. It showed a one-peak distribution (Unimodal dispersion), had a specific surface area of about 1 m 2 / g, and was controlled to have 10 or less coarse particles.
同じ配合成分システムにおいて比較例１および２と本発明における実施例１２および１３に対してアンダーフィルの性能検証を行い、試験結果は表１に示すとおり、 Underfill performance verification was performed on Comparative Examples 1 and 2 and Examples 12 and 13 in the present invention in the same compounding component system, and the test results are as shown in Table 1.
表１から分かるように、単一ピーク分布（Ｕｎｉｍｏｄａｌ ｄｉｓｔｒｉｂｕｔｉｏｎ）である球状シリコン微粉末製品は、流動性能は粒度配合後の球状シリコン微粉末製品よりはるかに低く、実施例１２、１３、によって得られた球状シリコン微粉末製品は、比表面積が増加するにつれて粘度が減少する傾向を示し、故に該球状シリコン微粉末製品の流動性、粘度などの性能を、球状シリコン微粉末製品の比表面積を調整することによって制御することができる。このシステムでは、比表面積が約５．５ｍ2／ｇに達すると、調製された球状シリコン微粉末は、粘度が比較的低いだけでなく、より良いフラッシュ特性も有する。また、本発明の方法を使用すると、球状シリコン微粉末における粗大粒子を１０個以下（普通は１００個以上）にするように制御することができ、本発明において、球状シリコン微粉末とは、粒度がＴｏｐ ｃｕｔ５５μｍ以下である製品をいい、粗大粒子の制御及び高充填における粒度分布への制御との問題を解決することを目的としているが、現在、業界内の研究のほとんどは、Ｔｏｐ ｃｕｔ７５μｍ以上の製品に着目しているという現状である。 As can be seen from Table 1, the spherical silicon fine powder product having a single peak distribution (Unimodal surface area) has a flow performance much lower than that of the spherical silicon fine powder product after the particle size compounding, and is obtained by Examples 12 and 13. The resulting spherical silicon fine powder product tends to decrease in viscosity as the specific surface area increases, and therefore the performance such as fluidity and viscosity of the spherical silicon fine powder product is adjusted by adjusting the specific surface area of the spherical silicon fine powder product. It can be controlled by doing. In this system, when the specific surface area reaches about 5.5 m 2 / g, the prepared spherical silicon fine powder not only has a relatively low viscosity, but also has better flash properties. Further, by using the method of the present invention, it is possible to control the number of coarse particles in the spherical silicon fine powder to be 10 or less (usually 100 or more), and in the present invention, the spherical silicon fine powder has a particle size. A product with a Top cut of 55 μm or less, which aims to solve the problem of controlling coarse particles and controlling the particle size distribution in high packing, but currently most of the research in the industry is Top cut of 75 μm or more. The current situation is that we are focusing on products.
Claims (4)
（２）ステップ（１）で得られた細粒度製品Ｂを精密分級装置に入れて精密分級を行い、粗大粒子の数が低減された球状シリコン微粉末製品Ｃを得る精密分級ステップと、
（３）ステップ（２）で得られた球状シリコン微粉末製品Ｃを、気流分散下でミキサーに入れ、ステップ（１）で得られた粗粒度製品Ａの球状シリコン微粉末と混合させて粒度配合を行うことで、電子パッケージング用の球状シリコン微粉末を得る粒度配合ステップと、を含み、
ステップ（３）に記載の粒度配合において、ステップ（２）に記載の球状シリコン微粉末製品Ｃとステップ（１）で得られた粗粒度製品Ａの球状シリコン微粉末との質量比が０．７５：０．３５～０．７０：０．３０である電子パッケージング用の球状シリコン微粉末の調製方法。 (1) Spherical silicon fine powder to be sieved is placed in a coarse classification device and coarsely classified to obtain a coarse particle size product A having a particle size of Top cut 55 μm or more and a fine particle size product B having a particle size other than that. Steps and
(2) A precision classification step of putting the fine particle size product B obtained in step (1) into a precision classification device and performing precision classification to obtain a spherical silicon fine powder product C having a reduced number of coarse particles.
(3) The spherical silicon fine powder product C obtained in step (2) is placed in a mixer under air flow dispersion and mixed with the spherical silicon fine powder of the coarse particle size product A obtained in step (1) to mix the particle size. To obtain a spherical silicon fine powder for electronic packaging, including a particle size compounding step.
In the particle size formulation described in step (3), the mass ratio of the spherical silicon fine powder product C described in step (2) to the spherical silicon fine powder of the coarse particle size product A obtained in step (1) is 0.75. : 0.35 to 0.70: 0.30: A method for preparing spherical silicon fine powder for electronic packaging.
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