JP5478193B2 - Solder powder manufacturing method - Google Patents
Solder powder manufacturing method Download PDFInfo
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- JP5478193B2 JP5478193B2 JP2009245077A JP2009245077A JP5478193B2 JP 5478193 B2 JP5478193 B2 JP 5478193B2 JP 2009245077 A JP2009245077 A JP 2009245077A JP 2009245077 A JP2009245077 A JP 2009245077A JP 5478193 B2 JP5478193 B2 JP 5478193B2
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- solder powder
- mixture
- aqueous solvent
- mass
- stirring
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- 229910000679 solder Inorganic materials 0.000 title claims description 207
- 239000000843 powder Substances 0.000 title claims description 188
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000000203 mixture Substances 0.000 claims description 83
- 239000002245 particle Substances 0.000 claims description 64
- 239000003125 aqueous solvent Substances 0.000 claims description 54
- 238000003756 stirring Methods 0.000 claims description 44
- 229910045601 alloy Inorganic materials 0.000 claims description 33
- 239000000956 alloy Substances 0.000 claims description 33
- 238000000227 grinding Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 23
- 238000000926 separation method Methods 0.000 claims description 20
- 238000010298 pulverizing process Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 238000009835 boiling Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 12
- 229910001338 liquidmetal Inorganic materials 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 7
- 230000002093 peripheral effect Effects 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- 125000003172 aldehyde group Chemical group 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 claims description 2
- 125000001302 tertiary amino group Chemical group 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 17
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 14
- 239000002904 solvent Substances 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 238000009826 distribution Methods 0.000 description 9
- 239000010949 copper Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 7
- 230000001186 cumulative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- -1 aliphatic aldehydes Chemical class 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010419 fine particle Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000009689 gas atomisation Methods 0.000 description 4
- 230000001603 reducing effect Effects 0.000 description 4
- 238000005476 soldering Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
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- 239000004677 Nylon Substances 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
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- 150000001299 aldehydes Chemical class 0.000 description 3
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- PDXRQENMIVHKPI-UHFFFAOYSA-N cyclohexane-1,1-diol Chemical compound OC1(O)CCCCC1 PDXRQENMIVHKPI-UHFFFAOYSA-N 0.000 description 2
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- NIOYUNMRJMEDGI-UHFFFAOYSA-N hexadecanal Chemical compound CCCCCCCCCCCCCCCC=O NIOYUNMRJMEDGI-UHFFFAOYSA-N 0.000 description 2
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- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
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- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical compound OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 description 2
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- MFEWNFVBWPABCX-UHFFFAOYSA-N 1,1,2,2-tetraphenylethane-1,2-diol Chemical compound C=1C=CC=CC=1C(C(O)(C=1C=CC=CC=1)C=1C=CC=CC=1)(O)C1=CC=CC=C1 MFEWNFVBWPABCX-UHFFFAOYSA-N 0.000 description 1
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 1
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 1
- JPZYXGPCHFZBHO-UHFFFAOYSA-N 1-aminopentadecane Chemical compound CCCCCCCCCCCCCCCN JPZYXGPCHFZBHO-UHFFFAOYSA-N 0.000 description 1
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- JOLQKTGDSGKSKJ-UHFFFAOYSA-N 1-ethoxypropan-2-ol Chemical compound CCOCC(C)O JOLQKTGDSGKSKJ-UHFFFAOYSA-N 0.000 description 1
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 1
- RUFPHBVGCFYCNW-UHFFFAOYSA-N 1-naphthylamine Chemical compound C1=CC=C2C(N)=CC=CC2=C1 RUFPHBVGCFYCNW-UHFFFAOYSA-N 0.000 description 1
- TZGPACAKMCUCKX-UHFFFAOYSA-N 2-hydroxyacetamide Chemical compound NC(=O)CO TZGPACAKMCUCKX-UHFFFAOYSA-N 0.000 description 1
- CRWNQZTZTZWPOF-UHFFFAOYSA-N 2-methyl-4-phenylpyridine Chemical compound C1=NC(C)=CC(C=2C=CC=CC=2)=C1 CRWNQZTZTZWPOF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
- 229910020816 Sn Pb Inorganic materials 0.000 description 1
- 229910020922 Sn-Pb Inorganic materials 0.000 description 1
- 229910008783 Sn—Pb Inorganic materials 0.000 description 1
- PCSMJKASWLYICJ-UHFFFAOYSA-N Succinic aldehyde Chemical compound O=CCCC=O PCSMJKASWLYICJ-UHFFFAOYSA-N 0.000 description 1
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- FUECIDVNGAUMGJ-UHFFFAOYSA-N acetic acid;2-(2-butoxyethoxy)ethanol Chemical compound CC(O)=O.CCCCOCCOCCO FUECIDVNGAUMGJ-UHFFFAOYSA-N 0.000 description 1
- OOCCDEMITAIZTP-UHFFFAOYSA-N allylic benzylic alcohol Natural products OCC=CC1=CC=CC=C1 OOCCDEMITAIZTP-UHFFFAOYSA-N 0.000 description 1
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- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は、粒径が微細であるはんだ粉の製造方法に関する。
The present invention relates to a method for producing solder powder having a fine particle size.
携帯通信機器等の電子機器の小型化か進んでおり、それに組み込まれる電子部品・電子回路の小型化が進み、今後もこの傾向は続くものと考えられる。はんだ粉を配合したはんだペーストが使用される部品・回路のサイズは小さくなっており、基板のスルーホールやＩＣチップの配線において１００μｍ程度の線幅または径に対応したファインピッチソルダリング技術の要求に適合したはんだペーストが必要となってきている。この場合、用いるはんだペーストに配合するはんだ粉の平均粒径は、５μｍ以下であることが望まれる場合がある。今後予想される電子部品や回路の更なる小型化の要請に対応するために、はんだペーストに配合するはんだ粉として、平均粒径３μｍ未満、更には平均粒径１μｍ未満のはんだ粉が要望されることが増加すると考えられる。 This trend is expected to continue in the future as electronic devices such as portable communication devices are becoming smaller and electronic components and electronic circuits incorporated therein are becoming smaller. The size of parts and circuits that use solder paste mixed with solder powder is becoming smaller, and it is necessary for fine pitch soldering technology that supports line widths and diameters of about 100 μm in substrate through holes and IC chip wiring. A suitable solder paste is needed. In this case, the average particle size of the solder powder blended in the solder paste used may be desired to be 5 μm or less. In order to meet the demand for further miniaturization of electronic components and circuits, solder powder having an average particle size of less than 3 μm and an average particle size of less than 1 μm is required as a solder powder to be blended in the solder paste. Is thought to increase.
従来よりはんだ粉は、ディスクアトマイズ法やガスアトマイズ法にてその多くが製造されているが、これらの方法では平均粒径１０μｍ以下のはんだ粉を得ることが困難であった。特許文献１には、ガスアトマイズ法でも製造条件を調整することにより、平均粒径５μｍ以下のはんだ粉が得られることが記載されている。しかし、ディスクアトマイズ法やガスアトマイズ法で平均粒径４μｍ以下のはんだ粉が得られた報告例はない。 Conventionally, many solder powders have been manufactured by a disk atomizing method or a gas atomizing method, but it has been difficult to obtain a solder powder having an average particle size of 10 μm or less by these methods. Patent Document 1 describes that solder powder having an average particle size of 5 μm or less can be obtained by adjusting the manufacturing conditions even in the gas atomization method. However, there is no report example in which solder powder having an average particle size of 4 μm or less was obtained by the disk atomizing method or the gas atomizing method.
また、ディスクアトマイズ法、ガスアトマイズ法以外のはんだ粉の製法としては、特許文献２に、オイルとハンダ溶融物を攪拌することによりはんだ粉を得る方法が記載されている。特許文献３には、微細粒状にされたリフローはんだを製造する方法が記載されているが、いずれの文献でも、平均粒径３μｍ以下のはんだ粉は得られていない。 As a method for producing solder powder other than the disk atomizing method and the gas atomizing method, Patent Document 2 describes a method of obtaining solder powder by stirring oil and solder melt. Patent Document 3 describes a method for producing a reflow solder having a fine particle shape, but in any document, a solder powder having an average particle diameter of 3 μm or less is not obtained.
上述したように、平均粒径３μｍ未満のはんだ粉は得られていない。そこで、本発明は、平均粒径が０．０５μｍ以上、３μｍ未満のはんだ粉の製造方法を得ることを目的とする。
As described above, solder powder having an average particle size of less than 3 μm has not been obtained. Then, an object of this invention is to obtain the manufacturing method of the solder powder whose average particle diameter is 0.05 micrometer or more and less than 3 micrometers.
本発明者らは、鋭意研究の結果、容器中に、固体または液体の金属と、非水系溶媒と、直径０．０５ｍｍ〜５ｍｍの粉砕用ボールとを入れ、混合物を得て、前記混合物を１５０℃以上に加熱し、攪拌した後、前記混合物から粉砕用ボールを分離して、はんだ粉と非水系溶媒の混合物を得て、前記はんだ粉と非水系溶媒の混合物を固液分離することにより、平均粒径０．０５μｍ以上、３μｍ未満のはんだ粉を得られることを知見し、本発明を完成するに至った。 As a result of diligent research, the inventors put solid or liquid metal, a non-aqueous solvent, and pulverizing balls having a diameter of 0.05 mm to 5 mm in a container to obtain a mixture. After heating to a temperature of ℃ or higher and stirring, the ball for pulverization is separated from the mixture to obtain a mixture of solder powder and non-aqueous solvent, and by solid-liquid separation of the mixture of solder powder and non-aqueous solvent, It has been found that solder powder having an average particle size of 0.05 μm or more and less than 3 μm can be obtained, and the present invention has been completed.
かかる知見に基づく本発明によれば、容器中に、固体または液体の金属と、非水系溶媒と、直径０．０５ｍｍ〜５ｍｍの粉砕用ボールとを入れ、混合物を得る工程と、前記混合物を１５０℃以上であって、且つ得ようとするはんだ粉の合金組成物の融点より高い温度に加熱し、攪拌する工程と、攪拌後の前記混合物から粉砕用ボールを分離して、はんだ粉と非水系溶媒の混合物を得る工程と、前記はんだ粉と非水系溶媒の混合物を固液分離して、はんだ粉を得る工程を有し、前記はんだ粉の平均粒径は０．０５μｍ以上、３μｍ未満である、はんだ粉の製造方法が提供される。
According to the present invention based on such knowledge, a step of obtaining a mixture by putting a solid or liquid metal, a non-aqueous solvent, and a pulverizing ball having a diameter of 0.05 mm to 5 mm in a container; Heating to a temperature higher than the melting point of the alloy composition of the solder powder to be obtained and stirring, and separating the balls for grinding from the mixture after stirring, so that the solder powder and the non-aqueous system A step of obtaining a mixture of the solvent and a step of obtaining a solder powder by solid-liquid separation of the mixture of the solder powder and the non-aqueous solvent, wherein the average particle size of the solder powder is 0.05 μm or more and less than 3 μm. A method for producing solder powder is provided.
また、本発明によれば、容器中に、固体または液体の金属と、非水系溶媒と、直径０．０５ｍｍ〜５ｍｍの粉砕用ボールとを入れ、混合物を得る工程と、前記混合物を１５０℃以上であって、且つ得ようとするはんだ粉の合金組成物の融点より高い温度に加熱し、攪拌する工程と、攪拌後の前記混合物から粉砕用ボールを分離して、はんだ粉と非水系溶媒の混合物を得る工程と、前記はんだ粉と非水系溶媒の混合物を固液分離して、はんだ粉を得る工程を有し、前記はんだ粉の平均粒径は０．０５μｍ以上、１μｍ未満である、はんだ粉の製造方法が提供される。Further, according to the present invention, a step of obtaining a mixture by putting a solid or liquid metal, a non-aqueous solvent, and a pulverizing ball having a diameter of 0.05 mm to 5 mm in a container, and the mixture at 150 ° C. or higher. And heating to a temperature higher than the melting point of the alloy composition of the solder powder to be obtained and stirring, and separating the grinding balls from the mixture after stirring, so that the solder powder and the non-aqueous solvent are mixed. A step of obtaining a mixture, and a step of solid-liquid separation of the mixture of the solder powder and the non-aqueous solvent to obtain a solder powder, wherein the solder powder has an average particle size of 0.05 μm or more and less than 1 μm. A method for producing a powder is provided.
また、本発明によれば、容器中に、固体または液体の金属と、非水系溶媒と、直径０．０５ｍｍ〜５ｍｍの粉砕用ボールとを入れ、混合物を得る工程と、前記混合物を１５０℃以上であって、且つ得ようとするはんだ粉の合金組成物の融点より高い温度に加熱し、攪拌する工程と、攪拌後の前記混合物から粉砕用ボールを分離して、はんだ粉と非水系溶媒の混合物を得る工程と、前記はんだ粉と非水系溶媒の混合物を固液分離して、はんだ粉を得る工程を有し、前記はんだ粉の平均粒径は０．０５μｍ以上、０．７μｍ未満である、はんだ粉の製造方法が提供される。Further, according to the present invention, a step of obtaining a mixture by putting a solid or liquid metal, a non-aqueous solvent, and a pulverizing ball having a diameter of 0.05 mm to 5 mm in a container, and the mixture at 150 ° C. or higher. And heating to a temperature higher than the melting point of the alloy composition of the solder powder to be obtained and stirring, and separating the grinding balls from the mixture after stirring, so that the solder powder and the non-aqueous solvent are mixed. A step of obtaining a mixture, and a step of obtaining a solder powder by solid-liquid separation of the mixture of the solder powder and the non-aqueous solvent, wherein the average particle size of the solder powder is 0.05 μm or more and less than 0.7 μm. A method for producing solder powder is provided.
前記はんだ粉は、Ｓｎを９０質量％〜９９．９質量％、Ａｇを０．０５質量％〜１０質量％含有するものでも良い。また、前記はんだ粉は、Ｓｎを５０質量％〜９０質量％、Ｐｂを１０質量％〜５０質量％含有するものでも良い。また、前記非水系溶媒の沸点は１５０℃以上であってもよい。また、前記非水系溶媒はアルデヒド基またはヒドロキシ基を有する有機溶媒であってもよい。また、前記非水系溶媒は一級アミノ基、または二級アミノ基、または三級アミノ基の内の少なくとも一種以上を含む有機溶媒であってもよい。 The solder powder may contain 90 mass% to 99.9 mass% of Sn and 0.05 mass% to 10 mass% of Ag. The solder powder may contain 50 mass% to 90 mass% of Sn and 10 mass% to 50 mass% of Pb. Further, the boiling point of the nonaqueous solvent may be 0.99 ° C. or higher. The non-aqueous solvent may be an organic solvent having an aldehyde group or a hydroxy group. The non-aqueous solvent may be an organic solvent containing at least one of a primary amino group, a secondary amino group, or a tertiary amino group.
また、羽根を周速２００ｃｍ／秒〜２００００ｃｍ／秒で回転することにより前記攪拌する工程を行ってもよい。また、前記固液分離を遠心分離またはフィルタープレスにより行ってもよい。また、前記はんだ粉と非水系溶媒の混合物を固液分離した後、はんだ粉を沸点１５０℃以下の有機溶媒で洗浄してもよい。また、前記金属の体積が、前記非水系溶媒の体積の０．１体積％〜２０体積％であってもよい。 Moreover, you may perform the said stirring process by rotating a blade | wing at a peripheral speed of 200 cm / sec-20000 cm / sec. The solid-liquid separation may be performed by centrifugation or a filter press. Further, after solid-liquid separation of the mixture of the solder powder and the non-aqueous solvent, the solder powder may be washed with an organic solvent having a boiling point of 150 ° C. or less. The volume of the metal may be 0.1% by volume to 20% by volume of the volume of the non-aqueous solvent.
本発明のはんだ粉は、平均粒径が３μｍ未満と小さく、今後ますます高度化することが予想されるファインピッチソルダリング技術の要求に適合したはんだペースト用材料として活用することができる。 The solder powder of the present invention has a small average particle size of less than 3 μm, and can be used as a solder paste material that meets the requirements of fine pitch soldering technology that is expected to become increasingly sophisticated in the future.
以下、本発明の実施の形態について説明する。なお、本実施の形態は本発明を限定するものではない。 Embodiments of the present invention will be described below. Note that this embodiment does not limit the present invention.
＜はんだ粉の合金組成＞
本発明におけるはんだ粉の合金組成としては、種々のはんだ合金を用いることが可能である。具体的な合金組成としては第１に、Ｓｎが９０質量％〜９９．９質量％、Ａｇが０．０５質量％〜１０質量％含有する合金が挙げられる。この場合、鉛を含有しない無鉛はんだ粉を得ることも可能である。第２に、Ｓｎが５０質量％〜９０質量％、Ｐｂが１０質量％〜５０質量％含有合金が挙げられる。これらの合金組成にすることにより、低融点のはんだ粉を得ることができ、低融点であることは、溶媒中で攪拌する本発明の製造方法を適用する上で、有利である。前記の合金は、必要に応じて、銅、亜鉛、ビスマス、インジウム、アンチモン等の元素のいずれか一種又は二種以上を含んでもよい。
<Alloy composition of solder powder>
As an alloy composition of the solder powder in the present invention, various solder alloys can be used. As a specific alloy composition, first, an alloy containing Sn of 90% by mass to 99.9% by mass and Ag of 0.05% by mass to 10% by mass is included. In this case, it is also possible to obtain lead-free solder powder that does not contain lead. Secondly, an alloy containing 50 mass% to 90 mass% of Sn and 10 mass% to 50 mass% of Pb. By using these alloy compositions, solder powder having a low melting point can be obtained. The low melting point is advantageous in applying the production method of the present invention in which stirring is performed in a solvent. The alloy may contain one or more elements such as copper, zinc, bismuth, indium, and antimony as necessary.
＜はんだ粉の平均粒径＞
はんだ粉の平均粒径は、０．０５μｍ以上、３μｍ未満であることが好ましい。３μｍ以上の場合には、ファインピッチソルダリング技術の要求に十分適合できない場合があり、０．０５μｍ未満のはんだ粉は、表面活性が高く、酸化等の変質による問題が生じることがある。
電子部品や電子回路の更なる小型化によるファインピッチソルダリング技術の要求水準高度化に対応するためには、はんだ粉の平均粒径は、１μｍ未満とすることが更に好ましく、０．７μｍ以下とすることが一層好ましい。
<Average particle size of solder powder>
The average particle size of the solder powder is preferably 0.05 μm or more and less than 3 μm. If it is 3 μm or more, it may not fully meet the requirements of fine pitch soldering technology, and solder powder of less than 0.05 μm has high surface activity and may cause problems due to alteration such as oxidation.
In order to meet the demand level of fine pitch soldering technology due to further miniaturization of electronic components and electronic circuits, the average particle size of the solder powder is more preferably less than 1 μm, and 0.7 μm or less. More preferably.
本発明のはんだ粉は、以下の工程を経ることにより、製造することができる。
容器中に、固体または液体の金属と、非水系溶媒と、直径０．０５ｍｍ〜５ｍｍの粉砕用ボールとを入れ、混合物を得る工程。
（２）前記混合物を１５０℃以上に加熱し、攪拌する工程。
（３）前記混合物から粉砕用ボールを分離して、はんだ粉と非水系溶媒の混合物を得る工程。
（４）前記はんだ粉と非水系溶媒の混合物を固液分離して、はんだ粉を得る工程。
必要に応じて、得られたはんだ粉に対して、洗浄、乾燥等を行ってもよい。
The solder powder of the present invention can be manufactured through the following steps.
A step of putting a solid or liquid metal, a non-aqueous solvent, and grinding balls having a diameter of 0.05 mm to 5 mm into a container to obtain a mixture.
(2) A step of heating and stirring the mixture to 150 ° C. or higher.
(3) A step of separating the grinding balls from the mixture to obtain a mixture of solder powder and a non-aqueous solvent.
(4) A step of obtaining a solder powder by solid-liquid separation of the mixture of the solder powder and the non-aqueous solvent.
You may perform washing | cleaning, drying, etc. with respect to the obtained solder powder as needed.
＜原料金属＞
はんだ粉の原料金属としては、得ようとするはんだ粉と同一の金属組成を持つ例えばＳｎが９０質量％〜９９．９質量％、Ａｇが０．０５質量％〜１０質量％含有するはんだ合金、Ｓｎが５０質量％〜９０質量％、Ｐｂが１０質量％〜５０質量％含有するはんだ合金またはこれらはんだ合金の原料となる金属の混合物を使用することができる。均一な金属組成をもつはんだ粉をより容易に得ることができるようにするためには、合金を使用することが好ましい。
<Raw metal>
As a raw material metal of the solder powder, a solder alloy having the same metal composition as the solder powder to be obtained, for example, Sn is contained in 90 mass% to 99.9 mass%, and Ag is contained in 0.05 mass% to 10 mass%, A solder alloy containing 50 mass% to 90 mass% of Sn and 10 mass% to 50 mass% of Pb or a mixture of metals used as a raw material of these solder alloys can be used. In order to obtain a solder powder having a uniform metal composition more easily, it is preferable to use an alloy.
＜非水系溶媒＞
本発明での非水系溶媒とはその沸点が、１５０℃以上であるものが好適であり、２００℃以上であるものが特に好適である。後述するように、はんだ粉を得るためには、非水系溶媒として得ようとするはんだ粉の融点よりも高い沸点をもつものが好ましいが、攪拌をおこなう容器に圧力容器を用いることにより、雰囲気圧力を上げ、常圧の沸点がはんだ粉の融点より低い非水系溶媒でも、使用が可能である。しかしながら製造装置に耐圧性能が必要となるので、沸点は、得ようとするはんだ粉の溶融温度よりも１０℃以上高いことが望ましい。更に非水系溶媒として、はんだ粉が酸素と反応して、表面に酸化物を形成しやすいために、還元性を有する溶媒であることが更に好ましい。
<Non-aqueous solvent>
The non-aqueous solvent in the present invention preferably has a boiling point of 150 ° C. or higher, and particularly preferably has a boiling point of 200 ° C. or higher. As will be described later, in order to obtain the solder powder, those having a boiling point higher than the melting point of the solder powder to be obtained as a non-aqueous solvent are preferable, but by using a pressure vessel as the vessel for stirring, the atmospheric pressure It is possible to use a non-aqueous solvent whose boiling point at normal pressure is lower than the melting point of the solder powder. However, since the pressure resistance performance is required for the manufacturing apparatus, the boiling point is desirably higher by 10 ° C. than the melting temperature of the solder powder to be obtained. Further, as the non-aqueous solvent, the solder powder reacts with oxygen and easily forms an oxide on the surface, so that a solvent having a reducing property is more preferable.
例えば、このような非水系溶媒の一例として、沸点が１５０℃から４００℃の範囲のアルコール系溶媒が挙げられる。具体的にはＳｎ−Ａｇ−Ｃｕ系はんだの融点が２１８℃の場合、且つ常圧下で以下に述べる攪拌操作を行ない、微粉化されたはんだ粉を得るためには、非水系溶媒の沸点は２２０℃以上であることが好ましく、２５０℃以上であることが更に好ましい。 For example, an alcohol solvent having a boiling point in the range of 150 ° C. to 400 ° C. is an example of such a non-aqueous solvent. Specifically, when the melting point of the Sn—Ag—Cu solder is 218 ° C. and the stirring operation described below is performed under normal pressure, a non-aqueous solvent has a boiling point of 220 in order to obtain finely divided solder powder. It is preferable that the temperature is higher than or equal to ° C, more preferably higher than or equal to 250 ° C.
具体的には、非水系溶媒として、一価アルコール、または二価アルコールのグリコールがある。一価アルコールとしては、例えば、ブチルアルコール、アミルアルコール、ヘキシルアルコール、ヘプチルアルコール、オクチルアルコール、デシルアルコール、ノニルアルコール、シクロペンタノール、ベンジルアルコール、シンナミルアルコール等がある。グリコール系の溶媒としては、グリセリン、エチレングリコール、ジエチレングリコール、トリエチレングリコール、プロピレングリコール、トリメチレングリコール、ブタンジオール、ペンタンジオール、ヘキサンジオール、ヘプタンジオール、オクタンジオール、ノナンジオール、デカンジオール、ベンズピナコール、ヒドロベンゾイル、シクロペンダジオール、シクロヘキサンジオール、シクロヘキサンジオール、グリコール酸アミド、ジエチレングリコールジメチルエーテル、ジエチレングリコールジエチルエーテル、プロピレングリコールモノエチルエーテル、ジエチレングリコールジブチルエーテル、酢酸ジエチレングリコールモノブチルエーテル、プロピレングリコールモノメチルエーテルアセタート等があり、分子量の大きいものではポリエチレングリコール、ポリエチレングリコールエステル、ポリエチレングリコールエーテルがある。特にグリコール、ジオール系のものは水酸基を二つ持つものであるため、極性を持ち、粉の分散性に寄与するので望ましい。このような溶媒としては、例えば−ＣＨ２−ＣＨＯＨ、または−ＣＨＲ−ＣＨＯＨ、−ＣＲ１Ｒ２−ＣＨＯＨ、＝ＣＨＣＨＯＨ、＝ＣＲＣＨＯＨ（Ｒ、Ｒ１、Ｒ２：側鎖）を分子中に含まれるもので、且つ溶媒の沸点は少なくとも１００℃以上のものである。更にはアルデヒド基−ＣＨＯを持つ有機化合物も同様な効果を持ち、例えば、脂肪族飽和アルデヒドとして、ラウリンアルデヒド、トリデシルアルデヒド、ミリスチンアルデヒド、カプロンアルデヒド、ヘプトアルデヒド、ペンタデシルアルデヒド、パルミチンアルデヒド、マルガリンアルデヒド、ステアリンアルデヒドが挙げられ、脂肪族ジアルデヒドとしては例えばスクシンジアルデヒドがあり、脂肪族不飽和アルデヒドとして、クロトンアルデヒド、更には芳香族アルデヒドには、ベンズアルデヒド、トルアルデヒド、サリチルアルデヒド、シンナムアルデヒド、ナフトアルデヒド等があり、複素環式アルデヒドにはフルフラールが挙げられる。アミン系の還元性溶媒としては、ヘキシルアミン、ヘブチンアミン、オクチルアミン、ウンデシルアミン、トリデシルアミン、テトラデシルアミン、ペンタデシルアミン、セチルアミン、ジブチルアミン、ジアミルアミン、シクロヘキシルアミン、アニリン、ナフチルアミン、トルイジン等がある。 Specifically, the non-aqueous solvent includes a monohydric alcohol or a dihydric alcohol glycol. Examples of the monohydric alcohol include butyl alcohol, amyl alcohol, hexyl alcohol, heptyl alcohol, octyl alcohol, decyl alcohol, nonyl alcohol, cyclopentanol, benzyl alcohol, and cinnamyl alcohol. Examples of glycol solvents include glycerin, ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, trimethylene glycol, butanediol, pentanediol, hexanediol, heptanediol, octanediol, nonanediol, decanediol, benzpinacol, hydro Benzoyl, cyclopentadiol, cyclohexanediol, cyclohexanediol, glycolic acid amide, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, propylene glycol monoethyl ether, diethylene glycol dibutyl ether, acetic acid diethylene glycol monobutyl ether, propylene glycol monomethyl ether acetate, etc. big Intended polyethylene glycol, polyethylene glycol esters, polyethylene glycol ethers. In particular, glycols and diols are preferable because they have two hydroxyl groups and thus have polarity and contribute to the dispersibility of the powder. As such a solvent, for example, —CH 2 —CHOH, or —CHR—CHOH, —CR 1 R 2 —CHOH, ═CHCHOH, ═CRCHOH (R, R 1 , R 2 : side chain) is included in the molecule. The boiling point of the solvent is at least 100 ° C. or higher. Furthermore, an organic compound having an aldehyde group —CHO has the same effect. For example, as an aliphatic saturated aldehyde, lauric aldehyde, tridecyl aldehyde, myristic aldehyde, capron aldehyde, heptaldehyde, pentadecyl aldehyde, palmitic aldehyde, marga aldehyde. Examples include aliphatic aldehydes such as succindialdehyde, aliphatic unsaturated aldehydes such as crotonaldehyde, and aromatic aldehydes such as benzaldehyde, tolualdehyde, salicylaldehyde, and cinnamaldehyde. And naphthaldehyde, and the heterocyclic aldehyde includes furfural. Examples of amine-based reducing solvents include hexylamine, hebutinamine, octylamine, undecylamine, tridecylamine, tetradecylamine, pentadecylamine, cetylamine, dibutylamine, diamylamine, cyclohexylamine, aniline, naphthylamine, and toluidine. is there.
＜粉砕用ボール＞
本発明に用いる粉砕用ボールとしては、材質としてセラミックス系を用いたアルミナボール、ジルコニアボール、ムライトボール、ガラスボール、金属系のステンレスボールや鉄ボール等を使用することができ、特に材質に制限はないが、粉砕用ボールの材質として、耐久性が高く、はんだ粉への不純物の混入が少ない利点のある、ジルコニア、アルミナ、ステンレス鋼が、特に好適である。
<Crushing ball>
As the grinding balls used in the present invention, alumina balls, zirconia balls, mullite balls, glass balls, metal stainless steel balls or iron balls using ceramics as materials can be used, and the material is not particularly limited. Nonetheless, zirconia, alumina, and stainless steel are particularly suitable as the material for the ball for pulverization, which has the advantages of high durability and low contamination of solder powder.
粉砕用ボールは、粒径が０．０５ｍｍ〜５ｍｍであることが好ましい。粒径１５ｍｍ超の粉砕用ボールのみを使用すると、目的とする微細な粒径をもつはんだ粉を得ることが難しくなり、粒径０．０５ｍｍ未満の粉砕用ボールのみを使用すると、攪拌後の固液分離に時間を要することがある。
より粒径の小さいはんだ粉を容易に得るためには、粉砕用ボールの粒径は、０．１〜５ｍｍが更に好ましく、０．１〜３ｍｍが一層好ましく、０．１〜１ｍｍが更に一層好ましい。粉砕用ボールを大きな粒径のものと小さな粒径のものとを組み合わせて使用することも可能である。この場合には、大きなボールサイズは特に粒径１５ｍｍにこだわる必要はなく、例えば、粒径３０ｍｍでも良い。少なくとも粒径０．０５ｍｍ〜１５ｍｍの粉砕用ボールが５０質量％入っていることが必要である。
The grinding balls preferably have a particle size of 0.05 mm to 5 mm. If only pulverizing balls having a particle diameter of more than 15 mm are used, it becomes difficult to obtain solder powder having a desired fine particle diameter. If only pulverizing balls having a particle diameter of less than 0.05 mm are used, solidification after stirring is difficult. Liquid separation may take time.
In order to easily obtain a solder powder having a smaller particle diameter, the particle diameter of the ball for grinding is more preferably 0.1 to 5 mm, further preferably 0.1 to 3 mm, and still more preferably 0.1 to 1 mm. . It is also possible to use a pulverizing ball in combination of a large particle size and a small particle size. In this case, the large ball size need not be particularly concerned with the particle size of 15 mm, and may be, for example, a particle size of 30 mm. It is necessary that at least 50% by mass of grinding balls having a particle diameter of 0.05 mm to 15 mm be contained.
粉砕用ボールの表面に、はんだが付着しにくい材質であるダイヤモンドライクカーボン（ＤＬＣ）やＢ，Ｃ，Ｎ等の化合物を形成することができる。 Diamond-like carbon (DLC) or a compound such as B, C, or N, which is a material to which solder is difficult to adhere, can be formed on the surface of the grinding ball.
＜混合物の体積比＞
前記混合物の体積比は、用いる非水系溶媒の体積に対して、金属原料は、０．１体積％〜２０体積％が好ましく、０．１体積％〜１０体積％が一層好ましい。粉砕用ボールは、用いる非水系溶媒の体積に対して、２０体積％〜６００体積％が好ましい。金属原料が０．１体積％未満の場合、生産性が低くなり、２０体積％超の場合には、得られるはんだ粉の粒径が十分小さくならないことがある。粉砕用ボールが２０体積％未満の場合には、得られるはんだ粉の粒径が十分小さくならないことがあり、６００体積％超の場合は、粉砕用ボールの表面に原料用金属が多く付着した状態となることがある。前記混合物を容器中で静置したときに、前記粉砕用ボールの上面と前記非水系溶媒の上面の高さが、略同一となるように、前記粉砕用ボールの前記非水系溶媒に対する体積比率を調整することにより、微粒子のはんだ粉が得やすくなるので、更に好ましい。
<Volume ratio of the mixture>
The volume ratio of the mixture is preferably 0.1% by volume to 20% by volume, and more preferably 0.1% by volume to 10% by volume with respect to the volume of the non-aqueous solvent used. The grinding balls are preferably 20% by volume to 600% by volume with respect to the volume of the non-aqueous solvent used. When the metal raw material is less than 0.1% by volume, the productivity is low, and when it exceeds 20% by volume, the particle size of the obtained solder powder may not be sufficiently small. When the pulverizing ball is less than 20% by volume, the particle size of the obtained solder powder may not be sufficiently small. When the pulverizing ball is more than 600% by volume, a large amount of raw material metal adheres to the surface of the pulverizing ball. It may become. When the mixture is allowed to stand in a container, the volume ratio of the grinding ball to the non-aqueous solvent is set so that the height of the top surface of the grinding ball and the top surface of the non-aqueous solvent are substantially the same. By adjusting, it becomes easier to obtain fine solder powder, which is more preferable.
＜加熱・攪拌工程＞
前記金属原料と、前記非水系溶媒と、前記粉砕用ボールの混合物を加熱・攪拌することにより、平均粒径が０．０５μｍ以上、３μｍ未満であるはんだ粉を生成することができる。
<Heating and stirring process>
By heating and stirring the mixture of the metal raw material, the non-aqueous solvent, and the grinding balls, a solder powder having an average particle size of 0.05 μm or more and less than 3 μm can be generated.
加熱・攪拌する雰囲気は、不活性ガスまたは還元性ガスとすることが好ましい。雰囲気を空気とした場合、生成したはんだ粉の表面に厚い酸化膜が生成することがあり、雰囲気中の酸素濃度は低いほうが好ましい。不活性ガスとしては、窒素、アルゴン等が挙げられ、還元性ガスとしては、水素または水素と不活性ガスの混合ガスが挙げられる。 The atmosphere for heating and stirring is preferably an inert gas or a reducing gas. When the atmosphere is air, a thick oxide film may be generated on the surface of the generated solder powder, and the oxygen concentration in the atmosphere is preferably low. Examples of the inert gas include nitrogen and argon, and examples of the reducing gas include hydrogen or a mixed gas of hydrogen and an inert gas.
加熱・攪拌する際、混合物の加熱温度は、得ようとするはんだ粉の合金組成物の融点より高い温度とすればよいが、前記融点より５℃以上高い温度に加熱することが好ましい。前記加熱温度が、前記融点に近いと、高い温度制御性が必要となり設備コストが高くなる。前記加熱温度は、使用する非水系溶媒の沸点（加圧下で加熱・攪拌する場合には、該加圧下での沸点）未満の温度とする。前記加熱温度は、前記合金組成物の融点より、５０℃以上高くしても特に効果はなく、前記融点に５０℃を加えた温度以下とすることができる。 When heating and stirring, the heating temperature of the mixture may be higher than the melting point of the alloy composition of the solder powder to be obtained, but it is preferable to heat the mixture to a temperature higher by 5 ° C. than the melting point. When the heating temperature is close to the melting point, high temperature controllability is required and the equipment cost is increased. The heating temperature is set to a temperature lower than the boiling point of the non-aqueous solvent to be used (in the case of heating and stirring under pressure, the boiling point under pressure). The heating temperature has no particular effect even if it is higher by 50 ° C. or more than the melting point of the alloy composition, and can be made equal to or lower than the temperature obtained by adding 50 ° C. to the melting point.
攪拌は、攪拌羽根を回転することによりおこなうことができ、ミル等の粉砕用ボールを用いることができる粉砕機を用いておこなってもよい。回転数等の粉砕条件は、混合物の内容と得ようとするはんだ粉の平均粒径に応じて、適宜選択すれば良く、攪拌羽根等の回転数を上昇させることにより、得られるはんだ粉の平均粒径を小さくすることができる。例えば、攪拌羽根を用いる場合、その回転数は、１００〜１０００００
ｒｐｍの範囲、攪拌羽根の周速は、１００〜５０００ｃｍ／ｓｅｃの範囲に設定することができる。
Stirring can be performed by rotating a stirring blade, and may be performed using a pulverizer that can use pulverizing balls such as a mill. The pulverization conditions such as the number of revolutions may be appropriately selected according to the content of the mixture and the average particle diameter of the solder powder to be obtained. By increasing the number of revolutions of the stirring blade, the average of the obtained solder powder The particle size can be reduced. For example, when a stirring blade is used, the rotational speed is 100 to 100,000.
The range of rpm and the peripheral speed of the stirring blade can be set in the range of 100 to 5000 cm / sec.
＜粉砕用ボールの分離＞
加熱・攪拌後、混合物は、攪拌をおこなった状態で、はんだ粉の融点より１０℃以上低い温度まで冷却する。その後、混合物から粉砕用ボールをメッシュを通す等の公知の手段により分離して、はんだ粉と非水系溶媒の混合物を得る。
<Separation of balls for grinding>
After the heating / stirring, the mixture is cooled to a temperature lower by 10 ° C. or more than the melting point of the solder powder in a state of stirring. Thereafter, the mixture is separated from the mixture by a known means such as passing a pulverizing ball through a mesh to obtain a mixture of solder powder and a non-aqueous solvent.
＜固液分離＞
前記工程で得られたはんだ粉と非水系溶媒の混合物の固液分離をおこなう。固液分離は、遠心分離、フィルタープレスによるろ過等の公知の方法によりおこなうことができる。なお、用いた非水系溶媒が、はんだ粉の分散媒として支障ない場合には、固液分離をおこなう必要はない。
<Solid-liquid separation>
Solid-liquid separation of the mixture of the solder powder and non-aqueous solvent obtained in the above step is performed. Solid-liquid separation can be performed by a known method such as centrifugation or filtration with a filter press. In addition, when the used non-aqueous solvent does not have a trouble as a dispersion medium of solder powder, it is not necessary to perform solid-liquid separation.
＜洗浄・乾燥＞
固液分離したはんだ粉は、溶媒で洗浄することができる。前記溶媒としては、メタノール、エタノール等の低沸点であるアルコールの有機溶媒が好適な例としてあげられる。洗浄後、真空乾燥等の高温加熱をおこなわない方法で乾燥することにより、使用した非水系溶媒の残留が少ないはんだ粉を得ることができる。
<Washing and drying>
The solid-liquid separated solder powder can be washed with a solvent. A suitable example of the solvent is an organic solvent of alcohol having a low boiling point such as methanol or ethanol. After washing, drying by a method that does not perform high-temperature heating, such as vacuum drying, can yield a solder powder with little residual non-aqueous solvent used.
［実施例１］
Ｓｎ−Ａｇ−Ｃｕ系はんだ粉を製造する実施例を以下に説明する。Ｓｎ９９質量％、Ａｇ０．３質量％、Ｃｕ０．７質量％である組成のはんだ合金線１ｍｍΦを５ｇを秤量し、このはんだ線を３００ｍＬのセパラブルフラスコに投入した。次に１ｍｍΦのジルコニアボール３００ｇを前記施パブルフラスコに投入し、更に、テトラエチレングリコールを５０ｍＬを投入して、混合物を得た。この後、セパラブルフラスコの上蓋をして密封し、窒素ガスを１００ｍＬ／ｍｉｎで流し、１０分間ガス置換をした。次に、セパブルフラスコ内に設置してあった回転径が６ｃｍのステンレス製の攪拌羽根を７００ｒｐｍ回転させることにより攪拌をおこなった状態で、混合物を２３０℃まで加熱した。混合物を２３０℃で１時間保持した後、前記攪拌状態を維持したまま、加熱を止めることにより自然冷却を行った。混合物が１２０℃以下になった段階で攪拌羽根の回転を止めた。次にこの混合物を１５０メッシュのナイロン生地の網を通過させて、１ｍｍΦのジルコニアボールを混合物から分離した。ろ過された側には微粉化したはんだ粉が分散した溶媒（テトラエチレングリコール）が回収された。テトラエチレングリコールを洗浄除去するために、前記はんだ粉が分散した溶媒を３０００ｒｐｍ、5分間の処理条件で遠心分離して固液分離し、上澄みの液体を除去して、はんだ粉を回収した。この後、下記の要領で、洗浄を行った。回収したはんだ粉を１００ｍLのエタノール中と攪拌混合し、再分散した後、３０００ｒｐｍ、5分間の処理条件で遠心分離して固液分離し、上澄みの液体を除去して、はんだ粉を回収した。この回収したはんだ粉をエタノール中に分散後、遠心分離による固液分離する操作を５回繰返しおこなった。得られたはんだ粉を６０℃で真空乾燥して、乾燥済みのはんだ粉を得た。
[Example 1]
An embodiment for producing Sn—Ag—Cu solder powder will be described below. 5 g of solder alloy wire 1 mmΦ having a composition of Sn 99% by mass, Ag 0.3% by mass, and Cu 0.7% by mass was weighed, and this solder wire was put into a 300 mL separable flask. Next, 300 g of zirconia balls having a diameter of 1 mmΦ were introduced into the applied flask, and 50 mL of tetraethylene glycol was further introduced to obtain a mixture. Thereafter, the upper lid of the separable flask was sealed and sealed, and nitrogen gas was allowed to flow at 100 mL / min to perform gas replacement for 10 minutes. Next, the mixture was heated to 230 ° C. while stirring was performed by rotating a stirring blade made of stainless steel having a rotational diameter of 6 cm, which had been installed in the separable flask, at 700 rpm. After maintaining the mixture at 230 ° C. for 1 hour, the mixture was naturally cooled by stopping heating while maintaining the stirring state. When the mixture became 120 ° C. or lower, the rotation of the stirring blade was stopped. The mixture was then passed through a 150 mesh nylon fabric net to separate 1 mmΦ zirconia balls from the mixture. On the filtered side, a solvent (tetraethylene glycol) in which finely divided solder powder was dispersed was recovered. In order to wash away tetraethylene glycol, the solvent in which the solder powder was dispersed was subjected to solid-liquid separation by centrifuging at 3000 rpm for 5 minutes, and the supernatant liquid was removed to collect the solder powder. Thereafter, cleaning was performed in the following manner. The collected solder powder was stirred and mixed with 100 mL of ethanol, redispersed, centrifuged at 3000 rpm for 5 minutes and solid-liquid separated, and the supernatant liquid was removed to collect the solder powder. The collected solder powder was dispersed in ethanol and then subjected to solid-liquid separation by centrifugation five times. The obtained solder powder was vacuum dried at 60 ° C. to obtain a dried solder powder.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲ（PerkinElmer社製、Spectrum 100）でテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined with a reflective FT-IR (PerkinElmer, Spectrum 100) for the presence or absence of a tetraethylene glycol hydroxy group peak, but no such peak was observed.
前記乾燥済みのはんだ粉について、ＳＥＭ観察を行った結果、図１、図２に示すように球状の粉が得られた。また、前記乾燥済みのはんだ粉について、ＴＥＭ観察を行った結果、前記はんだ粉の粒子は、図３、図４に示すように、粒子表面に３０ｎｍ以下の微細粒子が存在している形態であることが分かった。このような形態は、他の実施例でも同様であった。
作製された粉の粒度分布と累積分布を図５、図６に示した。図５より平均粒径Ｄ５０は５５０ｎｍであることが分かった。
なお、本願では、はんだ粉試料０．３ｇをイソプロピルアルコール３０ｍＬに入れ、４５Ｗ超音波洗浄器にて５分間処理後、当該処理液に対しマイクロトラック９３２０−Ｘ１００（ハネウエル−日機装製）を用いて粒径測定した際の、累積５０質量％粒径（Ｄ５０）を銀粉の平均粒径とした。ここで、平均粒径Ｄ５０について説明する。測定対象であるはんだ粉全体の粒度分布が求められたとき、その銀紛全体積を１００％として累積カーブを求めたとき、その累積カーブが、例えば、１０％、５０％、９０％となる点の粒子径をそれぞれＤ１０、Ｄ５０、Ｄ９０と表記した。そして、累積中位径（Ｍｅｄｉａｎ径）であるＤ５０を、平均粒径としている。
As a result of SEM observation of the dried solder powder, a spherical powder was obtained as shown in FIGS. Further, as a result of TEM observation of the dried solder powder, the solder powder particles are in a form in which fine particles of 30 nm or less exist on the particle surface as shown in FIGS. 3 and 4. I understood that. Such a form was the same in other examples.
The particle size distribution and cumulative distribution of the produced powder are shown in FIGS. From FIG. 5, it was found that the average particle diameter D50 was 550 nm.
In the present application, 0.3 g of a solder powder sample is placed in 30 mL of isopropyl alcohol, treated with a 45 W ultrasonic cleaner for 5 minutes, and then treated with Microtrac 9320-X100 (Honeywell-Nikkiso Co., Ltd.). The cumulative 50% by mass particle diameter (D50) when the diameter was measured was defined as the average particle diameter of the silver powder. Here, the average particle diameter D50 will be described. When the particle size distribution of the entire solder powder to be measured is obtained, the cumulative curve is, for example, 10%, 50%, and 90% when the cumulative curve is obtained with the total volume of the silver powder as 100%. Were expressed as D10, D50, and D90, respectively. And D50 which is an accumulation median diameter (Median diameter) is made into the average particle diameter.
［実施例２］
粉砕用ボールの直径を１ｍｍから０．３ｍｍに変更した以外は、実施例１と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
[Example 2]
A dried solder powder was obtained and evaluated in the same manner as in Example 1 except that the diameter of the grinding ball was changed from 1 mm to 0.3 mm.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉について、ＳＥＭ観察を行った結果、図７に示すように球状の粉が得られた。前記乾燥済みはんだ粉の粒度分布と累積分布を図８、図９に示した。図７より平均粒径Ｄ５０は３６０ｎｍであることが分かった。 As a result of SEM observation of the dried solder powder, a spherical powder was obtained as shown in FIG. The particle size distribution and cumulative distribution of the dried solder powder are shown in FIGS. FIG. 7 shows that the average particle diameter D50 is 360 nm.
［実施例３］
非水系溶媒をテトラエチレングリコールからトリエチレングリコールに変更し、攪拌羽根の回転数を７００ｒｐｍから、表1に記載の６種類の回転数に変更して、６種類の乾燥済みはんだ粉を得た以外は、実施例２と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
[Example 3]
The non-aqueous solvent was changed from tetraethylene glycol to triethylene glycol, and the number of rotations of the stirring blade was changed from 700 rpm to the six types of rotations shown in Table 1 to obtain six types of dried solder powder. Were obtained by the same method as in Example 2 to obtain dried solder powder.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉平均粒径Ｄ５０を表１に示した。この結果より、攪拌速度（周速）を上げるとはんだ粉の微細化が進行して、攪拌羽根の周速と粒径の関係は図１０に示すようになった。 The dried solder powder average particle diameter D50 is shown in Table 1. From this result, when the stirring speed (peripheral speed) was increased, the refinement of the solder powder progressed, and the relationship between the peripheral speed of the stirring blade and the particle diameter became as shown in FIG.
［実施例４］
混合物の加熱温度を２３０℃から２３５℃に変更し、粉砕用ボールを分離する網を１５０メッシュのナイロン生地の網から、２００メッシュのナイロン生地の網に変更し、粉砕用ボールの直径を１ｍｍから、表２に記載の５種類の直径に変更して、５種類の乾燥済みはんだ粉を得た以外は、実施例１と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
[Example 4]
The heating temperature of the mixture was changed from 230 ° C. to 235 ° C., and the mesh for separating the grinding balls was changed from a mesh of 150 mesh nylon fabric to a mesh of 200 mesh nylon fabric, and the diameter of the grinding balls was changed from 1 mm. The dried solder powder was obtained and evaluated in the same manner as in Example 1 except that the five kinds of diameters shown in Table 2 were changed to obtain five kinds of dried solder powder.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉平均粒径Ｄ５０を表２に示した。この結果より、粉砕用ボールの直径を大きくすると得られたはんだ粉の粒径は大きくなり、粉砕用ボールの直径と得られたはんだ粉の平均粒径の関係は図１１に示すようになった。 The dried solder powder average particle diameter D50 is shown in Table 2. From this result, when the diameter of the grinding ball is increased, the particle size of the obtained solder powder is increased, and the relationship between the diameter of the grinding ball and the average particle size of the obtained solder powder is as shown in FIG. .
［実施例５］
粉砕用ボールの材質をジルコニアからアルミナに変更し、２３５℃での攪拌保持時間を１時間から３時間に変更し、使用したはんだ合金線の質量を表３に記載の１０種類の質量に変更して、１０種類の乾燥済みはんだ粉を得た以外は、実施例４と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
The material of the ball for grinding was changed from zirconia to alumina, the stirring and holding time at 235 ° C. was changed from 1 hour to 3 hours, and the mass of the solder alloy wire used was changed to the 10 types of mass shown in Table 3. The dried solder powder was obtained and evaluated in the same manner as in Example 4 except that 10 kinds of dried solder powder were obtained.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉平均粒径Ｄ５０を表３に示した。この結果より、原料金属（はんだ粉）の非水系溶媒に対する体積比が大きくなると得られるはんだ粉の粒径が大きくなることがわかった。原料金属（はんだ粉）の非水系溶媒に対する体積比と得られたはんだ粉の平均粒径の関係を図１２に示す。 The dried solder powder average particle diameter D50 is shown in Table 3. From this result, it was found that the particle size of the obtained solder powder increases as the volume ratio of the raw metal (solder powder) to the non-aqueous solvent increases. FIG. 12 shows the relationship between the volume ratio of the raw metal (solder powder) to the non-aqueous solvent and the average particle size of the obtained solder powder.
［実施例６］
Ｓｎ−Ｐｂ系はんだ粉の実施例を以下に説明する。
はんだ合金線の組成を、Ｓｎ９９質量％、Ａｇ０．３質量％、Ｃｕ０．７質量％から、Ｓｎ６０質量％、Ｐｂ４０質量％に変更し、使用するはんだ合金線の質量を５ｇの１種類のみとし、加熱・攪拌終了後の攪拌を停止する温度を１２０℃から９０℃に変更して、乾燥済みはんだ粉を得た以外は、実施例５と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
[Example 6]
Examples of Sn—Pb solder powder will be described below.
The composition of the solder alloy wire was changed from Sn 99 mass%, Ag 0.3 mass%, Cu 0.7 mass% to Sn 60 mass%, Pb 40 mass%, and the mass of the solder alloy wire to be used is only one type of 5 g, The dried solder powder was obtained in the same manner as in Example 5 except that the temperature at which stirring after heating / stirring was stopped was changed from 120 ° C. to 90 ° C. to obtain dried solder powder. I did it.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉の平均粒径Ｄ５０は６１０ｎｍであった。 The average particle diameter D50 of the dried solder powder was 610 nm.
［実施例７］
使用するはんだ合金線の組成を、Ｓｎ９９質量％、Ａｇ０．３質量％、Ｃｕ０．７質量％から、Ｓｎ９６．５質量％、Ａｇ３．０質量％、Ｃｕ０．５質量％に変更し、使用するはんだ合金線の質量を５ｇから１０ｇに変更し、テトラエチレングリコールの量を５０ｍＬから１００ｍＬに変更した以外は、実施例１と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
[Example 7]
The composition of the solder alloy wire used is changed from Sn 99 mass%, Ag 0.3 mass%, Cu 0.7 mass% to Sn 96.5 mass%, Ag 3.0 mass%, Cu 0.5 mass%, and used solder A dried solder powder was obtained and evaluated in the same manner as in Example 1 except that the mass of the alloy wire was changed from 5 g to 10 g and the amount of tetraethylene glycol was changed from 50 mL to 100 mL.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉について、ＳＥＭ観察を行った結果、はんだ粉の形状は球状であった。前記乾燥済みはんだ粉の平均粒径Ｄ５０は９００ｎｍであった。 As a result of SEM observation of the dried solder powder, the shape of the solder powder was spherical. The average particle diameter D50 of the dried solder powder was 900 nm.
［実施例８］
使用する金属原料を、Ｓｎ９６．５質量％、Ａｇ３．０質量％、Ｃｕ０．５質量％はんだ合金線から、Ｓｎ９９．９質量％、Ａｇ０．１質量％の合金に変更し、混合物の加熱温度を２３０℃から２３７℃に変更した以外は、実施例７と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
[Example 8]
The metal raw material to be used is changed from Sn 96.5 mass%, Ag 3.0 mass%, Cu 0.5 mass% solder alloy wire to an alloy of Sn 99.9 mass%, Ag 0.1 mass%, and the heating temperature of the mixture is changed. Except for changing from 230 ° C. to 237 ° C., dried solder powder was obtained in the same manner as in Example 7 and evaluated.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉について、ＳＥＭ観察を行った結果、はんだ粉の形状は球状であった。前記乾燥済みはんだ粉の平均粒径Ｄ５０は、９５０ｎｍであった。 As a result of SEM observation of the dried solder powder, the shape of the solder powder was spherical. The average particle diameter D50 of the dried solder powder was 950 nm.
［実施例９］
使用する金属原料を、Ｓｎ９６．５質量％、Ａｇ３．０質量％、Ｃｕ０．５質量％はんだ合金線から、Ｓｎ９４．０質量％、Ａｇ６．０質量％の合金に変更し、混合物の加熱温度を２３０℃から２４０℃に変更した以外は、実施例７と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
[Example 9]
The metal raw material to be used is changed from Sn 96.5% by mass, Ag 3.0% by mass, Cu 0.5% by mass solder alloy wire to Sn 94.0% by mass, Ag 6.0% by mass alloy, and the heating temperature of the mixture is changed. Except for changing from 230 ° C. to 240 ° C., dried solder powder was obtained in the same manner as in Example 7, and evaluated.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉について、ＳＥＭ観察を行った結果、はんだ粉の形状は球状であった。前記乾燥済みはんだ粉の平均粒径Ｄ５０は、９００ｎｍであった。 As a result of SEM observation of the dried solder powder, the shape of the solder powder was spherical. The average particle diameter D50 of the dried solder powder was 900 nm.
［実施例１０］
使用する金属原料を、Ｓｎ９６．５質量％、Ａｇ３．０質量％、Ｃｕ０．５質量％はんだ合金線から、Ｓｎ９３．０質量％、Ａｇ７．０質量％の合金に変更し、混合物の加熱温度を２３０℃から２４５℃に変更した以外は、実施例７と同様の方法で乾燥済みはんだ粉を得て、評価をおこなった。
[Example 10]
The metal raw material to be used is changed from Sn 96.5% by mass, Ag 3.0% by mass, Cu 0.5% by mass solder alloy wire to Sn 93.0% by mass, Ag 7.0% by mass alloy, and the heating temperature of the mixture is changed. Except for changing from 230 ° C. to 245 ° C., dried solder powder was obtained in the same manner as in Example 7, and evaluated.
前記乾燥済みのはんだ粉を、反射型のＦＴ−ＩＲでテトラエチレングリコールのヒドロキシ基のピークの有無について調べたが、前記ピークは認められなかった。 The dried solder powder was examined for the presence or absence of a hydroxy group peak of tetraethylene glycol by a reflective FT-IR, but the peak was not observed.
前記乾燥済みのはんだ粉について、ＳＥＭ観察を行った結果、はんだ粉の形状は球状であった。前記乾燥済みはんだ粉の平均粒径Ｄ５０は、９５０ｎｍであった。 As a result of SEM observation of the dried solder powder, the shape of the solder powder was spherical. The average particle diameter D50 of the dried solder powder was 950 nm.
本発明は、粒径が微細であるはんだ粉の製造方法に適用できる。 The present invention can be applied to a method for producing solder powder having a fine particle size.
Claims (12)
前記混合物を１５０℃以上であって、且つ得ようとするはんだ粉の合金組成物の融点より高い温度に加熱し、攪拌する工程と、
攪拌後の前記混合物から粉砕用ボールを分離して、はんだ粉と非水系溶媒の混合物を得る工程と、
前記はんだ粉と非水系溶媒の混合物を固液分離して、はんだ粉を得る工程を有し、
前記はんだ粉の平均粒径は０．０５μｍ以上、３μｍ未満である、はんだ粉の製造方法。 In a container, a solid or liquid metal, a non-aqueous solvent, and a pulverizing ball having a diameter of 0.05 mm to 5 mm to obtain a mixture;
Heating the mixture to a temperature higher than 150 ° C. and higher than the melting point of the alloy composition of the solder powder to be obtained, and stirring the mixture ;
Separating the grinding balls from the mixture after stirring to obtain a mixture of solder powder and a non-aqueous solvent;
Solid-liquid separation of the mixture of the solder powder and the non-aqueous solvent to obtain solder powder,
The solder powder has a mean particle size of 0.05 μm or more and less than 3 μm.
前記混合物を１５０℃以上であって、且つ得ようとするはんだ粉の合金組成物の融点より高い温度に加熱し、攪拌する工程と、
攪拌後の前記混合物から粉砕用ボールを分離して、はんだ粉と非水系溶媒の混合物を得る工程と、
前記はんだ粉と非水系溶媒の混合物を固液分離して、はんだ粉を得る工程を有し、
前記はんだ粉の平均粒径は０．０５μｍ以上、１μｍ未満である、はんだ粉の製造方法。 In a container, a solid or liquid metal, a non-aqueous solvent, and a pulverizing ball having a diameter of 0.05 mm to 5 mm to obtain a mixture;
Heating the mixture to a temperature higher than 150 ° C. and higher than the melting point of the alloy composition of the solder powder to be obtained, and stirring the mixture ;
Separating the grinding balls from the mixture after stirring to obtain a mixture of solder powder and a non-aqueous solvent;
Solid-liquid separation of the mixture of the solder powder and the non-aqueous solvent to obtain solder powder,
The solder powder has a mean particle size of 0.05 μm or more and less than 1 μm.
前記混合物を１５０℃以上であって、且つ得ようとするはんだ粉の合金組成物の融点より高い温度に加熱し、攪拌する工程と、
攪拌後の前記混合物から粉砕用ボールを分離して、はんだ粉と非水系溶媒の混合物を得る工程と、
前記はんだ粉と非水系溶媒の混合物を固液分離して、はんだ粉を得る工程を有し、
前記はんだ粉の平均粒径は０．０５μｍ以上、０．７μｍ未満である、はんだ粉の製造方法。 In a container, a solid or liquid metal, a non-aqueous solvent, and a pulverizing ball having a diameter of 0.05 mm to 5 mm to obtain a mixture;
Heating and stirring the mixture to a temperature higher than 150 ° C. and higher than the melting point of the alloy composition of the solder powder to be obtained; and
Separating the grinding balls from the mixture after stirring to obtain a mixture of solder powder and a non-aqueous solvent;
Solid-liquid separation of the mixture of the solder powder and the non-aqueous solvent to obtain solder powder,
The solder powder has a mean particle size of 0.05 μm or more and less than 0.7 μm.
The method for producing solder powder according to claim 1, wherein the volume of the metal is 0.1% by volume to 20% by volume of the volume of the non-aqueous solvent.
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