JP2020055037A - 鉛フリーはんだフラックス、鉛フリーソルダペースト - Google Patents
鉛フリーはんだフラックス、鉛フリーソルダペースト Download PDFInfo
- Publication number
- JP2020055037A JP2020055037A JP2019172552A JP2019172552A JP2020055037A JP 2020055037 A JP2020055037 A JP 2020055037A JP 2019172552 A JP2019172552 A JP 2019172552A JP 2019172552 A JP2019172552 A JP 2019172552A JP 2020055037 A JP2020055037 A JP 2020055037A
- Authority
- JP
- Japan
- Prior art keywords
- component
- lead
- free solder
- acid
- rosin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910000679 solder Inorganic materials 0.000 title claims abstract description 96
- 230000004907 flux Effects 0.000 title claims abstract description 51
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 45
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 45
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000009835 boiling Methods 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 239000012190 activator Substances 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 125000003118 aryl group Chemical group 0.000 claims abstract description 8
- 150000001408 amides Chemical class 0.000 claims abstract description 6
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 12
- GZMAAYIALGURDQ-UHFFFAOYSA-N 2-(2-hexoxyethoxy)ethanol Chemical compound CCCCCCOCCOCCO GZMAAYIALGURDQ-UHFFFAOYSA-N 0.000 claims description 7
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 claims description 7
- 229960005323 phenoxyethanol Drugs 0.000 claims description 7
- ZUAURMBNZUCEAF-UHFFFAOYSA-N 2-(2-phenoxyethoxy)ethanol Chemical compound OCCOCCOC1=CC=CC=C1 ZUAURMBNZUCEAF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052736 halogen Inorganic materials 0.000 claims description 6
- 150000002367 halogens Chemical class 0.000 claims description 6
- WAEVWDZKMBQDEJ-UHFFFAOYSA-N 2-[2-(2-methoxypropoxy)propoxy]propan-1-ol Chemical compound COC(C)COC(C)COC(C)CO WAEVWDZKMBQDEJ-UHFFFAOYSA-N 0.000 claims description 5
- IBLKWZIFZMJLFL-UHFFFAOYSA-N 1-phenoxypropan-2-ol Chemical compound CC(O)COC1=CC=CC=C1 IBLKWZIFZMJLFL-UHFFFAOYSA-N 0.000 claims description 4
- 238000003860 storage Methods 0.000 abstract description 17
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- -1 maleated rosin Natural products 0.000 description 17
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 9
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- 238000002360 preparation method Methods 0.000 description 7
- 230000008719 thickening Effects 0.000 description 7
- RTWNYYOXLSILQN-UHFFFAOYSA-N methanediamine Chemical compound NCN RTWNYYOXLSILQN-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 125000005907 alkyl ester group Chemical group 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 239000003963 antioxidant agent Substances 0.000 description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 4
- JGHSBPIZNUXPLA-UHFFFAOYSA-N 2-hydroxyhexadecanoic acid Chemical compound CCCCCCCCCCCCCCC(O)C(O)=O JGHSBPIZNUXPLA-UHFFFAOYSA-N 0.000 description 3
- JYZJYKOZGGEXSX-UHFFFAOYSA-N 2-hydroxymyristic acid Chemical compound CCCCCCCCCCCCC(O)C(O)=O JYZJYKOZGGEXSX-UHFFFAOYSA-N 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 150000004678 hydrides Chemical class 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- ARXKVVRQIIOZGF-UHFFFAOYSA-N 1,2,4-butanetriol Chemical compound OCCC(O)CO ARXKVVRQIIOZGF-UHFFFAOYSA-N 0.000 description 2
- SHKKTLSDGJRCTR-UHFFFAOYSA-N 1,2-dibromoethylbenzene Chemical compound BrCC(Br)C1=CC=CC=C1 SHKKTLSDGJRCTR-UHFFFAOYSA-N 0.000 description 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 2
- CHUGKEQJSLOLHL-UHFFFAOYSA-N 2,2-Bis(bromomethyl)propane-1,3-diol Chemical compound OCC(CO)(CBr)CBr CHUGKEQJSLOLHL-UHFFFAOYSA-N 0.000 description 2
- FJWGRXKOBIVTFA-UHFFFAOYSA-N 2,3-dibromobutanedioic acid Chemical compound OC(=O)C(Br)C(Br)C(O)=O FJWGRXKOBIVTFA-UHFFFAOYSA-N 0.000 description 2
- KIHBGTRZFAVZRV-UHFFFAOYSA-N 2-Hydroxyoctadecanoic acid Natural products CCCCCCCCCCCCCCCCC(O)C(O)=O KIHBGTRZFAVZRV-UHFFFAOYSA-N 0.000 description 2
- OADIZUFHUPTFAG-UHFFFAOYSA-N 2-[2-(2-ethylhexoxy)ethoxy]ethanol Chemical compound CCCCC(CC)COCCOCCO OADIZUFHUPTFAG-UHFFFAOYSA-N 0.000 description 2
- WMFATTFQNRPXBQ-UHFFFAOYSA-N 2-bromopentanoic acid Chemical compound CCCC(Br)C(O)=O WMFATTFQNRPXBQ-UHFFFAOYSA-N 0.000 description 2
- SMNDYUVBFMFKNZ-UHFFFAOYSA-N 2-furoic acid Chemical compound OC(=O)C1=CC=CO1 SMNDYUVBFMFKNZ-UHFFFAOYSA-N 0.000 description 2
- YDZIJQXINJLRLL-UHFFFAOYSA-N 2-hydroxydodecanoic acid Chemical compound CCCCCCCCCCC(O)C(O)=O YDZIJQXINJLRLL-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000005639 Lauric acid Substances 0.000 description 2
- 235000021314 Palmitic acid Nutrition 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- XGSQVNLLKDVOAZ-UHFFFAOYSA-N bromic acid;n-ethylethanamine Chemical compound OBr(=O)=O.CCNCC XGSQVNLLKDVOAZ-UHFFFAOYSA-N 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- XSIFPSYPOVKYCO-UHFFFAOYSA-N butyl benzoate Chemical compound CCCCOC(=O)C1=CC=CC=C1 XSIFPSYPOVKYCO-UHFFFAOYSA-N 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 239000004359 castor oil Substances 0.000 description 2
- 235000019438 castor oil Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 239000000539 dimer Substances 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- WJJMNDUMQPNECX-UHFFFAOYSA-N dipicolinic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=N1 WJJMNDUMQPNECX-UHFFFAOYSA-N 0.000 description 2
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- CHTHALBTIRVDBM-UHFFFAOYSA-N furan-2,5-dicarboxylic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)O1 CHTHALBTIRVDBM-UHFFFAOYSA-N 0.000 description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 2
- 150000002366 halogen compounds Chemical class 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
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- 239000002530 phenolic antioxidant Substances 0.000 description 2
- JLUIOEOHOOLSJC-UHFFFAOYSA-N pyrrole-2,5-dicarboxylic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)N1 JLUIOEOHOOLSJC-UHFFFAOYSA-N 0.000 description 2
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- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 2
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
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- 150000004820 halides Chemical class 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
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- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- CLZGJKHEVKJLLS-UHFFFAOYSA-N n,n-diheptylheptan-1-amine Chemical compound CCCCCCCN(CCCCCCC)CCCCCCC CLZGJKHEVKJLLS-UHFFFAOYSA-N 0.000 description 1
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- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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Landscapes
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
Description
(C)成分が、融点160〜220℃であるアミドを含み、
(D)成分が、沸点220〜310℃の芳香環を有する溶剤(D1)及び沸点220〜280℃の芳香環を有さない溶剤(D2)を含む、鉛フリーはんだフラックス。
(1)ヒドロキシル基を有するカルボン酸及び第1級ジアミンを反応させる。
(2)ヒドロキシル基を有するカルボン酸のアルキルエステル及び第1級ジアミンを反応させる。
(3)ヒドロキシル基を有するカルボン酸、及びヒドロキシル基を有するカルボン酸のアルキルエステルの混合物、並びに第1級ジアミンを反応させる。
(4)ヒドロキシル基を有するカルボン酸のハライド及び第1級ジアミンを反応させる。
水素化ロジン21質量%(商品名「KE−614」、荒川化学工業(株)製)、水素化アクリル化ロジン(商品名「KE−604」、荒川化学工業(株)製)を21質量%、アジピン酸(東京化成工業(株)製)を2質量%、ジエチルアミン臭素酸塩を1質量%、ジアミド(商品名「ITOHWAX JHー180」、融点:184℃、伊藤製油(株)製)を5質量%、エチレングリコールモノフェニルエーテル(沸点:237℃)を25質量%及びジエチレングリコールモノヘキシルエーテル(沸点:263℃)を25質量%となるように混合し、加熱下で溶融させ、はんだフラックスを調製した。組成を表1に示す(以下同様)。
表1に示す組成に変更した他は、実施例1と同様にして鉛フリーはんだフラックスをそれぞれ調製した。
実施例1のはんだフラックスと市販の無鉛はんだ粉末(96.5Sn/3Ag/0.5Cu、三井金属(株)製、粒径20〜38μm、通常品)とを順に11質量%及び89質量%となるようソフナーで混練し、ソルダペーストを調製した。他の実施例及び比較例のはんだフラックスについても同様にしてソルダペーストを調製した。
各ソルダペーストについて、調製直後の粘度と、40℃の恒温槽中で24時間保温した後の粘度とを、それぞれ市販のスパイラル方式粘度計(製品名「PCU−205」、共軸二重円筒形回転型、(株)マルコム製)を用いて、予め温度25℃に調整したソルダペーストを回転数10rpmで測定し、以下の(式1)に基づき、増粘率(%)を算出した。増粘率が10%未満の場合、保存安定性が良好であることを示す。
各ソルダペーストについて、調製直後の粘度を測定した。次に連続印刷機(装置名「半自動スクリーン印刷機ミノマット ハンター Y−3540−CH」、(株)ミノグループ製)を用いて、スキージ速度30mm/秒、スキージストローク300mm、スキージタクト30秒及び温度25℃にて、前記ソルダペーストを12時間連続印刷した後の粘度を測定した。なお、粘度は市販のスパイラル方式粘度計(製品名「PCU−205」、共軸二重円筒形回転型、(株)マルコム製)を用いて、予め温度25℃に調整したソルダペーストを回転数10rpmで測定し、以下の(式2)に基づき、増粘率(%)を算出した。増粘率が10%未満の場合、保存安定性が良好であることを示す。
各ソルダペーストを厚み150μmのステンシルを用いて評価基板上の4532チップ抵抗パターンに印刷し、4532チップ抵抗10個をチップマウンターで搭載した後、酸素濃度約1000ppm雰囲気下において、図1に示すリフロー温度プロファイルに従って、リフローした。その後、4532チップ抵抗の長辺に隣接するサイドボールの発生の程度を目視観察し、以下の基準で評価した。
◎:サイドボールの数が5個以下
○:サイドボールの数が6個以上10個以下
△:サイドボールの数が11個以上15個以下
×:サイドボールの数が16個以上
・KE−614:商品名「KE−614」、水素化ロジン、荒川化学工業(株)製
・KE−604:商品名「KE−604」、水素化アクリル化ロジン、荒川化学工業(株)製
・KR−120:商品名「KR−120」、不均化ロジン、荒川化学工業(株)製
<チキソ剤>
・JH−180:商品名「ITOHWAX JH−180」、融点:184℃、伊藤製油(株)製
・JH−170:商品名「ITOHWAX JH−170」、融点:174℃、伊藤製油(株)製
・J−630:商品名「ITOHWAX J−630」、N,N’−ヘキサメチレン−ビス−12−ヒドロキシステアリルアミド、融点:135℃、伊藤製油(株)製
・MA−WAX−O:商品名「MA−WAX−O」、12−ヒドロキシステアリン酸エチレンビスアミド、融点:140℃、KFトレーディング(株)製
・HCO−P:商品名「硬化ひまし油 HCO−P」、硬化ひまし油、融点85℃、豊国製油(株)製
<溶剤>
・PhG :エチレングリコールモノフェニルエーテル(沸点:237℃)
・PhDG:ジエチレングリコールモノフェニルエーテル(沸点:298℃)
・HeDG:ジエチレングリコールモノn−ヘキシルエーテル(沸点:263℃)
・MFTG:トリプロピレングリコールモノメチルエーテル(沸点:243℃)
・HeG:エチレングリコールモノn−ヘキシルエーテル(沸点:205℃)
Claims (8)
- 重合ロジンを含まないロジン系樹脂(A)、活性剤(B)、チキソ剤(C)及び溶剤(D)を含み、
(C)成分が、融点160〜220℃であるアミドを含み、
(D)成分が、沸点220〜310℃の芳香環を有する溶剤(D1)及び沸点220〜280℃の芳香環を有さない溶剤(D2)を含む、鉛フリーはんだフラックス。 - (A)成分が、水素化ロジン、不均化ロジン及び水素化アクリル化ロジンからなる群より選ばれる少なくとも1種を含む、請求項1に記載の鉛フリーはんだフラックス。
- (B)成分が、非ハロゲン系酸活性剤(B1)及び/又はハロゲン系活性剤(B2)を含む請求項1又は2に記載の鉛フリーはんだフラックス。
- (C)成分が、ヒドロキシル基を有する請求項1〜3のいずれかに記載の鉛フリーはんだフラックス。
- (C)成分の含有量が、全フラックス成分100質量%に対して、1〜15質量%である請求項1〜4のいずれかに記載の鉛フリーはんだフラックス。
- (D1)成分が、エチレングリコールモノフェニルエーテル、ジエチレングリコールモノフェニルエーテル及びプロピレングリコールモノフェニルエーテルから選ばれる少なくとも1種を含む、請求項1〜5のいずれかに記載の鉛フリーはんだフラックス。
- (D2)成分が、ジエチレングリコールモノヘキシルエーテル及び/又はトリプロピレングリコールモノメチルエーテルを含む、請求項1〜6のいずれかに記載の鉛フリーはんだフラックス。
- 請求項1〜7のいずれかに記載のはんだフラックス及びはんだ粉末を含む鉛フリーソルダペースト。
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