CN1817508A - 制备精细焊粉的方法 - Google Patents
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Abstract
一种在生产精细焊粉时精炼和均匀分散合金成分以及除去软焊料中或来自软焊料的不希望的反应产物如氧化物和/或熔渣的方法,在所述方法中,将焊料合金要在耐高温的植物油和/或动物油中熔融,然后将熔体放置于温度高于液相线温度至少20℃的另一预置油中,在那里进行搅拌,并通过转子和定子对其进行多次剪切处理以形成由焊珠和油组成的分散体,借助后续的沉淀作用从分散体中分离出焊珠。
Description
本发明涉及一种在生产精细焊粉时精炼和均匀分散合金成分以及除去软焊料中或来自软焊料的不希望的反应产物如氧化物和/或熔渣的方法,在所述方法中,焊料合金要在耐高温的植物油和/或动物油中熔融,然后将熔体送入温度高于液相线温度至少20℃的另一预置油中,在那里进行搅拌,并通过转子和定子对其进行多次剪切处理以形成由焊珠和油组成的分散体,借助后续的沉淀作用从分散体中分离出焊珠。
在DE10161826A1中公开了一种无铅的锡-银-铜基焊料合金的软焊料,其中,在含有5至20重量%银、0.8至1.2重量%铜、余量为锡和常规杂质的基础合金中还总掺合有0.8至1.2重量%的铟和0.01至0.2重量%的一种镧系元素,例如镧或钕。
这种已知的不含铅的软焊料从214℃开始是低共熔的,会抑制大的锡的树枝状晶体(zinn dentrid)的生成,保证在熔融后能形成平滑且均质的表面,并且还具有良好的物理和化学性能,例如非常良好的润湿能力、高的交变应力疲劳强度、良好的耐腐蚀性、塑性和韧性以及微小的电阻性。
但是,合金的熔融和将这种已知合金加工成精细焊珠的过程特别会由于合金组分镧或钕的高反应性而导致非常严峻的问题,即在焊珠中会出现钕或镧的反应产物的团聚。钕的反应极其剧烈,例如它还会与总是以痕量存在于熔体中的结合的残余氧反应,并生成在焊珠中还能团聚成更大形成物的氧化物。这些氧化物积聚了相对较多的钕,从而使得后来这些钕在基体或晶界中缺乏。另外还可能产生组成为Ag3Sn和Cu6Sn5的金属间相。
这种软焊料的加工能力和电性能会由于这些硬的夹杂物而持久地受到限制。
在DE19830057C2中也公开了一种用于无压生产晶粒带谱(Kornbandspektrum)为1至100μm的软焊粉的方法,该方法中要使金属焊料在耐高温的植物油或动物油中熔融,接着进行搅拌并在多次的通过转子和定子的剪切处理过程中将其分散成特定大小的焊珠。
根据US5411602A的教导,熔融焊料并利用惰性气体将熔融的焊料打散成小滴。尽管是在惰性气体气氛中,但仍然不能排除活性金属如钕或镧会与结合氧反应,从而使得焊料合金中或多或少地含有这些金属的氧化物,并且例如添加的钕或镧也会或多或少地损失掉。
在US6231691B1中记载了一种无铅的锡基焊料合金,其含有4.7重量%的银、1.7重量%的铜和0.15重量%的镍。所公开的合金有生成Cu3Sn和/或Cu6Sn5型的金属间相的强烈倾向,而这会对焊接点的机械/物理性能造成非常负面的影响。
鉴于这些现有技术,本发明的任务在于在将无铅的软焊料合金加工成精细焊粉的过程中,要可靠地防止活性合金成分与氧、氮和其他反应物的反应,避免焊珠基体中发生反应产物的团聚,并且要将合金成分精细且均匀地分散于焊珠基体中。
该任务可通过一种具有权利要求1,10和11所述特征的文端所述类型的方法来解决。
该方法的优选方案可在从属权利要求中获知。
本发明的解决方案的特征在于,用于熔融焊料的油既是一种在软焊料合金中相对于合金成分如镧或钕呈惰性的介质,还是一种能够将焊料合金中所含的反应产物如氧化物和/或熔渣溶出的分离介质。
本发明的方法还允许将焊料合金中的合金成分进行一定程度上的精炼,并使其均匀且精细地分散在合金中。简明地说,这些过程的复杂的难点即在于要使剪切下的焊珠本身具有非常接近于那些元素的结构构成的尺寸。
通过在熔融过程中或在对这些焊料进行加工以制备精细焊粉中形成的镧系元素或其他活性金属的氧化物夹杂物以及有害熔渣的溶出能成功地制得满足所有微接触方面的要求的精细焊粉。
其他优点和细节将由以下说明书内容并结合附图来阐述。
以下将利用一个实施例来详尽阐述本发明。
附图为:
图1为现有技术中具有氧化钕夹杂物的无铅焊料合金的REM照片(影像),
图2为如图1的具有氧分布的REM照片(影像),
图3a和b为如图1的、具有细成为Ag3Sn和Cu6Sn5的金属间相的无铅焊料合金的REM照片,
图4a至f为根据本发明制得的且在焊珠中分布有合金组分(银、锡、铜、铟、钕和氧)的焊珠的REM照片。
利用本发明的方法可制得直径为5至15μm的无铅合金SnAg5Cu1In1Nd0.2的精细焊珠(6型)。
图1,2,3a和3b显示的是根据现有技术的无铅焊料合金的初始状态,从中可以很明显地辨认出由氧化钕(图1)以及金属间相Ag3Sn和Cu6Sn5(图3a和3b)组成的夹杂物。在图2中显示了合金中的氧分布情况,其提供了该夹杂物为氧化物(Nd2O3)的证据。该氧化物夹杂物具有2272℃的熔点和7.29g/cm3的密度,并且是坚硬、不可延展和易碎的。此外,氧化物还积聚了相对较多的元素钕,从而使得晶界中缺少钕,并因此由于开裂和开裂的快速生长而对焊点的温度交变应力疲劳强度产生不利影响。
接着,这些夹杂物会在焊接点中导致断裂和电性能的不均匀,从而使得这种焊料不再特别适合用于微接触。
图4a至4f所示为焊珠中无铅软焊料合金的合金成分锡、银、铜、铟和钕的分布情况,所述焊珠是根据本发明方法制得的。
为此,将12kg的块状或棒状无铅焊料合金SnAg5Cu1In1Nd0.2加入到装有3升蓖麻油的熔融容器中,并加热油至高于焊料合金的液相线温度至少20℃,例如240℃,以便熔融焊料合金。这种油能使焊料绝氧并完全隔绝焊料熔体与空气接触。在熔融时,焊料熔体中会释放出氧化钕。而它们又会由于具有低于熔体的密度而在油中浮起,并在那里于2小时内富集起来直至达到设备的操作温度。因此,所述的油不仅起到热载体和分散剂的作用,而且还起到分离介质的作用。
余下的焊料熔体会通过喷嘴体系而排放到另一由蓖麻油组成的预置油中,并从析出的杂质中分离出来。所述油的温度同样要高于焊料合金的液相线温度至少20℃。焊料熔体到达分散反应器中,在该反应器中,通过以23m/s的定子圆周速度运转的转子对焊料熔体进行剪切处理,从而将焊料熔体分割成小焊珠,由此,能将熔体的表面积扩展到2500倍大并释放出其中一直所包含着的杂质。然后,使分割下的焊珠与油一起多次,即至少20次循环通过分散反应器,直至焊珠达到理想的直径分布并且其余杂质也同时从焊料熔体中排出。在焊料的分散过程中,焊料与油的体积比为1∶20至1∶50,分散时间为16分钟。
在这段时间之后,将分散的焊珠-油混合物加入沉淀容器中,在该容器中,剪切下的焊珠会在油中硬化并沉淀。在分散过程中析出的杂质会由于其密度小于焊料而在油中积聚起来。将油和杂质抽走,从而将其与焊珠分离。
图4a显示的是根据本发明方法制得的焊珠的基体中钕的分布情况。从图4a中可以看到,钕的分布均匀而规则。不再存在有氧化钕或熔渣组成的粗夹杂物。金属间相变小了且分布均匀。同样,所有其他合金成分也都均匀分布在珠体体积中,从而能够得到最佳的焊料性质。
Claims (11)
1.一种在生产精细焊粉时精炼和均匀分散合金成分以及除去软焊料中或来自软焊料的不希望的反应产物如氧化物和/或熔渣的方法,在所述方法中,将焊料合金要在耐高温的植物油和/或动物油中熔融,然后将熔体送入温度高于液相线温度至少20℃的另一预置油中,在那里进行搅拌,并通过转子和定子对其进行多次剪切处理以形成由焊珠和油组成的分散体,借助后续的沉淀作用从分散体中分离出焊珠,其物征于以下步骤:
a)将油用作熔体和反应产物和/或熔渣的分离介质以及在焊料熔融时释放出反应产物和/或熔渣,
b)由于步骤a)中的熔体和反应产物和/或熔渣之间存在密度差,使释放出的反应产物和/或熔渣富集在油中,
c)通过将熔体排放到在高于液相线温度至少20℃的温度下的另一预置油中而分离含有反应产物和/或熔渣的油,并抽去含有反应产物和/或熔渣的油,
d)在以15.0至25m/s的定子圆周速度进行剪切,并保持熔体与油之间的体积比为1∶20至1∶50的条件下,通过增大焊料熔体的表面积而排出仍然存在于焊料熔体内部的反应产物和/或熔渣,
e)在剪切时从焊料熔体内部排出的反应产物和/或熔渣如步骤b)那样由于密度差而富集在油中,
f)在10至30分钟的循环时间段内湍流混合留下的焊料熔体,以使合金成分在焊料中均匀分布,
g)在焊珠沉淀后,与油一起分离步骤c)和e)的经富集的反应产物和/或熔渣。
2.如权利要求1所述的方法,其特征在于,所用的软焊料是一种基本上由Sn、Ag、Cu、In和镧系元素以及镧系元素的反应产物组成的合金。
3.如权利要求1或2所述的方法,其特征在于,所用的软焊料是一种基本上由Sn、Ag、Cu、In和Nd以及氧化钕和/或Ag3Sn和Cu6Sn5型金属间相形式的反应产物组成的合金。
4.如权利要求1所述的方法,其特征在于,所用的软焊料是一种基本上由Sn、Ag、Cu和Ni以及Cu3Sn和/或Cu6Sn5型金属间相形式的反应产物组成的合金。
5.如权利要求1所述的方法,其特征在于,所用的软焊料是一种基本上由Sn和Ag以及Ag3Sn型金属间相形式的反应产物组成的合金。
6.如权利要求1所述的方法,其特征在于,所用的软焊料是一种基本上由Sn和Cu以及Cu3Sn和/或Cu6Sn5型金属间相形式的反应产物组成的合金。
7.如权利要求1至6所述的方法,其特征在于,所制得的精细焊粉具有2.5至45μm的直径。
8.如权利要求1至7所述的方法,其特征在于,通过剪切将焊料熔体的表面积扩增到2000至4000倍。
9.如权利要求1至8所述的方法,其特征在于,使用蓖麻油作为分离油。
10.动物油和/或植物油,优选蓖麻油的用途,所述用途为用于精炼和均匀分散软焊料中的合金成分,以制备直径在2.5至45μm之间的精细焊粉。
11.动物油和/或植物油,优选蓖麻油的用途,所述用途为用于从软焊料中分离出反应产物如氧化物和/或熔渣,以制备直径在2.5至45μm之间的精细焊粉。
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Application Number | Priority Date | Filing Date | Title |
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DE102004038280A DE102004038280B4 (de) | 2004-08-03 | 2004-08-03 | Verfahren zum Herstellen von Feinstlotpulvern |
DE102004038280.8 | 2004-08-03 |
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Publication Number | Publication Date |
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CN1817508A true CN1817508A (zh) | 2006-08-16 |
CN100574940C CN100574940C (zh) | 2009-12-30 |
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CN200510023009A Active CN100574940C (zh) | 2004-08-03 | 2005-08-03 | 制备精细焊粉的方法 |
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US (1) | US7331498B2 (zh) |
EP (1) | EP1623791B1 (zh) |
JP (1) | JP2006045676A (zh) |
KR (1) | KR101243283B1 (zh) |
CN (1) | CN100574940C (zh) |
AT (1) | ATE445478T1 (zh) |
DE (2) | DE102004038280B4 (zh) |
DK (1) | DK1623791T3 (zh) |
ES (1) | ES2332918T3 (zh) |
PL (1) | PL1623791T3 (zh) |
PT (1) | PT1623791E (zh) |
SI (1) | SI1623791T1 (zh) |
TW (1) | TW200609072A (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104178655A (zh) * | 2013-05-21 | 2014-12-03 | 西南科技大学 | 一种含稀土La的中温合金钎料及其制备方法 |
CN106271216A (zh) * | 2016-08-31 | 2017-01-04 | 邓柳平 | 一种不吸潮焊粉及其制备方法 |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
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TWI465312B (zh) * | 2005-07-19 | 2014-12-21 | Nihon Superior Co Ltd | 追加供應用無鉛焊料及焊浴中之Cu濃度及Ni濃度之調整方法 |
DE102006047764A1 (de) * | 2006-10-06 | 2008-04-10 | W.C. Heraeus Gmbh | Bleifreies Weichlot mit verbesserten Eigenschaften bei Temperaturen >150°C |
DE202006015429U1 (de) * | 2006-10-09 | 2008-02-21 | Innowatec Dipl.-Ing. Grieger & Englert Gmbh & Co. Kg | Vorrichtung zum Reinigen eines Druckzylinders |
JP4375485B2 (ja) * | 2008-02-22 | 2009-12-02 | 日本ジョイント株式会社 | 鉛フリーはんだ合金の製造方法及び半導体装置の製造方法 |
JP4375491B1 (ja) * | 2008-06-23 | 2009-12-02 | 日本ジョイント株式会社 | 電子部品のはんだ付け装置およびはんだ付け方法 |
WO2010089905A1 (ja) * | 2009-02-09 | 2010-08-12 | 日本ジョイント株式会社 | 電子部品用錫またははんだ合金の製造方法、製造装置、及びはんだ合金 |
JP4485604B1 (ja) * | 2009-02-09 | 2010-06-23 | 日本ジョイント株式会社 | 電子部品用錫またははんだ合金の製造方法、製造装置、及びはんだ合金 |
CN103221164B (zh) | 2010-11-18 | 2016-06-15 | 同和控股(集团)有限公司 | 焊料粉末以及焊料粉末的制造方法 |
CN107442965A (zh) * | 2017-08-11 | 2017-12-08 | 东北大学 | 一种Sn‑Bi系合金焊粉及其制备方法 |
Family Cites Families (9)
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SE8801894D0 (sv) * | 1988-05-20 | 1988-05-20 | Alfa Laval Agri Int | Fibronektinbindande protein |
JP2555715B2 (ja) * | 1988-10-26 | 1996-11-20 | 三菱マテリアル株式会社 | はんだ合金微粉末の製造方法 |
US5411602A (en) | 1994-02-17 | 1995-05-02 | Microfab Technologies, Inc. | Solder compositions and methods of making same |
US6231691B1 (en) * | 1997-02-10 | 2001-05-15 | Iowa State University Research Foundation, Inc. | Lead-free solder |
DE19830057C1 (de) * | 1998-06-29 | 2000-03-16 | Juergen Schulze | Verfahren und Vorrichtung zum drucklosen Herstellen von Weichlotpulver |
US6517602B2 (en) * | 2000-03-14 | 2003-02-11 | Hitachi Metals, Ltd | Solder ball and method for producing same |
JP2003166007A (ja) * | 2001-03-28 | 2003-06-13 | Tamura Kaken Co Ltd | 金属微粒子の製造方法、金属微粒子含有物及びソルダーペースト組成物 |
JP2005512813A (ja) | 2001-12-15 | 2005-05-12 | プファル・シュタンツテヒニク・ゲゼルシャフト・ミト・ベシュレンクテル・ハフツング | 無鉛ソフトハンダ |
JP2003268418A (ja) * | 2002-03-19 | 2003-09-25 | Tamura Kaken Co Ltd | 金属粉末の製造方法 |
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2004
- 2004-08-03 DE DE102004038280A patent/DE102004038280B4/de not_active Expired - Fee Related
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- 2005-07-21 TW TW094124734A patent/TW200609072A/zh unknown
- 2005-07-27 DE DE502005008305T patent/DE502005008305D1/de active Active
- 2005-07-27 AT AT05076782T patent/ATE445478T1/de active
- 2005-07-27 ES ES05076782T patent/ES2332918T3/es active Active
- 2005-07-27 SI SI200530849T patent/SI1623791T1/sl unknown
- 2005-07-27 PT PT05076782T patent/PT1623791E/pt unknown
- 2005-07-27 PL PL05076782T patent/PL1623791T3/pl unknown
- 2005-07-27 DK DK05076782.1T patent/DK1623791T3/da active
- 2005-07-27 EP EP05076782A patent/EP1623791B1/de active Active
- 2005-07-28 US US11/193,758 patent/US7331498B2/en active Active
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104178655A (zh) * | 2013-05-21 | 2014-12-03 | 西南科技大学 | 一种含稀土La的中温合金钎料及其制备方法 |
CN106271216A (zh) * | 2016-08-31 | 2017-01-04 | 邓柳平 | 一种不吸潮焊粉及其制备方法 |
Also Published As
Publication number | Publication date |
---|---|
DE502005008305D1 (de) | 2009-11-26 |
DK1623791T3 (da) | 2010-03-01 |
EP1623791B1 (de) | 2009-10-14 |
JP2006045676A (ja) | 2006-02-16 |
EP1623791A2 (de) | 2006-02-08 |
US7331498B2 (en) | 2008-02-19 |
SI1623791T1 (sl) | 2010-02-26 |
ES2332918T3 (es) | 2010-02-15 |
DE102004038280A1 (de) | 2006-02-23 |
PL1623791T3 (pl) | 2010-06-30 |
TWI317671B (zh) | 2009-12-01 |
PT1623791E (pt) | 2009-12-29 |
KR101243283B1 (ko) | 2013-03-13 |
DE102004038280B4 (de) | 2006-07-27 |
CN100574940C (zh) | 2009-12-30 |
KR20060049046A (ko) | 2006-05-18 |
ATE445478T1 (de) | 2009-10-15 |
US20060208042A1 (en) | 2006-09-21 |
EP1623791A3 (de) | 2007-08-22 |
TW200609072A (en) | 2006-03-16 |
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