CN1670246A - 保持金属化熔池的方法 - Google Patents
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Abstract
本发明涉及一种方法，用于再生用于无电流金属化的含有锌、镍的碱性无氰化物电解熔池。依据本发明的方法包括以下步骤：将至少一个电解质分流从过程容器导入再生单元，再生导出的电解质分流并将再生的电解质分流回输到过程容器内，其中，再生单元具有带阴离子选择膜的渗析和/或电渗析单元，里面无电流金属化过程中产生的阴离子与氢氧根交换。这样再生的电解质流所消耗的成分可以得到补充。
Description
技术领域
本发明涉及一种用于保持电镀技术中金属化熔池的方法。本发明特别是涉及用于在金属的无电流沉积时保持金属化熔池的方法。
背景技术
在例如像铜从相应的电解质中无外电流化学沉积这种金属的无外电流沉积中，为电解质添加一种还原剂，它可以作为内部电源使金属沉积。
这里以铜电解质为例介绍无外电流金属沉积的基本原理。
用于无外电流化学沉积铜的电解质一般含有例如像铜酒石酸盐络合物或者铜-EDTA-螯合物这种络合或螯合结合的铜离子。作为还原剂一般使用甲醛或者可比较的还原剂，这种还原剂因为氧化还原成甲酸盐或相应的阴离子提供铜还原所需的电子。
但是，甲醛只有在约pH11～pH14的高碱性pH-范围内，才能对一般在电解质中用于无外电流沉积铜所使用的二价铜离子起到足够强的还原剂的作用并可以使金属沉积。由此造成铜离子如此强地络合或者螯合存在于该电解质中，从而它们不能形成难溶解的金属氢氧化物。
此外，铜一般以硫酸盐的方式加入电解质中。作为二价铜离子反应成元素铜的后果是增加电解质的硫酸根。硫酸根在与通过甲醛氧化引起的甲酸根浓度提高结合下的这种增加导致pH-值下降。为将电解质保持在具有工作能力的pH-范围内，为这种碱金属氢氧化物添加如氢氧化钠。此外，为该电解质补充消耗量的硫酸铜和甲醛。根据前面所述，因此改变了电解质的化学和物理特性，从而导致同一电解质有限的可保持性和可应用性。
无电流镍熔池大多在酸性pH-范围内工作。借助于电渗析进行熔池保持已经由EP 1 239 057 A1、DE 198 49 278 C1和EP 0 787 829 A1有所公开。但是那里所介绍的过程控制和方法与膜的结合不能在碱性无电流工作的金属化熔池中用于无电流的铜或者其他金属。
发明内容
本发明的目的因此在于提供一种方法，该方法能够克服上述缺点并保证用于金属无电流沉积的电解质更长的使用时间和工作能力。
该目的依据本发明通过一种用于再生无电流金属化电解熔池的方法得以实现，具有以下方法步骤：
a)将至少一个电解质分流从过程容器导出，
b)再生导出的电解质流，
c)添加在金属化过程中消耗的成分，以及
d)将再生的电解质流回输到过程容器内，
其特征在于，为再生而将导出的分流输送到一渗析和/或电渗析单元，里面将无电流金属化过程中释放的阴离子通过离子选择膜进行交换。
具有优点的是，在依据本发明的方法中，将在金属化过程中释放的阴离子在渗析和/或电渗析单元中与氢氧根交换。
为此目的，渗析和/或电渗析单元在依据本发明的方法中具有优点地具有阴离子选择膜。
作为与电解质的渗析和/或电渗析的对流溶液，在依据本发明的方法中具有优点地可以使用含碱金属和/或碱土金属氢氧化物的溶液。
这种方法适用于无电流沉积铜、镍、三元镍合金、金的电解质。
借助于渗析和/或电渗析所要交换的离子可以是硫酸根、甲酸根、次磷酸根、亚磷酸根、磷酸根、氯离子等易于溶解的阴离子。
在依据本发明方法的另一构成方式中，作为在渗析和/或电渗析过程中使用的含碱金属和/或碱土金属氢氧化物的对流溶液在渗析过程之后再生。这一点依据本发明可以通过适当的氧化剂产生。在这种再生之后可以将含碱金属和/或碱土金属的溶液根据需要而浓缩。
在依据本发明的方法中再生所使用的含碱金属和/或碱土金属溶液的另一种可能性是，在渗析和/或电渗析过程中吸收的阴离子作为难溶盐沉淀。这种盐在硫酸根的情况下可以是例如难溶的硫酸钡，通过向渗析和/或电渗析过程所要再生的含碱金属和/或碱土金属氢氧化物对流溶液添加氢氧化钡可以将其沉淀出来。其他适用的盐例如为氢氧化钙或者一般其他与硫酸盐形成难溶化合物的物质。
甲酸根可以通过适用于再生对流溶液的氧化剂转换成CO2和水。适用于这种反应的氧化剂为过氧化氢、过氧化硫酸盐或者Degussa公司作为Caroat公知的制品。
将渗析和/或电渗析法用于再生金属无外电流沉积电解质的前提条件是，渗析和/或电渗析步骤中使用阴离子选择膜。
适用于依据本发明方法的阴离子选择膜例如为市场上常见的Tokuyama Soda Co，Ltd；Asaki Glass Co.Ltd.，Purolite International，Polymerchemie Altmeier或者Reichelt Chemietechnik公司的一价和二价阴离子交换膜。
在依据本发明方法的渗析步骤中施加电场可以具有优点地加速分离过程。
原则上无论是使用渗析化阶时还是在使用电渗析化阶时，所要再生的电解质和含碱金属和/或碱土金属的对流溶液均可以顺流以及对流进行。
具体实施方式
图1示出一种用于基质无电流金属化的常规方法。在为获得金属化的基质(7)在基质(3)上进行无电流铜沉积的情况下，从电解质(4)中提取分流(5)，在取决于金属离子和还原剂消耗量的情况下增加例如硫酸铜(1)和甲醛(2)，并再输送给电解质(4)。电解质(4)在该方法的过程中增加甲酸根和硫酸根(6)。
图2示出依据本发明用于为无电流沉积金属再生电解质的方法。从电解质(4)例如通过泵(8)提取分流并输送到渗析和/或电渗析单元(11)。渗析和/或电渗析单元(11)具有阴离子选择膜(19)。与渗析/电渗析(9)的对流溶液同样例如通过泵(8)输送到渗析和/或电渗析单元(11)。这一点可以与所要再生的电解质(4)顺流也可以对流进行。分流的电解质分流(5)在渗析和/或电渗析单元(11)内再生之后重新增加金属离子和还原剂。它例如可以是硫酸铜(1)和甲醛(2)。在硫酸铜和甲醛的情况下通过阴离子选择膜(19)的甲酸根和硫酸根由渗析和/或电渗析单元(11)内的对流溶液(9)吸收。为再生对流溶液，现在可以为硫酸盐沉淀(13)向其添加例如像氢氧化钡这种沉淀剂(12)。沉淀的硫酸盐(14)可以分离。吸收到对流溶液内的甲酸根可以通过添加氧化剂(15)在氧化(16)中转换成二氧化碳(17)和水。再生的对流溶液(18)可以在添加碱金属和/或碱土金属氢氧化物(10)的情况下回输。
附图符号
1 添加硫酸铜
2 添加甲醛
3 所要金属化的基质
4 用于无电流铜沉积的电解质
5 分流
6 增加甲酸根和硫酸根
7 金属化的基质
8 泵
9 用于渗析/电渗析的对流溶液
10 添加碱金属/碱土金属氢氧化物
11 渗析/电渗析单元
12 添加沉淀剂
13 硫酸盐沉淀
14 沉淀的硫酸盐
15 添加氧化剂
16 氧化甲酸根
17 二氧化碳
18 回输再生的对流溶液
19 阴离子选择膜
Claims (10)
1.用于再生无电流金属化所使用的电解熔池的方法，具有以下方法步骤：
将至少一个电解质分流从过程容器导出，
再生导出的电解质流，
将再生的电解质流回输到过程容器内，
其中，为再生而将导出的分流输送到一渗析和/或电渗析单元，里面将无电流金属化过程中释放的阴离子通过离子选择膜进行交换，其中，作为与电解质的渗析和/或电渗析的对流溶液使用含碱金属和/或碱土金属氢氧化物的溶液，其特征在于，在回输到过程容器之前向电解质添加在金属化过程中消耗的成分，其中，在渗析和/或电渗析过程中使用的碱金属和/或碱土金属氢氧化物溶液在渗析过程之后再生。
2.按权利要求1所述的方法，其中，在金属化过程中释放的阴离子与氢氧根交换。
3.按前述权利要求至少之一所述的方法，其中，渗析和/或电渗析单元具有阴离子选择膜。
4.按前述权利要求至少之一所述的方法，其中，无电流沉积的金属为由铜、镍、三元镍合金、金构成的组中的至少一种金属。
5.按前述权利要求至少之一所述的方法，其中，在渗析和/或电渗析过程中所要交换的离子为由硫酸根、甲酸根、次磷酸根、亚磷酸根、磷酸根和氯离子构成的组中的至少一种离子。
6.按前述权利要求至少之一所述的方法，其中，在渗析和/或电渗析过程中使用的含碱金属和/或碱土金属氢氧化物的溶液在渗析和/或电渗析单元内以对流或者顺流输送到所要再生的电解质。
7.按前述权利要求至少之一所述的方法，其中，在渗析和/或电渗析过程中使用的含碱金属和/或碱土金属的溶液通过适当的氧化剂再生并随后根据需要而浓缩。
8.按权利要求7所述的方法，其中，为氧化含碱金属和/或碱土金属氢氧化物的溶液而使用由过氧化氢、过氧化硫酸盐或者Caroat构成的组的至少一种氧化剂。
9.按权利要求1-6至少之一所述的方法，其中，在渗析和/或电渗析过程中使用的含碱金属和/或碱土金属氢氧化物的溶液通过将在渗析和/或电渗析过程中吸收的阴离子作为难溶盐沉淀而再生，并在需要时浓缩。
10.按权利要求9所述的方法，其中，为将在渗析和/或电渗析过程中吸收的阴离子作为难溶盐沉淀，使用由氢氧化钡、氢氧化钙或者其他与硫酸盐形成难溶化合物的物质构成的组中的至少一种物质。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102004002778.1 | 2004-01-20 | ||
| DE102004002778.1A DE102004002778C5 (de) | 2004-01-20 | 2004-01-20 | Verfahren zur Regenerierung von Metallisierungsbädern |
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| CN1670246A true CN1670246A (zh) | 2005-09-21 |
| CN100434567C CN100434567C (zh) | 2008-11-19 |
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| EP (1) | EP1557482B1 (zh) |
| JP (1) | JP2005206945A (zh) |
| KR (1) | KR20050076668A (zh) |
| CN (1) | CN100434567C (zh) |
| DE (1) | DE102004002778C5 (zh) |
| ES (1) | ES2386444T3 (zh) |
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| DE102010015361A1 (de) | 2010-04-16 | 2011-10-20 | Atotech Deutschland Gmbh | Membranelektrolysestapel, diesen enthaltende Elektrodialyseeinrichtung sowie Verfahren zum Regenerieren eines außenstromlos arbeitenden Bades zur Metallabscheidung |
| KR101218062B1 (ko) * | 2011-04-28 | 2013-01-03 | 씨큐브 주식회사 | 은 코팅 안료 및 그 제조 방법 |
| DE102018008312A1 (de) * | 2018-10-22 | 2020-04-23 | RIAG Oberflächentechnik AG | Verfahren zur Beschichtung von Substratoberflächen, Vorrichtung mit Beschichtungsbad, Dichtemesseinrichtung, Entnahmeeinrichtung, Zugabeeinrichtungen und Steuerung |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3454490A (en) * | 1966-08-10 | 1969-07-08 | Atomic Energy Commission | Concentration of ions using ion selective membranes |
| US3663403A (en) * | 1970-11-27 | 1972-05-16 | Ppg Industries Inc | Double ion exchange of an ultrafiltrate derived from an electrodeposition bath |
| ZA801260B (en) * | 1979-03-05 | 1981-03-25 | Electrochem Int Inc | Process for electrodialytically regenerating an electroless plating bath by removing at least a portion of the reacted products |
| US4253928A (en) * | 1979-10-04 | 1981-03-03 | Shell Oil Company | Process for sour water treatment |
| US4357220A (en) * | 1980-02-01 | 1982-11-02 | Eisenmann John L | Method and apparatus for recovering charged ions from solution |
| JPS5811775A (ja) | 1981-07-13 | 1983-01-22 | Matsushita Electric Ind Co Ltd | 銅の化学メッキ廃液の再生方法 |
| US4600493A (en) * | 1985-01-14 | 1986-07-15 | Morton Thiokol, Inc. | Electrodialysis apparatus for the chemical maintenance of electroless copper plating baths |
| JPS63484A (ja) | 1986-06-18 | 1988-01-05 | Nec Corp | 無電解銅めつき液の再生方法およびその装置 |
| JPS637382A (ja) | 1986-06-25 | 1988-01-13 | Nec Corp | 無電解銅めつき液の再生方法およびその装置 |
| US4805553A (en) * | 1986-10-27 | 1989-02-21 | Morton Thiokol, Inc. | Apparatus for bailout elimination and for enhancing plating bath stability in electrosynthesis/electrodialysis electroless copper purification process |
| US4762601A (en) * | 1986-11-10 | 1988-08-09 | Morton Thiokol, Inc. | Copper bath for electroless plating having excess counter-cation and process using same |
| EP0613862A3 (de) * | 1993-02-03 | 1994-12-28 | Metallgesellschaft Ag | Verfahren zur Reduzierung der Schadstoffkonzentration von aus industriellen Prozessen stammenden Abwässern. |
| US5419821A (en) * | 1993-06-04 | 1995-05-30 | Vaughan; Daniel J. | Process and equipment for reforming and maintaining electroless metal baths |
| JPH07286279A (ja) | 1994-04-20 | 1995-10-31 | Matsushita Electric Works Ltd | 無電解めっき方法 |
| US5472585A (en) * | 1994-11-30 | 1995-12-05 | At&T Corp. | Regeneration of spent electroless copper plating solution |
| US5523001A (en) * | 1994-12-30 | 1996-06-04 | At&T Corp. | Treatment of electroless plating waste streams |
| JP2873578B1 (ja) | 1998-02-15 | 1999-03-24 | 株式会社ワープエンジニアリング | 無電解ニッケルめっき廃液の処理方法および装置 |
| US6264809B1 (en) * | 1998-10-30 | 2001-07-24 | Pti Advanced Filtration, Inc. | Enhanced membrane electrode devices useful for electrodeposition coating |
| US6797141B1 (en) * | 1999-11-25 | 2004-09-28 | Enthone Inc. | Removal of coagulates from a non-glare electroplating bath |
| US6436213B1 (en) * | 2000-08-24 | 2002-08-20 | Pti Advanced Filtration, Inc. | Enhanced electro-deposition device and method |
| EP1184487A1 (de) * | 2000-08-29 | 2002-03-06 | Enthone-OMI (Deutschland) GmbH | Verfahren zur Reinigung eines Elektrolyten |
| DE50113264D1 (de) * | 2001-03-08 | 2007-12-27 | Enthone | System zur elektrodialytischen Regeneration eines stromlosen Badelektrolyten |
| DE10246453A1 (de) * | 2002-10-04 | 2004-04-15 | Enthone Inc., West Haven | Verfahren zur stromlosen Abscheidung von Nickel |
-
2004
- 2004-01-20 DE DE102004002778.1A patent/DE102004002778C5/de not_active Expired - Lifetime
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2005
- 2005-01-12 EP EP05000435A patent/EP1557482B1/de active Active
- 2005-01-12 ES ES05000435T patent/ES2386444T3/es active Active
- 2005-01-17 JP JP2005008890A patent/JP2005206945A/ja active Pending
- 2005-01-19 US US11/039,088 patent/US8057678B2/en active Active
- 2005-01-19 CN CNB2005100038620A patent/CN100434567C/zh active Active
- 2005-01-19 KR KR1020050004964A patent/KR20050076668A/ko not_active Application Discontinuation
Also Published As
| Publication number | Publication date |
|---|---|
| CN100434567C (zh) | 2008-11-19 |
| DE102004002778C5 (de) | 2017-04-20 |
| US8057678B2 (en) | 2011-11-15 |
| ES2386444T3 (es) | 2012-08-21 |
| EP1557482A2 (de) | 2005-07-27 |
| JP2005206945A (ja) | 2005-08-04 |
| EP1557482A3 (de) | 2006-06-07 |
| US20050194256A1 (en) | 2005-09-08 |
| EP1557482B1 (de) | 2012-06-06 |
| DE102004002778B4 (de) | 2008-03-27 |
| KR20050076668A (ko) | 2005-07-26 |
| DE102004002778A1 (de) | 2005-08-11 |
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