CN108374168A - 用于改善氧化锆预处理的锌表面的腐蚀性能的方法和组合物 - Google Patents

用于改善氧化锆预处理的锌表面的腐蚀性能的方法和组合物 Download PDF

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CN108374168A
CN108374168A CN201810314926.6A CN201810314926A CN108374168A CN 108374168 A CN108374168 A CN 108374168A CN 201810314926 A CN201810314926 A CN 201810314926A CN 108374168 A CN108374168 A CN 108374168A
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ion
agent
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alkaline
zirconium
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E·卡皮克
B·H·古德雷奥
A·博瓦迪利娅
M·费布拉罗
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Henkel AG and Co KGaA
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Abstract

本发明涉及改善包含涂布有氧化锆转化涂层的锌表面的金属基底的腐蚀性能的方法，通过在转化涂布之前通过使锌表面与包含以下的组合物接触：a)铁(III)离子；b)氢氧根离子源；c)至少一个络合剂，所述选自络合剂具有至少一个官能团‑COOX的有机化合物，其中X表示H或碱金属和/或碱土金属；d)0.0至约4g/l钴(II)离子；和任选存在的e)硅酸根源；其中所述组合物的pH为至少10。

Description

用于改善氧化锆预处理的锌表面的腐蚀性能的方法和组合物
本申请是2012年2月8日提交的国际申请号为WO2012/109339，中国国家申请号为201280004419.3，发明名称为“用于改善氧化锆预处理的锌表面的腐蚀性能的方法和组合物”的发明专利申请的分案申请。
相关申请的交叉引用
无。
技术领域
本发明涉及在与形成转化涂层组合物的氧化锆接触之前通过使用含钴和/或铁的组合物预处理含锌表面而改善沉积于含锌表面上的氧化锆转化涂层的腐蚀性能的方法。更具体地，本发明涉及多步骤涂布方法和其中使用的浴组合物，其在含锌表面例如热浸镀锌(下文称为HDG)和电镀锌(下文称为EG)基底上提供了改善的腐蚀性能，特别是循环腐蚀。本发明还提供了用于浴中的浓缩物组合物、制备和使用所述浓缩物和浴的方法、以及包含本发明的涂层的金属物品。
背景技术
目前在市场上已有用于替代汽车装配线中的磷酸锌产品的氧化锆沉积转化涂层产品。这些已知的产品用于涂布含铁金属表面以及含铝和含锌表面。
目前的氧化锆转化涂层工艺的问题是在某些环境下和在某些基底上它们不能提供像常规的磷酸锌方法一样好的防腐蚀。
一个特别的问题是用于含锌基底特别是HDG和EG的氧化锆转化涂层的现有方法不能提供符合某些汽车测试要求的经涂布的金属物品。当与目前用于汽车工业中的常规的磷酸锌处理相比较时，用可商购的氧化锆预处理浴处理的热浸镀锌(HDG)和电镀锌(EG)钢基底在两个独立的汽车工业腐蚀测试中显示出较弱的性能。因此，需要用氧化锆转化涂层涂布这些基底的方法，所述方法能够提供在HDG和EG基底上氧化锆转化涂层的改善的腐蚀性能。
本发明通过在氧化锆转化涂布方法中包括至少一个预处理步骤而解决氧化锆涂布方法中的上述问题中的一个或多个，其中在所述预处理步骤中使含锌表面与含钴和/或铁的组合物例如清洁剂(cleaner)和/或预清洗剂(pre-rinse)接触。
发明内容
在一个实施方案中，本发明提供了改善金属基底的腐蚀性能的方法，包括以下步骤：
1)提供包含至少一个锌或锌合金表面的金属基底；
2)使所述表面与包含以下的碱性预清洗剂组合物接触：
a)铁(III)离子；
b)氢氧根离子源；
c)至少一种络合剂，所述络合剂选自具有至少一个官能团-COOX的有机化合物，其中X表示H或碱金属和/或碱土金属；
d)0.0至约4g/l钴(II)离子；和
任选存在的
e)硅酸根源；
其中所述组合物的pH为至少10；
3)任选地清洗(rinsing)所述表面；
4)向所述金属基底施用包含锆的锆基(zirconium-based)金属预处理涂布组合物，由此在所述金属基底上形成预处理涂层；和
5)任选地向金属预处理涂布的金属基底施用漆(paint)。
在另一个实施方案中，本发明提供了所述方法中使用的含水碱性组合物。这些组合物和方法可以提供含水碱性组合物，所述含水碱性组合物包含量为1ppm至钴(II)离子的溶解度极限的钴(II)离子，并且如实施例中所示可以为不含磷酸盐的，含有低水平的硅酸盐或不含硅酸盐。
在所述方法的一个实施方案中，步骤2)的接触时间为10-60秒，且碱性预清洗组合物的温度为85-125°F。
在另一个实施方案中，所述组合物和方法可以包括锆基金属预处理涂布组合物，其进一步包含氟离子和螯合剂。在一个实施方案中，所述锆基金属预处理涂布组合物包含50-300ppm溶解的Zr、0-50ppm溶解的Cu、0-100ppm SiO2、150-2000ppm总氟离子、10-100ppm游离氟离子和任选存在的螯合剂。
在本发明的另一个方面，提供了经涂布的金属物品，其包含：
A)钢基底；
B)第一层，其包含沉积于所述钢基底上的锌或锌合金金属表面；
C)第二层，其通过与本发明的组合物接触而沉积于所述锌或锌合金金属表面上；
D)第三层，其包含通过使所述第二层与包含溶解的Zr的锆基金属预处理涂布组合物接触而沉积的氧化锆；
E)第四层，其包含至少一种漆；
其中与涂布有所述第一层、所述包含溶解的Zr的锆基金属预处理涂布组合物和所述至少一种漆而不包含C)的对比金属物品相比较，所述经涂布的金属物品具有更优的对循环腐蚀的耐性。
附图说明
图1显示根据实施例1中所述的三种方法处理的四种不同基底在循环腐蚀测试GM9540P中的性能的一系列柱状对比图。图1A显示热浸镀锌(HDG)的钢面板的腐蚀测试性能；图1B显示电镀锌(EG)的钢面板的腐蚀测试性能；图1C显示铝合金面板(Al6111)的腐蚀测试性能；图1D显示冷轧钢(CRS)面板的腐蚀测试性能。
图2显示根据实施例2中所述的三种方法处理的四种不同基底在循环腐蚀测试APGE中的性能的一系列柱状对比图。图2A显示热浸镀锌(HDG)的钢面板的腐蚀测试性能；图2B显示电镀锌(EG)的钢面板的腐蚀测试性能；图2C显示铝合金面板(Al6111)的腐蚀测试性能；图2D显示冷轧钢(CRS)面板的腐蚀测试性能。
具体实施方式
为了修饰大多数为锌的HDG和EG表面以改善腐蚀性能，申请人开发了可用作预清洗剂和清洁剂的包含钴和/或铁的碱性组合物，其用于在所述基底与产生氧化锆的转化涂层浴接触之前预处理HDG和EG基底，其为氧化锆涂布的基底提供改善的耐腐蚀性。
本发明的一个方面包括含水碱性组合物，其包含以下成分，基本上由以下成分组成，或由以下成分组成：
a)铁(III)离子；
b)氢氧根离子源；
c)至少一种络合剂，所述络合剂选自具有至少一个官能团-COOX的有机化合物，其中X表示H或碱金属和/或碱土金属；和
任选存在的
d)0.0至约4g/l钴(II)离子；
e)硅酸根源；
其中所述组合物的pH为至少10。
还提供了涂布包含至少一个锌或锌合金表面的金属基底的方法，由此改善所述金属基底的腐蚀性能，包括以下步骤:
1)提供包含至少一个锌或锌合金表面的金属基底，例如钢基底；
2)使所述表面与包含以下的组合物接触：
a)铁(III)离子；
b)氢氧根离子源；
c)至少一个络合剂，所述络合剂选自具有至少一个官能团-COOX的有机化合物，其中X表示H或碱金属和/或碱土金属；和
任选存在的
d)0.0至约4g/l钴(II)离子；
e)硅酸根源；
其中所述组合物的pH为至少10；
3)任选地清洗所述表面；
4)向所述金属基底施用包含50-300ppm溶解的Zr、0-50ppm溶解的Cu、0-100ppmSiO2、150-2000ppm总氟离子、10-100ppm游离氟离子和任选存在的螯合剂的锆基金属预处理涂布组合物，由此在所述金属基底上形成预处理涂层；和
5)任选地向所述金属预处理涂布的金属基底施用漆。
在用可商购的氧化锆预处理浴涂布之前与含钴和/或含铁的组合物例如碱性清洁剂和/或预清洗剂接触的HDG和EG钢基底在循环腐蚀测试中显示出改善的腐蚀性能。
用于制造具有含锌表面的抛光的(finished)氧化锆涂布的基底的典型方法将顺序地包括以下步骤：施用清洁剂溶液；在温水中清洗；施用抗腐蚀转化涂层；去离子水清洗；压缩空气干燥基底；通过电沉积施用初始的漆层，通常伴随烘烤；施用底漆层；施用基涂层漆层；和最后施用透明涂层漆层。术语“漆(paint)”理解为是指这些层中的任意层及其组合。在本发明中，通过使用包含钴和/或铁的本发明的清洁剂溶液、在清洁和抗腐蚀转化涂布之间增加碱性预清洗剂步骤(其中所述碱性预清洗剂包含钴和/或铁)或两者改变所述方法。钴和/或铁的引入使氧化锆转化涂布的锌表面的腐蚀性能产生出人意料的变化。
通常，清洁剂溶液的组成成分通常在高水平例如2-20重量％的硅酸盐和/或磷酸盐的条件下产生碱性pH，并且在清洁剂中没有主动添加的铁或钴，这与本发明优选所述的不同。在一个实施方案中，本发明的清洁剂组合物可以通过喷洒至基底上并随后在搅拌下浸入清洁剂浴而施用。在另一个实施方案中，在转化涂布之前，可以将基底浸入本发明的组合物中，移除，并任选地用蒸馏水清洗。
在一个实施方案中，发明人出人意料地发现通过添加钴和/或铁改变碱性清洁剂组合物可以使随后用抗腐蚀预处理例如氧化锆转化涂层涂布并根据工业标准上漆的含锌表面获得增加的耐腐蚀性。
根据本发明的组合物，例如清洁剂和预清洗剂包含：
a)铁(III)离子；
b)氢氧根离子源；
c)至少一种络合剂，所述络合剂选自具有至少一个官能团-COOX的有机化合物，其中X表示H或碱金属和/或碱土金属；和
任选存在的
d)0.0至约4g/l钴(II)离子；
e)硅酸根源；
其中所述组合物的pH为至少10。
组分a)铁(III)离子通常以(以越来越优选的顺序)约5、10、15、20、25、30、40、50、60、70、80、90、或100ppm的量存在，且至多以(以越来越优选的顺序)约500、400、350、300、250、200、150ppm的量存在。铁(III)离子的适合的来源为铁的水溶性盐或碱溶性盐，非限定性的实例为例如硝酸铁、硫酸铁、柠檬酸铁铵、柠檬酸铁、硫酸铁铵和氯化铁。优选硝酸铁和硫酸铁。
组分b)氢氧根离子源通常以(以越来越优选的顺序)约0.5、0.75、1、1.5、2、2.5g/l的量存在，且至多以(以越来越优选的顺序)约4.0、3.5、3.0、2.75g/l的量存在。可以使用更大量的氢氧根源，条件是组合物不会导致基底的过度蚀刻。适合的源为水溶性碱金属盐或氢氧化铵盐，优选NaOH或KOH。
组分c)一种或多种络合剂通常以(以越来越优选的顺序)约30、40、50、60、70、80、90或100ppm的量存在，且至多以(以越来越优选的顺序)约500、400、350、300、250、200、150ppm的量存在。
适合的络合剂的来源是选自具有至少一个官能团-COOX的水溶性有机化合物的那些，其中X表示H或碱金属和/或碱土金属。在一个实施方案中，络合剂选自单羧酸和/或二羧酸及其盐，任选地具有一个或多个氢氧根部分。
任选存在的组分d)钴(II)离子在浓度范围为0.0至约4g/l钴(II)离子。如果存在，钴通常有利地以(以越来越优选的顺序)约1、2、3、4、5、6、7、8、9、10、11、12、14、16、20、25、50ppm的量存在，且至多以(以越来越优选的顺序)约200、150、100、75、60ppm的量存在。可以添加更大的量，直至钴的溶解度极限。适合的钴离子源是水溶性或碱溶性的那些钴化合物，例如硝酸钴、硫酸钴、柠檬酸钴、氧化钴、氯化钴。优选硝酸钴和硫酸钴。
任选存在的组分e)硅酸根源的通常存在的量足以提供量为(以越来越优选的顺序)约30、40、50、60、70、80、90、100、150、200、250或300ppm且至多提供量为(以越来越优选的顺序)约1000、900、800、700、600、500、400、或350ppm的硅酸根。适合的硅酸根源包括水溶性硅酸盐例如碱金属硅酸盐。优选硅酸钠和硅酸钾。
本发明的组合物为碱性的，并且pH可以为至少(以越来越优选的顺序)10、10.5、11、11.5、12且至多为(以越来越优选的顺序)13.5、13、12.5。通常，通过在浴中存在约0.5-3g/L的OH而获得此pH。
本发明的组合物的应用条件为在(以越来越优选的顺序)约85、90、95、100、105、110、120°F的温度下，且至多在(以越来越优选的顺序)约125、130、135、140、145、150、155、160°F的温度下，即约30、35、40、45、50、55、60、65或70℃。
通常，任选地使用常规的清洁剂清洁待用氧化锆涂层涂布的锌或锌合金表面，随后将其与本发明的组合物接触10、15、20、25、30、45、60秒的时间，随后清洗。完整的方法可以参见以下的实施例。
可以通过喷洒、浸渍浴或两者而施用含锆预处理涂层，通常持续30-180秒的时间。通常，所述暴露在环境温度下发生，并且可以在约10-50℃的温度下发生，通常在20-30℃或25℃的温度下发生。
除非另有说明，否则上述浓度为用于工作浴的浓度。可以以给定的工作浴的浓度的1x-20x浓度提供用于制备工作浴的浓缩物，条件是浓度的增加不会导致浓缩物的沉淀或不稳定。期望地，如果浓缩物在环境温度下储存至少30、45、60、90、120天而不沉淀或结块，则所述浓缩物是稳定的。
除非在操作实施例中，或另有说明，否则此处使用的表示成分的量、反应条件、或限定成分参数的所有的数字应理解为在所有情况中都被术语“约”修饰。除非另有说明，否则所有的比例和百分比都为重量百分比。
实施例
实验室测试结果显示本发明的碱性预清洗剂改善了使用氧化锆转化涂层涂布的EG和HDG的循环腐蚀性能。
实施例1
测试方法包括：
方法1 Bonderite 958(可商购的磷酸锌：对照)
方法2 TD-1323-HB/HC标准方法(对照)
方法3碱性Co/Fe预清洗剂+TD-1323-HB/HC
方法4含Fe清洁剂+TD-1323-HB/HC
方法5含Co/Fe清洁剂+TD-1323-HB/HC
*TD-1323-HB/HC是可商购的氧化锆预处理浴。
标准(12”x4”)测试样板获自ACT Laboratories,Hillsdale,Michigan USA；冷轧钢(CRS)、电镀锌的钢(EG)、铝6111(AL6111)、热浸镀锌的钢(HDG)。根据以下方法中的一种方法处理四种基底中的每一种基底的样板。用于测试预清洗剂的方法步骤如下：
方法1(对照)Bonderite 958
1.Parco清洁剂1533–120秒(喷洒)
2.温水清洗-30秒(喷洒)
3.Fixodine Z8-30秒(喷洒)
4.Bonderite 958(磷酸锌处理)-120秒(浸渍)
5.冷水清洗-30秒(喷洒)
6.Parcolene 91-60秒(喷洒)
7.去离子水(DIW)清洗-30秒(喷洒)
方法2(对照)TD-1323-HB
1.Parco清洁剂1533-120秒(喷洒)
2.温水清洗-30秒(喷洒)
3.DIW清洗-30秒(喷洒)
4.TD-1323-HB-90秒(浸渍)
5.冷水清洗-30秒(喷洒)
6.DIW清洗-30秒(喷洒)
方法3 TD-1323-HB+碱性Co/Fe预清洗剂
1.Parco清洁剂1533-120秒(喷洒)
2.温水清洗-30秒(喷洒)
3.碱性Co/Fe预清洗剂9体积％浓缩物–15秒(喷洒)
4.温水清洗-30秒(喷洒)
5.DIW清洗-30秒(喷洒)
6.TD-1323-HB-90秒(浸渍)
7.冷水清洗-30秒(喷洒)
8.DIW清洗-30秒(喷洒)
表1
将测试样板上漆，使漆固化，并使样板经历40个循环的GM9540P腐蚀测试或50个循环的APGE测试。这样循环腐蚀测试为本领域技术人员公知的标准的汽车工业循环腐蚀测试。
表2
与氧化锆对照相比较，上述腐蚀结果显示HDG和EG的更佳的耐腐蚀性，显示为较小的锈蚀宽度(scribe creep)，并且在一些测试中与汽车常用的转化涂层磷酸锌(Bonderite958)一样好或比其更好。图1和2提供了与方法2相比较，本发明方法3的改善的结果的示意图，在方法2中使用锌、包含溶解的Zr的锆基金属预处理涂布组合物(TD-1323-HB)和漆涂布比较的金属物品而不使用碱性预清洗剂。测试还显示预清洗剂对CRS样板的耐腐蚀性没有不利影响，在将相同的方法用于CRS和锌表面以及由CRS和锌表面制成的金属物品中这对于可用性而言是重要的。
实施例2
测试了若干所提出的碱性预清洗剂制剂。浓缩物配方示于下表3中。
表3
配方1A、2A、4A和5A使用Co和Fe，配方3A和6A仅使用Fe。配方4A-6A使用添加的硅酸盐，配方1A-6A不含磷酸盐。配方1A和2A与配方4A和5A相似，但络合剂的水平不同。
标准(12”x4”)测试样板获自ACT Laboratories,Hillsdale,Michigan USA；冷轧钢(CRS)、电镀锌的钢(EG)、铝6111(AL6111)、热浸镀锌的钢(HDG)。方法步骤概括于下表5中。对于表4中的各浓度和时间，处理四种基底中的每一种基底的三个样板。
表4
表5:方法步骤:
测试样板使用DuPont的VI电泳涂布(e-coat)进行湿上加湿(wet-on-wet)电泳涂布。
方法浴的条件
清洁(所有方法)：
在20L喷洒罐中根据制造商的说明构建Parco清洁剂1533浴。游离碱度＝5.5～6.6，总碱度＝5.8～7.5，pH＝11.2～12.3，温度＝120°F(49℃)。
调整(用于 958方法)：
在20L喷洒罐中以1.2g/L构建Fixodine Z8浴。可滤过Ti＝6ppm，总Ti＝9ppm，pH≈9。
958浴：
游离酸＝0.8，总酸＝23.4，促进剂(accelerator)＝3.5，游离F–＝178ppm，Zn＝1000ppm，Ni＝900ppm，Mn＝570ppm，温度＝120°F(49℃)。
氧化锆涂布浴：
用于处理对照样板和碱性预清洗的样板的制剂相同：
初始：Zr＝159ppm，Cu＝24ppm，pH＝3.8～3.9，游离F–＝-95～-100RmV。用于转化涂布的氧化锆涂布浴参数为Zr 135-166ppm，Cu 15-26ppm，在整个研究期间将浴中的游离氟离子保持在-97至-110RmV之间，且pH为3.75-4.25。
碱性预清洗剂浴条件和各碱性预清洗剂变化示于表6中。
表6:各方法变化的碱性预清洗剂浴条件
腐蚀测试步骤
福特APGE循环腐蚀测试(FLTM BI 123-01)–CRS上15次循环，EG、HDG、和AL6111上50次循环。
通用汽车循环腐蚀测试(GM9540P)–所有基底上均40次循环。
EG上的腐蚀性能：
对于APGE测试；在大多数变化中EG经历约4-7mm的最大腐蚀。在少数情况下最大腐蚀高于7mm：配方1A在30秒和4％浓度下＝15.49mm，配方2A在30秒和4％浓度下＝12.00mm，配方3A在30秒和7％浓度下＝8.70mm。这三个变化的平均腐蚀值与其他变化相当；所有变化的范围都在4.62mm(1％和15秒)-1.70(7％，30秒)的范围内。配方2A在15秒和10％浓度下，以及在30秒和7％浓度下显示出最佳的结果，最大腐蚀为约3mm。
在GM9540P测试中，最大腐蚀大多数为约3.5-5mm之间。平均腐蚀的范围为3.69-1.88mm之间。在所有测试的浓度中，配方5A在15秒下具有≤3mm的最大腐蚀。
HDG上的腐蚀性能：
在APGE测试中，大多数变化的平均最大腐蚀为约4-7mm。在大多数情况下，漆的分层显著降低或被消除。在GM9540P中，最大腐蚀大多数为约4mm。
前述测试结果显示，与未使用预清洗剂步骤涂布并喷漆的相同的基底相比较，碱性预清洗剂改善了用锆基预处理涂布并喷漆的EG和HDG的腐蚀性能。在一些情况下，经预清洗的基底的腐蚀性能与磷酸锌预处理相当，且平均而言，经预清洗的基底似乎满足所需汽车制造商的耐腐蚀性测试规格。碱性预清洗剂对CRS的腐蚀性能没有不利影响。对于CRS，在30秒的处理时间下，配方1A显示出显著的改善。在加工中发现所使用的碱性预清洗剂在铝基底上导致金属刻蚀增加，因此可能适于非铝物品和基底。
根据相关法律标准描述了本发明，因此说明书本质上是示例性而非限定性的。对所公开的实施方案的变化和修改对于本领域技术人员而言是明显的并且在本发明的范围之内。因此，本发明提供的法律保护的范围仅能够通过研究以下权利要求而确定。

Claims (6)

1.使用碱性预清洗剂组合物预清洗汽车工业中的热浸镀锌或电镀锌的钢基底的方法，包括：
1)使所述锌表面与碱性预清洗剂组合物接触2-60秒的接触时间，所述碱性预清洗剂组合物包含：
a)5-400ppm的铁(III)离子；
b)0.5-4.0g/l的氢氧根离子源；
c)30-500ppm的至少一种络合剂，所述络合剂选自具有至少一个官能团-COOX的有机化合物，其中X表示H或碱金属和/或碱土金属；
d)0.0至4g/l钴(II)离子；和
任选存在的
e)硅酸根源；
其中所述组合物的pH为至少10；
2)任选地清洗所述锌表面；
3)向所述由冷轧钢和锌表面制成的金属制品施用包含锆的锆基金属预处理涂布组合物，接触时间为30-180秒，由此在所述金属制品的所有表面上形成氧化锆预处理涂层，得到氧化锆转化涂层涂布的金属制品；和
4)任选地向所述金属预处理涂布的金属制品施用漆。
2.如权利要求1所述的方法，其中步骤1)的接触时间为10-60秒，且碱性预清洗剂组合物的温度为85-125°F。
3.如权利要求1所述的方法，其中所述钴(II)离子以1ppm至所述钴(II)离子的溶解度极限的量存在。
4.如权利要求1所述的方法，其中所述碱性预清洗剂组合物不含磷酸盐。
5.如权利要求1所述的方法，其中所述锆基金属预处理涂布组合物还包含氟离子和螯合剂。
6.如权利要求1所述的方法，其中所述锆基金属预处理涂布组合物包含50-300ppm溶解的Zr、0-50ppm溶解的Cu、0-100ppm SiO2、150-2000ppm总氟离子、10-100ppm游离氟离子和任选存在的螯合剂。
CN201810314926.6A 2011-02-08 2012-02-08 用于改善氧化锆预处理的锌表面的腐蚀性能的方法和组合物 Pending CN108374168A (zh)

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