CN85101297A - 金属磷化工艺 - Google Patents

金属磷化工艺 Download PDF

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CN85101297A
CN85101297A CN198585101297A CN85101297A CN85101297A CN 85101297 A CN85101297 A CN 85101297A CN 198585101297 A CN198585101297 A CN 198585101297A CN 85101297 A CN85101297 A CN 85101297A CN 85101297 A CN85101297 A CN 85101297A
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phosphatization liquid
phosphatization
salt
zinc
trichloroacetate
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格哈德·米勒
维尔讷·劳施
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GEA Group AG
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Metallgesellschaft AG
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/23—Condensed phosphates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/08—Orthophosphates
    • C23C22/12—Orthophosphates containing zinc cations
    • C23C22/17—Orthophosphates containing zinc cations containing also organic acids
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
    • C23C22/362—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing also zinc cations

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Abstract

在低锌磷化工艺中，覆盖层的质量通过加入甲酸盐，次氮基三乙酸盐，三氯乙酸盐，乙二胺四乙酸盐中一种活化剂而得到改善，生成的磷化层均匀，特别适于电泳涂漆。

Description

本发明涉及金属磷化工艺，特别是钢和镀锌钢的磷化工艺。本发明使用含有加速剂锌、镍（如合适的话）的含水酸性磷化液，采用喷淋法实施，用于电泳涂漆之前。
德国专利申请公开说明书描述了一种含水酸性磷化液。该溶液Zn∶PO4（重量比）为1∶（12～110），用于金属特别是钢铁的表面处理上。由于锌含量低于普通磷化液，因而生成了一层薄而均匀的磷化层。该磷化层附着性强，耐蚀性能好，特别适于做为后续电泳涂漆的底层。
专利合作条约刊物WO    84/00386公开了一种磷化液。该溶液含有0.2～0.6g/l的锌和镍，Zn∶Ni（摩尔比）为1∶（5.2～16）。特别是金属在该溶液中磷化后，其表面生成了难溶于碱的磷化层。
日本专利刊物（按照化学文摘99/216843μ）58114477中描述了一种用于钢的喷淋磷化液。该溶液含有0.1～0.5g/l的锌，15～30g/l的磷酸盐，0.01～0.2g/l的亚硝酸盐，由此产生的磷化层特别适于后续阴极电泳涂漆的予处理。以前的其它刊物包括美国的Serial    No.373475，现在的美国专利4419199都公开了适用于某些磷酸锌溶液的活化剂。
采用锌浓度为0.1～0.6g/l的磷化槽液的普通工艺的缺点是：当这种磷化液用来喷淋金属时，经常产生不平整的磷化层，而且部分发灰，部分呈兰绿彩虹色。这种不均匀性在后面进行阴极电泳涂漆时就会变得更为明显，而且后处理的费用可能很高。此外，当面漆承截时，例如在与水接触的弯曲或拉伸中，其附着力往往不能满足形变的要求。
本发明旨在提供一项比普通工艺先进的工艺方法。利用该方法能够生产一层平整、均匀与面漆附着良好的磷化层。
如果按照本发明的内容完成上述工艺，这种目的就可达到。在本发明中，金属表面与含水的酸性磷化液相接触，该溶液含有
Zn++0.2～0.5g/l
Ni++0～1g/l
P2O58～20g/l
NO20.5～0.2g/l和/或硝基苯磺酸盐0.1～1g/l并且该磷化液中至少含有甲酸盐，次氮基三乙酸盐，三氯乙酸盐，乙二胺四乙酸盐中的一种化合物作为活化剂。
按照本发明，本工艺特别适用于铁、钢和镀锌钢的磷化处理，但也适用于锌合金，铝合金的磷化处理。
该磷化处理采用喷淋法，例如与铁、钢和铝的接触时间是90～240秒，锌为5～240秒。
根据本发明，磷化液一般在槽温30～60℃中使用。
一般说来，镍加到磷化液中对磷化速度，难磷化的钢表面层的形成，锌表面的磷化以及抗腐蚀性都起了有利作用。
在磷化过程中，为了建立平衡，按照本发明所使用的磷化液最好含有碱金属离子，例如钠、钾、锂或氨，如果需要，还可含有阴离子，如NO3、C1、或SO4。此外，磷化槽中还可含有磷化技术中常用的其它阳离子，例如，钴、铜、锰、钙、镁和铁。
在本发明的工艺中，用亚硝酸盐和/或硝基苯磺酸盐作为氧化反应的促进剂。此外，还可使用氧化反应促进剂的伴随化合物，例如氯酸盐，这可对氧化反应有利。
本发明的工艺中所使用的活化剂对磷化层的生成起了加速和均匀作用并且控制了磷化层单位面积的重量。例如，它们可以以相应的酸、碱金属盐的形式添加。在磷化液中，单一组份的活化剂的最佳浓度如下：甲酸盐5～15g/l，次氮基三乙酸盐0.3～3g/l，三氯乙酸盐2～15g/l，乙二胺四乙酸盐0.1～3g/l。除上述外，还可加其它添加剂/活化剂：氟化物0.5～3g/l，六氟硅酸盐1～5g/l，四氟硼酸盐3～10g/l，乙二醇脂（盐）0.3～5g/l，柠檬酸盐0.01～0.5g/l，酒石酸盐0.03～0.8g/l，缩合磷酸盐例如：焦磷酸盐，三聚磷酸盐，六偏磷酸盐0.03～0.3g/l。
根据本发明由该工艺产生的金属表面磷化层单位面积重一般在0.8和2.5g/m2之间。为了进一步促进特别细而薄的结晶磷化层的生成，最好使用普通活化剂例如，磷酸钛基的活化剂用在予清洗或最后清理阶段。
按本发明工艺产生的磷化层，原理上适用于磷化层的通用用途。磷化层与面漆的结合大大改善了面漆在腐蚀应力下的耐穿透性。在遭到刮伤，冲击和弯曲应力时，明显的增加了面层与金属底层的附着力，这些优点是显而易见的，特别是在电泳涂漆或阴极电泳涂漆后更为显著。鉴于此，这种工艺最适合作为以这种方法涂漆前的准备工作中。根据本发明，这种工艺已用在实际中，例如：汽车车体磷化。
下面根据本发明的工艺，通过举例的方法，较为详细的说明这种工艺。
实例
通过喷淋的方法，首先将钢板用弱碱、活性清洗剂除油，然后用水冲洗。将该钢板在55℃下喷淋磷化液不到两分钟，再用水冲洗，用稀Cr（Ⅵ）/Cr（Ⅲ）液钝化，用去离子水喷淋洗净，部分钢板干燥后，然后将此部分钢板进行阴极电泳。根据实例1～7，每种磷化液含有：Ni    0.5g/l
P2O514g/l
CLO31.5g/l
NO20.1g/l
锌含量在表中表明。
根据实例8～11，磷化液含有：
Zn    0.4g/l
Ni    0.5g/l
P2O514.0g/l
CLO31.5g/l
NO20.1g/l
另外，表中提到了活化剂的含量。阐述过的每一种磷化液都应用碱进行磷化平衡。
用评价磷化层的形式说明磷化处理的效果，如下：
表1
磷化液    磷化层评价
1    Zn    0.1g/l    兰亮
2    Zn    0.2g/l    约80%兰亮
约20%灰色细结晶
3    Zn    0.3g/l    约60%兰亮
约40%灰色细结晶
4    锌    0.4g/l    约30%兰亮
约70%灰色细结晶
5    锌    0.5g/l    约20%兰亮
约80%灰色细结晶
6    锌    0.6g/l    约5%兰亮
约95%灰色细结晶
7    锌    0.7g/l    灰色细结晶
8    甲酸盐7g/l    灰色细结晶
9    次氮基三乙酸盐1    灰色细结晶
10    三氯乙酸盐10g/l    灰色细结晶
11    乙二胺四乙酸盐0.3g/l    灰色细结晶
根据本发明工艺的优点与根据先有技术的例1～6相比的磷化层评定情况，清楚地表明在例8～11中。由于分批轧制的钢板显示出不同的化学活性，尽管这不会严重影响相对差别，但自测评定的绝对值受到了一定的影响。
如果适当地加一些亚硝酸盐，使用含亚硝酸盐无氯酸盐的磷化液和含有硝基苯磺酸盐的磷化液进行磷化处理，所得磷化层的评价结果类似。
在阴极电泳涂漆后，根据实例1～6磷化得到的钢板表面漆膜不平，而根据实例7～11磷化的钢板漆膜平整。
使用自动涂漆方法所得到的某些阴极电泳钢板的漆膜厚度可达100μA，并用多种方法对其检测。通过盐雾对VVV路面碎石冲击试验，在湿热大气中暴露后的交叉影线试验及在园锥轴芯上的弯曲试验，表明根据本发明处理的钢板实验结果很好，比按先有技术中实例4和实例7所得到的钢板实验结果好的多。
补正    85101297
文件名称    页    行    补正前    补正后
说明书    1    4    说明书描述    说明书2232067描述
1    9    刊物    公告
2    倒数4    还可使用氧化反    “还可伴随使用氧化反应
应促进剂的伴随    促进剂”
化合物
3    5    乙二醇脂    甘醇酸酯
5    8    自测    目测
权利要求书    1    11、12    乙二醇酯    甘醇酸酯
1    19    所述    所述的方法

Claims (6)

1、金属磷化工艺，特别是钢和镀锌钢磷化工艺，通过喷淋的方法，使用含锌促进剂的水溶液酸性磷化液，其中金属表面与磷化液相接触。该溶液含有：
zn++0.2～0.5g/l
P2O58～20g/l
NO2 -0.05～0.2g/l
硝基苯磺酸盐  0.1～1g/l
且至少从含有甲酸盐，次氮基三乙酸盐，三氯乙酸盐，乙二胺四乙酸盐中选取一种化合物做为促进剂。
2、根据权项1所述的方法，其中金属表面与磷化液相接触，该溶液至少含有下列一种添加剂：氟化物，六氟硅酸盐，四氟硼酸盐，乙二醇酯，柠檬酸盐，酒石酸和浓缩磷酸盐。
3、根据权项1所述的方法，其中金属表面与磷化液相接触，在该磷化液中活化剂的含量为
甲酸盐  5～15g/l
次氮基三乙酸盐  0.3～3g/l
三氯乙酸盐  2～15g/l
乙二胺四乙酸盐  0.1～3g/l
4、根据权项2或3所述，含有的其它添加剂如下：
氟化物  0.5～3g/l
六氟硅酸盐  1～5g/l
四氟硼酸盐  3～10g/l
乙二醇酸盐  0.3～5g/l
柠檬酸盐  0.01～0.5g/l
5、根据权项1或2所述的方法，其中磷化后的表面要经过电泳涂漆。
6、根据权项1或2所述的方法，其中磷化液还含有0～1g/l的镍离子。
CN198585101297A 1984-03-09 1985-04-01 金属磷化工艺 Pending CN85101297A (zh)

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DE19843408577 DE3408577A1 (de) 1984-03-09 1984-03-09 Verfahren zur phosphatierung von metallen

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EP (1) EP0154367B1 (zh)
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AT (1) ATE37203T1 (zh)
AU (1) AU575380B2 (zh)
CA (1) CA1224121A (zh)
DE (2) DE3408577A1 (zh)
ES (1) ES8602152A1 (zh)
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CN103668149A (zh) * 2013-12-19 2014-03-26 湖南金裕化工有限公司 常温快速磷化液及其制备方法
CN103695881A (zh) * 2013-12-19 2014-04-02 湖南金裕化工有限公司 常温无渣快速磷化液及其制备方法

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CN103695881A (zh) * 2013-12-19 2014-04-02 湖南金裕化工有限公司 常温无渣快速磷化液及其制备方法
CN103668149B (zh) * 2013-12-19 2016-08-24 湖南金裕化工有限公司 常温快速磷化液及其制备方法
CN103695881B (zh) * 2013-12-19 2016-08-24 湖南金裕化工有限公司 常温无渣快速磷化液及其制备方法

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GB8506049D0 (en) 1985-04-11
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EP0154367A3 (en) 1986-08-20
US4637838A (en) 1987-01-20
ZA851761B (en) 1985-11-27
GB2155960A (en) 1985-10-02
DE3564967D1 (en) 1988-10-20
EP0154367B1 (de) 1988-09-14
AU3957485A (en) 1985-09-12
DE3408577A1 (de) 1985-09-12
AU575380B2 (en) 1988-07-28
EP0154367A2 (de) 1985-09-11
ES541015A0 (es) 1985-12-01
ES8602152A1 (es) 1985-12-01

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