CN114134541A - 制备用于电化学工艺的板材材料的方法 - Google Patents
制备用于电化学工艺的板材材料的方法 Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 42
- 239000002184 metal Substances 0.000 claims abstract description 42
- 238000011282 treatment Methods 0.000 claims abstract description 14
- 239000010949 copper Substances 0.000 claims description 38
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 35
- 229910052802 copper Inorganic materials 0.000 claims description 35
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 28
- 239000011651 chromium Substances 0.000 claims description 13
- 239000011572 manganese Substances 0.000 claims description 13
- 229910001220 stainless steel Inorganic materials 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 12
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
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- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
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- C21D7/00—Modifying the physical properties of iron or steel by deformation
- C21D7/02—Modifying the physical properties of iron or steel by deformation by cold working
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Abstract
本发明涉及一种制备用于电化学工艺的板材材料的方法。制造板材材料的方法,该板材材料用于金属电化学工艺中作为在其表面上沉积金属的阴极的一部分。用卷取工艺线中的至少一种处理来得到用于金属沉积物和板材材料之间的附着的板材材料的表面粗糙度。
Description
本申请是2016年1月26日提交的题为“制备用于电化学工艺的板材材料的方法”的中国专利申请201680007364.X的分案申请。
本发明涉及一种用于金属的电化学工艺如电解精炼或电解冶金的板材材料的制造方法。
阴极板材材料的表面粗糙度是在湿法冶金工业中的电化学镀覆金属的附着力的重要参数。工业经验表明,表面需要足够粗糙以确保电镀金属的附着并避免电镀金属的预剥离(prestripping),但另一方面需要不太粗糙,以防止附着力太高,使得移出电镀金属非常难或在剥离过程中破坏板材。在铜工业中,不锈钢已经用作电解精炼和电解冶金的阴极板材。用于阴极板材的优选不锈钢等级为具有冷轧表面2B的EN 1.4404(316L/UNSS31603)。该不锈钢等级通常含有10-13重量%的镍,这是一种昂贵的成分。因此,铜业不仅寻求更成本有效的替代品,例如作为阴极板材的双相不锈钢,而且还寻求更经济的制造阴极板材的工艺。
电化学工艺步骤是处理例如金属性铜的最后步骤之一。在电解精炼中,铜阳极和阴极位于含有硫酸铜和硫酸的电解质溶液中。使电流通过溶液,使来自带正电的阳极的铜沉积在带负电的阴极上。铜的电解冶金通过类似的方法进行,但是从溶液中而不是阳极移出铜,且铜沉积在阴极上。当在阴极上沉积了适量的铜时,将阴极从溶液中移出并剥离,以从阴极板材的表面移出铜沉积物。
美国专利7,807,029涉及永久不锈钢阴极板材,该阴极由低镍双相钢或较低等级的“304”钢组成,其中至少一个阴极表面具有表面粗糙度以产生对于允许操作粘附性必要的附着力。附着力对于防止铜沉积物与表面的机械分离不够强。然而,美国专利7,807,029中期望的附着力仅基于预定的附着力特性,其确定了各表面的表面粗糙度Ra在0.6-2.5微米的范围内。没有给出表面上的附着力的任何具体确定以及制造阴极板材的方法。
WO公开2012/175803描述了永久阴极和用于处理永久阴极的表面的方法。在该方法中,化学或电化学处理永久阴极板材表面的晶界,以得到对于沉积金属在表面上的附着力和从表面剥离金属所期望的表面性能。
所引用的美国专利7,807,029和引用的WO公开2012/175803关注待用作电精炼或电解冶金中的电极的单独和分离的阴极板材的表面处理。这些参比文献没有描述如何生产单独和分离的阴极板材。
本发明的目的是为了防止现有技术的一些缺陷,并且实现用于制造待用在金属的电化学工艺(例如电解精炼或电解冶金)中的板材材料的改进方法。本发明的基本特征列在所附权利要求中。
根据本发明,使用板材材料作为阴极的一部分,在其表面上在金属的电化学工艺例如电解精炼或电解沉积中沉积金属。该板材材料是在卷取工艺线例如冷轧工艺线中制造的,从而得到了对金属沉积物和板材材料之间的附着力而言所期望的表面粗糙度。通过卷取工艺线中的至少一种机械和/或化学处理制成待用作阴极的一部分的板材的表面粗糙度。对于所期望的表面粗糙度的处理可以是例如以下处理中的一种或多种:图案化轧制(pattern rolling)、湿磨、干磨、喷丸、酸洗、刷涂、光整冷轧或这些处理的任何组合。
待在卷取工艺线中处理的板材材料有利地是由不锈钢制成的带材。在卷取工艺线中的最终处理之后,将具有期望的表面粗糙度的板材材料(即从卷取工艺线接收的产品)保持为板材的形状,但是可以有利地处理以具有卷材的形式。作为板材的形状,该材料可以被切割成期望的尺寸以用作阴极的一部分,在其表面上在电化学工艺中沉积金属。在板材材料作为卷材形式的情况下,板材材料基本容易地转移到进行金属的电化学工艺的位置。然后将卷取的板材材料切割成对于金属的电化学工艺的操作有利的形状。
根据本发明的卷取工艺线有利地包括工艺步骤例如退火、化学表面处理、机械表面处理、冷轧。可以例如酸洗化学表面处理。机械处理可以例如是研磨、湿磨或干磨、刷涂和喷丸。冷轧可以例如通过图案化轧制来进行。可以利用这些工艺步骤的任何组合从而使板材材料具有所期望的表面粗糙度。根据本发明的一个优选实施方案,用于板材材料的卷取工艺线由以下处理构成:预退火和酸洗、冷轧、研磨、最终退火和酸洗。
用本发明处理的板材材料在金属的电化学工艺中用作阴极的一部分,其中待沉积在板材材料上的金属例如是铜、镍或银。电化学工艺可以例如是电解精炼或电解冶金。
为了得到对于待用作金属的电化学工艺中的板材所期望的表面粗糙度,通过测量分离在板材的表面和沉积在板材表面上的金属之间的沉积金属所需的剪切力来确定金属电化学工艺中的附着力。使用用于拉伸试验机的工具测量剪切力。将由板材材料例如不锈钢制成的样品放置在工具中,使得样品可移动但足够紧密,使得样品表面上沉积的金属保留在固定金属片的工具壁上。然后,将工具和样品放置在拉伸试验机中,使得样品被压下,同时将金属沉积物保持在固定位置。当样品降低时,测量从样品分离金属沉积物所需的剪切力。
参照下面的附图更详细地描述本发明,其中
图1示出了本发明的一个优选实施方案,以铜作为待沉积在板材材料上的金属,示出了剪切力和表面粗糙度Ra之间的相关性,
图2示出了本发明的一个优选实施方案,以铜作为待沉积在板材材料上的金属,示出了剪切力和表面粗糙度Ra(工业规模)的相关性。
一方面使用不同的板材材料,另一方面使用板材表面上的不同表面粗糙度值,确定板材材料的化学组成和表面粗糙度对在待沉积的铜和待用于铜的电化学工艺中的板材之间的剪切力的影响。为了比较板材材料本身是否影响剪切力,将板材样品研磨成相似的表面粗糙度值。为了确定由表面粗糙度引起的对剪切力的影响,对于由相同板材材料制成的样品,得到了不同的表面粗糙度。此外,通过在表面上得到平行于样品长度的研磨槽和基本垂直于样品长度的研磨槽来确定由在板材样品的表面上的研磨所有利得到的槽对准的效果。
在电化学电池中得到板材样品表面上的铜沉积物,其中由水合硫酸铜、氯化钠、硫脲和硫酸组成的电解质模拟在铜电解精炼中的工业规模的电解质。在电化学电池中,在操作期间使用饱和甘汞参比电极(SCE)对电势进行配准(register),并将铂网作为对电极。在电化学工艺中,将空气鼓入电解质中以促进搅拌。当期望量的铜沉积在板材样品的表面上时,将停止电化学工艺。
在表1中是测试的板材材料的化学组成的主要元素含量(以重量%计):
表1
C% | Mn% | Cr% | Ni% | Mo% | N% | Cu% | |
A | 0.020 | - | 17.2 | 10.1 | 2.1 | - | - |
B | 0.030 | 5.0 | 21.5 | 1.5 | 0.30 | 0.22 | 0.30 |
C | 0.020 | - | 22.0 | 5.7 | 3.1 | 0.17 | - |
合金A表示EN 1.4404(316L/UNS S31603)奥氏体不锈钢,其通常用于阴极板材,并其以重量%计含有小于0.03%的碳(C)、小于2%锰(Mn)、16.5-18.5%铬(Cr)、10-13%镍、2-2.5%钼(Mo)和小于0.10%氮(N)。
合金B表示EN 1.4162(LDX2101/UNS32101)双相奥氏体铁素体不锈钢,其通常以重量%计包含小于0.04%碳(C)、4-6%锰(Mn)、21-22%铬(Cr)、1.35-1.70%镍、0.1-0.8%钼(Mo)、0.2-0.25%氮(N)和0.1至0.8铜(Cu)。
合金C表示EN 1.4462(2205/UNS32205)双相奥氏体铁素体不锈钢,其通常以重量%计包含小于0.03%碳(C)、小于2%锰(Mn)、21-23%铬(Cr)、4.5-6.5%镍、2.5-3.5%钼(Mo)和0.10-0.22%氮(N)。
为了确定合金A-C中的表面粗糙度和剪切力之间的相关性,通过使用不同的砂带并且使用已或多或少磨损的砂带来得到不同的表面粗糙度值。此外,通过表面的干磨或湿磨获得不同的表面粗糙度。此外,还测试了喷丸和酸洗的表面以及在卷取工艺线中光整冷轧的材料。
根据本发明,用表面粗糙度计对表面粗糙度值Ra(粗糙度平均值)进行表面粗糙度测量,其中对于Ra值小于2.26微米的样品,截取值(cut-off)设定为0.8mm,针穿过速度为0.5mm/s。对于Ra值高于2.26微米的样品,截取值设定为2.5mm,针穿行速度为1mm/s。
将每个板材样品放置在电化学电池中从而在每个板材样品的表面上得到铜沉积。在开始剪切过程之前,注意到沉积的铜和样品之间的界面显示出铜非常好地渗透到样品表面的非常小的形貌特征中。
为了通过沉积的铜和板材表面之间的剪切力测量附着力,将具有沉积铜的样品设置在工具中,使得样品可移动,但是沉积的铜保持在固定位置。然后,将该工具放置在拉伸试验机中,并将阴极板材样品进行移动以用于将铜沉积物与板材样品分离所需要的力的测量。
在下表2列出了具有表面粗糙度和测量的剪切力的板材样品,和在图1中示出表面粗糙度Ra。参比材料的值也列于表2中。在表2中,术语“磨损带”是指在实际处理之前曾用于至少一次研磨处理的磨带,而术语“新带”是指在实际处理前未曾用于根据发明的处理的磨带。
表2
测试样品 | 合金 | 表面粗糙度R<sub>a</sub>(μm) | 剪切力(N) |
参比表面(干磨的) | A | 0.36 | 574.8 |
参比表面(干磨的) | B | 1.87 | 487.5 |
参比表面(干磨的) | B | 1.2 | 480.6 |
喷丸和酸洗的 | B | 2.89 | 655.8 |
湿磨测试1磨损带 | B | 0.96 | 262.8 |
湿磨测试1新带 | B | 2.24 | 551.5 |
湿磨测试2新带 | B | 1.55 | 407.5 |
湿磨测试3磨损带端 | B | 5.15 | 633.3 |
湿磨测试3新带端 | B | 2.26 | 323.9 |
湿磨测试3磨损带开始 | B | 4.56 | 560.0 |
湿磨测试3新带开始 | B | 2.18 | 301.0 |
在表2中,结果基于三次测试,其中表面粗糙度通过湿磨和一次测试得到,其中表面粗糙度通过喷丸和酸洗的组合得到。注意,当表面粗糙度值增加时,通过剪切力测量的附着力增加。对湿磨表面,可以看到基本线性的趋势。通过板材的表面粗糙度调节沉积在板材表面上的板材和铜之间的测得剪切力,且如图1所示,当通过研磨得到板材的表面粗糙度时,剪切力与板材的表面粗糙度正成比。对于以喷丸和酸洗的组合(首先通过喷丸处理然后通过酸洗)处理的样品测得最高剪切力值。此外,还从铜沉积物和不锈钢表面之间的界面注意到,铜沉积物良好渗透到不锈钢表面的非常小的形貌特征中。因此,表面粗糙度Ra 0.7-5.5微米,优选0.7-2.5微米,对于铜沉积物和不锈钢表面之间的期望附着力是足够的。因此,剪切力为250-800N,优选250-650N。
还以工业规模测试了表面粗糙度与剪切力之间的关系,在表3给出了结果,且在图2给出了合金B的。
表3
样品 | 表面粗糙度R<sub>a</sub>(μm) | 剪切力(N) |
1 | 0.92 | 302 |
2 | 1.01 | 397 |
3 | 1.1 | 509 |
4 | 0.99 | 409 |
5 | 1.25 | 521 |
6 | 1.35 | 509 |
7 | 1.31 | 656 |
8 | 1.33 | 507 |
9 | 1.18 | 505 |
10 | 1.18 | 506 |
11 | 1.12 | 516 |
12 | 1.09 | 474 |
13 | 1 | 521 |
14 | 1.18 | 492 |
15 | 0.89 | 370 |
16 | 1.27 | 624 |
表3和图2中的测试结果表明,表面粗糙度和剪切力具有彼此的线性依赖性。此外,通过剪切力测量的附着力结果基本在与实验室规模中的剪切力值相同的范围。
Claims (25)
1.一种制造板材材料的方法,该板材材料用于在金属的电化学工艺中作为阴极的一部分,金属沉积在该阴极的表面上,其中该方法包括:
在卷取工艺线例如冷轧工艺线中制造该板材材料,从而得到对金属沉积物和板材材料之间的附着力而言所期望的表面粗糙度,所述板材材料的表面提供了将沉积金属与该板材材料表面分离所需的250-800N的剪切力,
其中通过卷取工艺线中的机械和/或化学处理中的至少一种,使待用作阴极的一部分的板材的表面粗糙度具有0.7-5.5微米的粗糙度平均值。
2.根据权利要求1所述的方法,其中机械地得到板材材料表面的表面粗糙度的改变。
3.根据权利要求1所述的方法,其中通过湿磨而得到所述板材材料表面的表面粗糙度的改变。
4.根据权利要求1所述的方法,其中通过干磨而得到所述板材材料表面的表面粗糙度的改变。
5.根据权利要求1所述的方法,其中通过喷丸而得到所述板材材料表面的表面粗糙度的改变。
6.根据权利要求1所述的方法,其中通过刷涂而得到所述板材材料表面的表面粗糙度的改变。
7.根据权利要求1所述的方法,其中通过图案化轧制而得到所述板材材料表面的表面粗糙度的改变。
8.根据权利要求1所述的方法,其中化学地得到板材材料表面的表面粗糙度的改变。
9.根据权利要求1所述的方法,其中机械和化学地得到板材材料表面的表面粗糙度的改变。
10.根据权利要求9所述的方法,其中通过喷丸和酸洗而得到所述板材材料表面的表面粗糙度的改变。
11.根据权利要求1所述的方法,其中通过处理的组合而得到所述板材材料表面的表面粗糙度的改变。
12.根据权利要求1所述的方法,其中粗糙度平均值Ra为0.7-2.5微米。
13.根据前述权利要求1所述的方法,其中剪切力为250-650N。
14.根据前述权利要求1所述的方法,其中所述金属是铜。
15.根据权利要求14所述的方法,其中所述电化学工艺是电解精炼且所述金属是铜。
16.根据权利要求14所述的方法,其中所述电化学工艺是电解冶金且所述金属是铜。
17.根据权利要求1所述的方法,其中所述金属是银。
18.根据权利要求17所述的方法,其中所述电化学工艺是电解精炼且所述金属是银。
19.根据权利要求17所述的方法,其中所述电化学工艺是电解冶金且所述金属是银。
20.根据权利要求1所述的方法,其中所述金属是镍。
21.根据权利要求20所述的方法,其中所述电化学工艺是电解精炼且所述金属是镍。
22.根据权利要求20所述的方法,其中电化学工艺是电解冶金且所述金属是镍。
23.根据前述权利要求1所述的方法,其中板材材料是奥氏体不锈钢制成,其以重量%计含有小于0.03%碳(C)、小于2%锰(Mn)、16.5-18.5%铬(Cr)、10-13%镍(Ni)、2-2.5%钼(Mo)和小于0.10%的氮(N)。
24.根据前述权利要求1所述的方法,其中板材材料是双相奥氏体铁素体不锈钢,其以重量%计含有小于0.04%碳(C)、4-6%锰(Mn)、21-22%铬(Cr)、1.35-1.70%镍(Ni)、0.1-0.8%的钼(Mo)、0.2-0.25%的氮(N)和0.1-0.8铜(Cu)。
25.根据前述权利要求1所述的方法,其中板材材料是双相奥氏体铁素体不锈钢,其以重量%计含有小于0.03%碳(C)、小于2%锰(Mn)、21-23%铬(Cr)、4.5-6.5%镍(Ni)、2.5-3.5%钼(Mo)和0.10-0.22%氮(N)。
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EP3250732A1 (en) | 2017-12-06 |
MX2017009658A (es) | 2017-12-11 |
CN107208292A (zh) | 2017-09-26 |
EA201791385A1 (ru) | 2018-01-31 |
FI20155057A (fi) | 2016-07-28 |
CA2973426A1 (en) | 2016-08-04 |
BR112017016139A2 (pt) | 2018-04-17 |
FI128294B (en) | 2020-02-28 |
EP3250732A4 (en) | 2018-07-25 |
JP6534446B2 (ja) | 2019-06-26 |
AU2016211073A1 (en) | 2017-08-10 |
BR112017016139B1 (pt) | 2022-06-14 |
CA2973426C (en) | 2023-01-03 |
CL2017001839A1 (es) | 2018-03-09 |
AU2016211073B2 (en) | 2021-06-10 |
US11001932B2 (en) | 2021-05-11 |
KR20170098934A (ko) | 2017-08-30 |
JP2018509526A (ja) | 2018-04-05 |
US20180038005A1 (en) | 2018-02-08 |
WO2016120525A1 (en) | 2016-08-04 |
KR102062964B1 (ko) | 2020-01-06 |
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