CN108468072B - 铁镍合金荫罩及其制备方法 - Google Patents
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- CN108468072B CN108468072B CN201810206291.8A CN201810206291A CN108468072B CN 108468072 B CN108468072 B CN 108468072B CN 201810206291 A CN201810206291 A CN 201810206291A CN 108468072 B CN108468072 B CN 108468072B
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- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000005323 electroforming Methods 0.000 claims abstract description 31
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 4
- 239000012190 activator Substances 0.000 claims description 3
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 239000008139 complexing agent Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 229910000990 Ni alloy Inorganic materials 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 239000006179 pH buffering agent Substances 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 13
- 239000000956 alloy Substances 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 229910001374 Invar Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910017709 Ni Co Inorganic materials 0.000 description 2
- 229910003267 Ni-Co Inorganic materials 0.000 description 2
- 229910003262 Ni‐Co Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N coumarin Chemical compound C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 229960000956 coumarin Drugs 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
- H01L21/2885—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition using an external electrical current, i.e. electro-deposition
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/70—Microphotolithographic exposure; Apparatus therefor
- G03F7/70691—Handling of masks or workpieces
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J29/00—Details of cathode-ray tubes or of electron-beam tubes of the types covered by group H01J31/00
- H01J29/02—Electrodes; Screens; Mounting, supporting, spacing or insulating thereof
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- H01J29/07—Shadow masks for colour television tubes
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Abstract
本申请公开了一种铁镍合金荫罩,其制备方法包括:提供一模板、电铸形成铁镍合金层、退膜、分离以及退火等步骤。制备完成的铁镍合金荫罩的含铁量高、热膨胀系数低,从而具有形状稳定性高、不易变形等特性,有助于提高重复利用率。
Description
技术领域
本申请涉及有机发光二极管显示技术领域,具体涉及一种金属荫罩及其制备方法。
背景技术
OLED技术是下一代平板显示技术的有力竞争者,各大显示器生产厂商也陆续推出高分辨率,高清晰度的OLED显示屏。为了赶上这项技术的发展速度,满足不同的市场需求,因此,开发高精度,小孔径尺寸的掩模板技术显得尤为迫切和重要。
目前Ni或Ni-Co合金通常采用电铸的方式生产高精度的荫罩,但是,由于Ni或Ni-Co合金的热膨胀系数较高,约为13ppm/℃,因此在沉积电致发光材料的过程中温度较高,其形状稳定性较差容易产生变形,导致重复利用率低。而传统的铁镍合金,尤其是因瓦合金(Fe-36%Ni)的热膨胀系数很低,约为1-2ppm/℃。但目前此类金属荫罩的生产方式主要采用刻蚀因瓦金属箔带,厚度较厚,存在刻蚀区域精度差的问题。同时,高能耗,高成本等缺点制约其进一步发展。因此,亟需开发一种低成本,低能耗,高精度的荫罩生产方法。
发明内容
本申请的目的在于提供一种铁镍合金荫罩及其制备方法,用以解决生产成本高,能耗高,开口精度差等以及在高温下容易产生变形等问题。
为了解决上述问题,本申请提供了一种铁镍合金荫罩的制备方法,包括:提供一模板(可以是但不限于带有设计图形的基板);电铸所述模板,在所述模板上形成铁镍合金层;退膜(去除感光膜);将所述铁镍合金层自所述模板上分离;以及对所述铁镍合金层退火,获得所述铁镍合金荫罩等步骤。
本申请同时提供一种通过上述制备方法所制成的铁镍合金荫罩。
与现有技术相比,本申请可以获得包括以下技术效果:
本申请公开了一种铁镍合金荫罩及其制备方法,采用电铸的方法,在有精细图形的模板上制备铁镍合金金属荫罩。通过调节各项参数,可以获得铁含量40%-70%的铁镍合金荫罩,其热膨胀系数在4-10ppm/℃之间,并且在通过热处理后可以将热膨胀系数进一步降低到1-3ppm/℃。因此本申请可以获得低能耗、易于生产的高精度金属荫罩,其形状稳定性高、不易变形,有助于提高重复利用率。
附图说明
此处所说明的附图用来提供对本申请的进一步理解,构成本申请的一部分,本申请的示意性实施例及其说明用于解释本申请,并不构成对本申请的不当限定。在附图中:
图1是本申请实施例的方法流程图。
图2是本申请实施例的镍含量与热热膨胀系数的关系图。
具体实施方式
以下将配合附图及实施例来详细说明本申请的实施方式,藉此对本申请如何应用技术手段来解决技术问题并达成技术功效的实现过程能充分理解并据以实施。
如在说明书及权利要求当中使用了某些词汇来指称特定组件。本领域技术人员应可理解,硬件制造商可能会用不同名词来称呼同一个组件。本说明书及权利要w还需要说明的是,术语“包括”、“包含”或者其任何其它变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、商品或者系统不仅包括那些要素,而且还包括没有明确列出的其它要素,或者是还包括为这种过程、方法、商品或者系统所固有的要素。在没有更多限制的情况下,由语句“包括一个……”限定的要素,并不排除在包括所述要素的过程、方法、商品或者系统中还存在另外的相同要素。
实施例描述
本申请的一具体实施例提供一种铁镍合金荫罩的制备方法,其步骤包括:
步骤S101:提供一模板。模板是使用感光膜经过涂布,曝光,显影步骤后带有设计图形感光膜的基板,但不限于此。模板可以是经过前处理程序的干净模板,或者是在此步骤中,先对模板进行除油、水洗、酸洗以及再次水洗等前处理程序,以去除模板表面的杂质。
步骤S103:电铸模板,在模板上形成铁镍合金层。在操作上,将模板置入一电铸液中,在适当温度下对模板进行电沉积程序。例如,将模板置入pH值介于2-3.5的电铸液中,并且在40-60℃的温度下进行电铸程序。在本申请的一些实施例中,电铸模板的步骤可以是在pH值介于3的电铸液中,以50℃的温度进行电铸程序。电铸阳极可以为因瓦合金(Invar)复合材料阳极或者1:2到2:1比例排布的镍阳极和铁阳极。并且可以通过整流器,例如双整流器,分别控制铁阳极和镍阳极的电流,其中给电方式可以采用电流值为2-4A/dm2的直流电或者开关比1:3到3:1的脉冲电流。阴阳极距离10-50cm。在30-60分钟的电铸时间内可以获得厚度为2-100um的铁镍合金层。对于OLED荫罩(或掩膜板)而言,其厚度越薄蒸镀阴影越小,普通Invar电铸容易产生20%甚至更多的厚度不均匀性,本实施例在电铸过程中另对电铸液进行搅拌,让电铸液的分布更均匀,并且在电铸过程中通过夹具控制电流均匀分布,本实施例中可以实现电铸层厚度不均匀性<10%,从而可以实现薄至2-4um的铁镍合金层,仍然可以从模板上撕下。对于普通的均匀性管控不好的电铸,有些点位会出现镀层太薄(<2um)而无法分离的现象。下列表格一和二为本申请一些实施例中作为示例性的Invar电镀荫罩(铁镍合金层)厚度和成分数据。
表格一、第1样品荫罩厚度和成分数据。
表格二、第2样品荫罩厚度和成分数据。
表格一和表格二的内容显示出本实施例中铁镍合金层的厚度和成分的不均匀性控制到+/-(4-7)%,因此可以得到均匀性极佳的铁镍合金层。
此外,在本实施例中,电铸液的成分包含硫酸镍40-80g/L、硫酸亚铁20-40g/L、pH缓冲剂30-45g/L、抗氧化剂1-5g/L、阳极活化剂10-20g/L以及络合剂0.2-1g/L。抗氧化剂可以使用柠檬酸,酒石酸,草酸,抗坏血酸,苹果酸,香豆素酸中的一种或多种;阳极活化剂可以使用氯化镍,氯化亚铁,盐酸中的一种或多种;络合剂可以为氨水,柠檬酸钠,草酸钠中的一种或多种。不同铁含量的合金镀品磁性和热膨胀系数不同,铁含量越高磁性越强。
如图2所示,在40%-64%铁含量范围内,热膨胀系数(CET,α)随着铁含量增加而降低,在64%铁含量左右达到最低值,然后随着铁含量增加热膨胀系数增大(相对地镍含量减少)。OLED蒸镀用掩膜板在使用的时候需要具有磁性和小的热膨胀性,所以理想的OLED金属掩膜板材料最好是带有磁性的CTE接近0的镍铁合金材质。铁含量多少可以通过电铸液中的硫酸亚铁离子的浓度,铁阳极的含量及电镀参数来调节。本实施例通过此电铸工艺可以获得铁含量占40%-70%的铁镍合金层。
步骤S105:退膜。例如将电铸后的模板浸泡在退膜液中20-40分钟,褪膜液溶解掉感光膜,从而达到褪膜目的。
步骤S107:将所述铁镍合金层自所述模板上分离。
步骤S109:对所述铁镍合金层退火,获得所述铁镍合金荫罩。此步骤可以在氩氢混合气或真空环境下进行,其中退火温度大约为200-1000℃,进行2-10小时。下列表格三给出了一组CTE数据比对。
表格三、CTE数据比对。
从表格三可以看出退火步骤可以有效地降低铁镍合金电铸品(即铁镍合金层)的热膨胀系数。
通过上述电铸制备方法,可以直接通过电铸获得铁含量40%-70%的铁镍合金荫罩,其热膨胀系数在4-10ppm/℃之间,经过步骤S109的退火处理程序后,可以将热膨胀系数进一步降低到1-3ppm/℃,且具有结构稳定不易变形以及厚度薄且均匀等特性。
上述说明示出并描述了本申请的若干优选实施例,但如前所述,应当理解本申请并非局限于本文所披露的形式,不应看作是对其他实施例的排除,而可用于各种其他组合、修改和环境,并能够在本文所述发明构想范围内,通过上述教导或相关领域的技术或知识进行改动。而本领域人员所进行的改动和变化不脱离本申请的精神和范围,则都应在本申请所附权利要求的保护范围内。
Claims (9)
1.一种铁镍合金荫罩的制备方法,其特征在于,包括以下步骤:
提供一模板;
电铸所述模板,于电铸液中在所述模板上形成铁镍合金层;
退膜;
将所述铁镍合金层自所述模板上分离;以及
对所述铁镍合金层退火,获得所述铁镍合金荫罩;
其中所述电铸液包含硫酸镍40-80g/L、硫酸亚铁20-40g/L、抗氧化剂1-2g/L、阳极活化剂10-20g/L以及络合剂0.2-0.4g/L;
在所述电铸所述模板的步骤中,还包含搅拌所述电铸液的步骤;
所述电铸液的pH值介于2-3.5之间;所述电铸液还包含30-45g/L的pH缓冲剂;
所述电铸液的温度介于40-60℃;在所述电铸所述模板的步骤中,使用整流器控制铁阳极和镍阳极的电流,并通过夹具控制电流均匀分布;
所述铁镍合金层的厚度为2-4um,厚度不均匀性<10%。
2.如权利要求1所述的方法,其特征在于,所述铁镍合金层的铁含量为40%-70%。
3.如权利要求1所述的方法,其特征在于,所述退膜步骤包含:在退膜液中浸泡20-40分钟后,进行水洗。
4.如权利要求1所述的方法,其特征在于,所述对所述铁镍合金层退火的步骤是在氩氢混合气或真空环境下进行。
5.如权利要求4所述的方法,其特征在于,所述对所述铁镍合金层进行退火的步骤是在200-1000℃的温度下退火2-10小时。
6.如权利要求1所述的方法,其特征在于,所述铁镍合金荫罩直接电铸后的热膨胀系数在4-10ppm/℃之间,经过退火处理后热膨胀系数降为1-3ppm/℃之间。
7.一种铁镍合金荫罩,其特征在于,通过如权利要求1所述的方法制备而成。
8.如权利要求7所述的铁镍合金荫罩,其特征在于,所述铁镍合金层的铁含量占40%-70%。
9.如权利要求7所述的铁镍合金荫罩,其特征在于,其热膨胀系数为1-3ppm/℃。
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