JP4949416B2 - Etching solution composition for ITO film and method for etching ITO film using the same - Google Patents
Etching solution composition for ITO film and method for etching ITO film using the same Download PDFInfo
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Description
本発明は、ＩＴＯ膜用のエッチング液組成物およびそれを利用したＩＴＯ膜のエッチング方法に関する。より詳細には、本発明は、ＩＴＯ透明導電膜に対して優秀なエッチング能力を有し、その組成が安定的であり、エッチング工程時にフォトレジストなどの光反応物質に対する侵食を減少させ、残渣または析出物を残さない優秀な特性を有するエッチング液組成物、および、前記エッチング液組成物を利用して酸化インジウム錫（Indium Tin Oxide：ＩＴＯ）膜をエッチングする方法に関する。 The present invention relates to an etching solution composition for an ITO film and an ITO film etching method using the same. More specifically, the present invention has excellent etching ability for ITO transparent conductive film, its composition is stable, reduces erosion to photoreactive substances such as photoresist during the etching process, The present invention relates to an etching solution composition having excellent characteristics that does not leave deposits, and a method of etching an indium tin oxide (ITO) film using the etching solution composition.
液晶表示素子（liquid crystal display device: ＬＣＤ device）は、高解像度による鮮明な映像を提供し、省エネ化および薄膜化も可能である。そのため、平板ディスプレイ装置の中で最も脚光を浴びている。現在、このような液晶表示素子を駆動する電子回路として代表的なものは、薄膜トランジスタ（ＴＦＴ）回路であって、典型的な薄膜トランジスタ液晶表示（ＴＦＴ−ＬＣＤ）素子は、ディスプレイ画面の画素を形成している。 A liquid crystal display device (LCD device) provides a clear image with high resolution, and can be energy-saving and thin. For this reason, it is attracting the most attention among flat panel display devices. At present, a typical electronic circuit for driving such a liquid crystal display element is a thin film transistor (TFT) circuit, and a typical thin film transistor liquid crystal display (TFT-LCD) element forms a pixel of a display screen. ing.
ＴＦＴ−ＬＣＤ素子においてスイッチング素子として作用するＴＦＴはマトリックス状に配列したＴＦＴ用基板と、その基板と対向するカラーフィルター基板との間に、液晶物質を満たして製造したものである。ＴＦＴ−ＬＣＤの全体の製造工程は、ＴＦＴ基板の製造工程と、カラーフィルター工程と、セル工程と、モジュール工程とに大別されるが、正確かつ鮮明な映像を表示するに当り、ＴＦＴ基板およびカラーフィルターの製造工程は非常に重要である。 A TFT acting as a switching element in a TFT-LCD element is manufactured by filling a liquid crystal substance between a TFT substrate arranged in a matrix and a color filter substrate facing the substrate. The entire manufacturing process of a TFT-LCD is roughly divided into a TFT substrate manufacturing process, a color filter process, a cell process, and a module process, and in displaying an accurate and clear image, the TFT substrate and The manufacturing process of the color filter is very important.
ＴＦＴ−ＬＣＤ装置の画素表示電極の製造には、透明な光学的特性を有し、かつ高導電性物質からなる薄膜が必要であるが、現在酸化インジウムを基盤にした酸化インジウム錫（Indium Tin Oxide：ＩＴＯ）と酸化インジウム亜鉛（Indium Zinc Oxide：ＩＺＯ）が透明導電膜の材料として用いられている。 In order to manufacture a pixel display electrode of a TFT-LCD device, a thin film made of a highly conductive material with transparent optical characteristics is required. Currently, indium tin oxide based on indium oxide (Indium Tin Oxide) : ITO) and indium zinc oxide (IZO) are used as materials for the transparent conductive film.
画素表示電極に所望の電気回路のパターンを形成しようとするならば、回路パターン通り薄膜層を削るエッチング過程が必要である。しかし、金属二重層のエッチングに通用される既存のエッチング液としては酸化物であるＩＴＯの強い耐化学性のために、ＩＴＯやＩＺＯ素材の透明導電膜をエッチングし難かった。具体的には、王水（aqua regia、ＨＣｌ＋ＣＨ３ＣＯＯＨ＋ＨＮＯ３）や塩酸第二鉄（ＩＩＩ）の塩酸溶液（ＦｅＣｌ３／ＨＣｌ）、燐酸（Ｈ３ＰＯ４）または臭化水素酸（ＨＢｒ）を利用した透明導電膜ウェットエッチング液が使われてきたが、王水系エッチング液または塩酸第２鉄の塩酸溶液を利用してＩＴＯ膜をエッチングする場合、安価ではあるが、パターンの側面でさらに速くエッチングされてプロファイルが不良となり、かつ主成分である塩酸や硝酸が揮発しやすいために、経時的にエッチング液組成物の変動が激しくなる。また、燐酸の場合、アルミニウム腐食と高粘性および高価の問題、臭化水素酸の場合、高価と猛毒性とが問題となる。シュウ酸（Oxalic Acid）を利用して非晶質ＩＴＯをエッチングしてもよいが、このような場合、ＩＴＯパターン周囲に残渣が発生しやすく、かつ低温でシュウ酸の溶解度が低いために、析出物が発生してエッチング装備の故障を発生させる問題がある。 If a desired electric circuit pattern is to be formed on the pixel display electrode, an etching process is required to cut the thin film layer in accordance with the circuit pattern. However, it is difficult to etch a transparent conductive film made of ITO or an IZO material because of the strong chemical resistance of ITO, which is an oxide, as an existing etchant used for etching a metal double layer. Specifically, aqua regia, HCl + CH 3 COOH + HNO 3 , hydrochloric acid solution of ferric chloride (III) (FeCl 3 / HCl), phosphoric acid (H 3 PO 4 ) or hydrobromic acid (HBr) The transparent conductive film wet etching solution used has been used, but when etching an ITO film using an aqua regia type etching solution or a ferric hydrochloric acid hydrochloric acid solution, it is cheaper, but it is etched faster on the side of the pattern. As a result, the profile becomes poor, and hydrochloric acid and nitric acid, which are the main components, are likely to volatilize, so that the etchant composition fluctuates over time. Further, in the case of phosphoric acid, there are problems of aluminum corrosion and high viscosity and high cost, and in the case of hydrobromic acid, high cost and high toxicity are problems. Oxalic acid may be used to etch amorphous ITO, but in such cases, residue is likely to occur around the ITO pattern and the solubility of oxalic acid is low at low temperatures. There is a problem that an object is generated and a failure of the etching equipment occurs.
本発明の目的は、ＩＴＯ透明導電膜に対して優秀なエッチング性能を有し、その組成が安定的であり、エッチング工程時フォトレジストなどの光反応物質に対する侵食を減少させ、残渣または析出物を残さない優秀な特性を有するエッチング液組成物を提供することを目的とする。 The object of the present invention is to have excellent etching performance with respect to the ITO transparent conductive film, its composition is stable, it reduces erosion to photoreactive substances such as photoresist during the etching process, and residues or precipitates are removed. An object of the present invention is to provide an etching solution composition having excellent characteristics that does not remain.
前記課題を解決するために本発明は、ＩＴＯ膜用のエッチング液組成物の総質量に対して、ａ）硫酸４〜１０質量％、ｂ）硝酸２．５〜６．０質量％、ｃ）エッチング調整剤０．５〜５質量％および組成物総質量を１００質量％にする量の水を含み、前記エッチング調整剤は、ＫＮＯ ３ であることを特徴とするＩＴＯ膜用のエッチング液組成物を提供する。 In order to solve the above-mentioned problems, the present invention provides a) 4 to 10% by mass of sulfuric acid, b) 2.5 to 6.0% by mass of nitric acid, and c) based on the total mass of the etching solution composition for the ITO film. see contains water in an amount of etching modifier 0.5-5 wt% and the composition total weight to 100% by mass, the etching modifier etchant for ITO film, which is a KNO 3 Offer things.
また、本発明は、ＴＦＴ−ＬＣＤ画素表示電極の製造において、ＩＴＯ膜用のエッチング液組成物の総質量に対して、硫酸４〜１０質量％、硝酸２．５〜６．０質量％、エッチング調整剤０．５〜５質量％および組成物総質量を１００質量％にする量の水を含むエッチング液組成物を利用してＩＴＯ膜をエッチングする段階を含み、前記エッチング調整剤は、ＫＮＯ ３ であることを特徴とするＩＴＯ膜のエッチング方法を提供する。 Further, in the production of TFT-LCD pixel display electrodes, the present invention provides 4 to 10% by mass of sulfuric acid, 2.5 to 6.0% by mass of nitric acid, and etching with respect to the total mass of the etchant composition for the ITO film. look including the step of etching the ITO film by using an etchant composition comprising an amount of water for adjusting agent 0.5 to 5% by weight and the composition total weight to 100% by mass, the etching modifier, KNO The method for etching an ITO film is provided.
本発明のＴＦＴ−ＬＣＤのＩＴＯ透明導電膜用のエッチング液組成物は、ＩＴＯ透明導電膜に対して優秀なエッチング能力を有し、エッチング工程時にフォトレジストのような光反応物質に対する浸食を減少させ、残渣または析出物を残さない優秀な特性を有する。また、本発明のエッチング液組成物は、従来のシュウ酸系エッチング液で表される０℃以下でのシュウ酸結晶化現象もなく、塩酸系のエッチング液で表される下部金属膜質に対する影響もない。したがって、ＴＦＴ−ＬＣＤをはじめとする、ＩＴＯ膜を利用する表示装置などの電子部品製造工程において生産性を顕著に向上させ、硫酸のような安価でかつ高安定性成分を活用して、工程時間におけるエッチング液の組成変化を抑え、生産コストを低減できる。 The etching composition for the ITO transparent conductive film of the TFT-LCD of the present invention has an excellent etching ability with respect to the ITO transparent conductive film, and reduces erosion to photoreactive substances such as photoresist during the etching process. It has excellent properties that leave no residue or precipitate. In addition, the etching solution composition of the present invention has no oxalic acid crystallization phenomenon at 0 ° C. or lower, which is represented by a conventional oxalic acid-based etching solution, and has an influence on the lower metal film quality represented by a hydrochloric acid-based etching solution. Absent. Therefore, in the manufacturing process of electronic parts such as TFT-LCD and other display devices using ITO film, the productivity is significantly improved, and inexpensive and highly stable components such as sulfuric acid are utilized to reduce the process time. The production cost can be reduced by suppressing the composition change of the etching solution.
以下、本発明の実施形態について詳細に説明する。
本発明の実施形態に係るエッチング液組成物は、エッチング液組成物総質量に対して、ａ）硫酸４〜１０質量％、ｂ）硝酸２．５〜６．０質量％、ｃ）エッチング調整剤０．５〜５質量％および組成物総質量を１００質量％にする量の水を含む。
エッチング調整剤とは、エッチング液内で容易に解離される物質であって、電解質効果をさらに極大化させ、フォトレジストと金属膜との間の凝着力を減少させ、非晶質ＩＴＯで優秀なエッチング効果を示すように作用する。
Hereinafter, embodiments of the present invention will be described in detail.
The etching solution composition according to the embodiment of the present invention is a) 4 to 10% by mass of sulfuric acid, b) 2.5 to 6.0% by mass of nitric acid, and c) an etching regulator with respect to the total mass of the etching solution composition. 0.5 to 5% by weight and an amount of water which makes the total composition weight 100% by weight are included.
Etching modifier is a material that is easily dissociated in the etchant, further maximizes the electrolyte effect, reduces the adhesion between the photoresist and the metal film, and is excellent in amorphous ITO. It acts to show the etching effect.
この際、エッチング調整剤が０．５質量％未満である場合、フォトレジストと金属膜との凝着力を減少させられず、直進度（Linearity）が落ち、一方、５質量％を超える過度なエッチング調整剤の使用時、エッチング液のコストもかさみ、またフォトレジストが損傷される恐れがある。 At this time, if the etching conditioner is less than 0.5% by mass, the adhesion force between the photoresist and the metal film cannot be reduced, and the linearity decreases, while excessive etching exceeding 5% by mass. When the adjusting agent is used, the cost of the etching solution is increased, and the photoresist may be damaged.
このようなエッチング調整剤としては、カリウム（Ｋ＋）イオンを含有する化合物であって、ＫＮＯ３、ＣＨ３ＣＯＯＫ、ＫＨＳＯ４、ＫＨ２ＰＯ４、Ｋ２ＳＯ４、Ｋ２ＨＰＯ４またはＫ３ＰＯ４などを使用し、望ましくは、ＫＮＯ３またはＣＨ３ＣＯＯＫを使用することができる。 As such an etching regulator, a compound containing potassium (K + ) ions, which is KNO 3 , CH 3 COOK, KHSO 4 , KH 2 PO 4 , K 2 SO 4 , K 2 HPO 4 or K 3 PO 4 or the like is used, and preferably KNO 3 or CH 3 COOK can be used.
硝酸は、インジウム酸化膜に対して優秀なエッチング能力を有し、フォトレジストのような光反応物質に対する浸食を減少させ、残渣が残らないようにする。硝酸が２．５質量％未満含まれている場合、インジウム酸化膜のエッチング速度を低下させ、６質量％を超える場合には、モリブデンおよびアルミニウムのような隣接金属に化学的浸食を発生させる恐れがある。 Nitric acid has excellent etching ability for indium oxide films, reduces erosion to photoreactive materials such as photoresist, and leaves no residue. If nitric acid is contained in an amount of less than 2.5% by mass, the etching rate of the indium oxide film is decreased. If the nitric acid exceeds 6% by mass, chemical erosion may occur in adjacent metals such as molybdenum and aluminum. is there.
硫酸は、主酸化剤であってＩＴＯをエッチングする役割を果たす。このような硫酸は、通常公知の方法によって製造可能であり、特に半導体工程用の純度を有することが望ましい。 Sulfuric acid is a main oxidant and serves to etch ITO. Such sulfuric acid can be produced by a generally known method, and it is particularly desirable that the sulfuric acid has a purity for a semiconductor process.
硫酸が４質量％未満含まれている場合、エッチング速度を低下させ、１０質量％を超える場合、フォトレジストおよび／または隣接金属に化学的浸食を発生させる恐れがある。また、本発明の実施形態に係るエッチング液は、水溶液として前記必須成分の質量比の和に対する残部ほど水を必須的に含めて、全体質量比を１００％にする。この際、使用する水は、超純水であることが望ましい。 When the sulfuric acid is contained in an amount of less than 4% by mass, the etching rate is decreased, and when it exceeds 10% by mass, chemical erosion may occur in the photoresist and / or the adjacent metal. Moreover, the etching liquid which concerns on embodiment of this invention contains water essentially as the remainder with respect to the sum of the mass ratio of the said essential component as aqueous solution, and makes the whole mass ratio 100%. At this time, it is desirable that the water to be used is ultrapure water.
以下、実施例を挙げて発明をさらに詳細に説明する。下記実施例の構成は、あくまでも発明の理解を助けるためのものであり、いかなる場合にも、本発明の技術的範囲を実施例で提示した実施態様に限定しようとするものではない。 Hereinafter, the present invention will be described in more detail with reference to examples. The configurations of the following examples are merely to help understanding of the invention, and in any case, the technical scope of the present invention is not intended to be limited to the embodiments presented in the examples.
下記表１の組成（質量％）によってエッチング液組成物を製造した。エッチング調整剤としてはＫＮＯ３を使用した。 The etching liquid composition was manufactured by the composition (mass%) of the following Table 1. KNO 3 was used as an etching regulator.
（試験例）
前記製造した実施例および本発明者が想定した比較例１〜３のエッチング液に対して、ＩＴＯ透明導電膜に対するそのエッチング能力を比較した。エッチング速度の測定結果は、下記表２に現れており、図１ないし４は、それぞれ実施例および本発明者が想定した比較例１〜３のエッチング液を使用してエッチングを終えたＩＴＯ透明導電膜を電子顕微鏡で観察した写真である。
(Test example)
The etching ability with respect to the ITO transparent conductive film was compared with the etching liquids of the manufactured examples and Comparative Examples 1 to 3 assumed by the inventors. The measurement results of the etching rate appear in Table 2 below, and FIGS. 1 to 4 show ITO transparent conductive materials that have been etched using the etching solutions of Examples and Comparative Examples 1 to 3 assumed by the inventors. It is the photograph which observed the film | membrane with the electron microscope.
前記表２および図１によれば、本発明の前記実施例のエッチング液でエッチングされた場合には、エッチング速度が優秀であり、表面が滑らかで、粒状の残渣が残っていない良好な表面が現れる。 According to Table 2 and FIG. 1, when etched with the etching solution of the above embodiment of the present invention, the etching rate is excellent, the surface is smooth, and a good surface with no granular residue remains. appear.
比較例１のエッチング液を使用した場合、表２および図２によれば、硫酸の含量が本発明の範囲より少ないために、エッチング速度が低下してＩＴＯの残渣が残る。 When the etching solution of Comparative Example 1 is used, according to Table 2 and FIG. 2, since the sulfuric acid content is less than the range of the present invention, the etching rate is lowered and the ITO residue remains.
比較例２のエッチング液でエッチングした場合には、表２および図３によれば、硝酸の含有量が本発明の範囲より少ないために、エッチング速度が低下してＩＴＯの残渣が残る。 When etching is performed with the etching solution of Comparative Example 2, according to Table 2 and FIG. 3, since the nitric acid content is less than the range of the present invention, the etching rate is reduced and the ITO residue remains.
表２および図４によれば、本発明者が想定した比較例３のエッチング液でエッチングした場合には、エッチング速度の低下はないが、エッチング調整剤の含量が本発明の範囲より少ないために、フォトレジストと金属膜との凝着力によって直進度が落ちてパターン不良が引き起こされる。 According to Table 2 and FIG. 4, when etching is performed with the etching solution of Comparative Example 3 assumed by the present inventor, the etching rate does not decrease, but the content of the etching regulator is less than the range of the present invention. The degree of straightness decreases due to the adhesive force between the photoresist and the metal film, causing a pattern defect.
本発明のＩＴＯ膜用のエッチング液組成物およびそれを利用したＩＴＯ膜のエッチング方法は、液晶表示素子関連の製造技術分野に好適に適用され得る。 The etching solution composition for ITO film of the present invention and the etching method of ITO film using the same can be suitably applied to the manufacturing technical field related to liquid crystal display elements.
Claims (2)
ＩＴＯ膜用のエッチング液組成物総質量に対して、硫酸４〜１０質量％、硝酸２．５〜６．０質量％、エッチング調整剤０．５〜５質量％および組成物総質量を１００質量％にする量の水を含むエッチング液組成物を利用して酸化インジウム錫膜をエッチングする段階を含み、4 to 10% by mass of sulfuric acid, 2.5 to 6.0% by mass of nitric acid, 0.5 to 5% by mass of etching regulator and 100% by mass of the composition with respect to the total mass of the etching solution composition for ITO film Etching the indium tin oxide film using an etchant composition comprising water in an amount of
前記エッチング調整剤は、ＫＮＯThe etching regulator is KNO. ３3 であることを特徴とするＩＴＯ膜のエッチング方法。A method for etching an ITO film, wherein:
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| KR1020080008715A KR20090082772A (en) | 2008-01-28 | 2008-01-28 | Etchant composition for indium tin oxide layer and etching method using the same |
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| KR101774484B1 (en) | 2011-02-15 | 2017-09-05 | 삼성디스플레이 주식회사 | Non-halogenated etchant for etching an indium oxide layer and method of manufacturing a display substrate using the non-halogenated etchant |
| CN102585832A (en) * | 2011-12-30 | 2012-07-18 | 江阴江化微电子材料股份有限公司 | Low-tension ITO (Indium Tin Oxide) etching liquid and preparation method thereof |
| KR20140086666A (en) * | 2012-12-28 | 2014-07-08 | 동우 화인켐 주식회사 | Etchant composition for metal oxide layer |
| JP6261926B2 (en) | 2013-09-18 | 2018-01-17 | 関東化學株式会社 | Metal oxide etchant composition and etching method |
| KR102282955B1 (en) * | 2015-02-23 | 2021-07-28 | 동우 화인켐 주식회사 | Etching solution composition for indium oxide layer and manufacturing method of an array substrate for Liquid crystal display using the same |
| CN106479505B (en) * | 2016-09-29 | 2018-09-28 | 杭州格林达电子材料股份有限公司 | A kind of fine etching solution and preparation method thereof for ITO conductive films |
| CN114106835A (en) * | 2021-11-11 | 2022-03-01 | Tcl华星光电技术有限公司 | Etching solution composition and display panel |
| CN116540792B (en) * | 2023-06-25 | 2023-09-12 | 福建天甫电子材料有限公司 | Flow automatic control method and system for preparation of oxalic acid ITO etching solution |
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| JP2000008184A (en) * | 1998-06-24 | 2000-01-11 | Toppan Printing Co Ltd | Etching of multilayer electrically conductive film |
| TWI223661B (en) * | 2000-10-19 | 2004-11-11 | Techno Semichem Co Ltd | Etchant formulation for ITO film |
| KR101191405B1 (en) * | 2005-07-13 | 2012-10-16 | 삼성디스플레이 주식회사 | Etchant and method for fabricating liquid crystal display using the same |
| KR101393599B1 (en) * | 2007-09-18 | 2014-05-12 | 주식회사 동진쎄미켐 | Etchant composition for patterning circuits in thin film transistor-liquid crystal devices |
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| CN101497793A (en) | 2009-08-05 |
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