TWI503401B - Etching composition - Google Patents
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- TWI503401B TWI503401B TW100144791A TW100144791A TWI503401B TW I503401 B TWI503401 B TW I503401B TW 100144791 A TW100144791 A TW 100144791A TW 100144791 A TW100144791 A TW 100144791A TW I503401 B TWI503401 B TW I503401B
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- C—CHEMISTRY; METALLURGY
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- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
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- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
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- C23F1/16—Acidic compositions
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Description
本發明係關於金屬氧化物被膜的蝕刻液組成物，特別係適用於含有銦-錫氧化物(以下簡稱「ITO」)、銦-鋅氧化物(以下簡稱「IZO」)等氧化銦之氧化銦系被膜的加工用之蝕刻液。The present invention relates to an etching liquid composition of a metal oxide film, and particularly to an indium oxide containing indium oxide such as indium-tin oxide (hereinafter referred to as "ITO") or indium-zinc oxide (hereinafter referred to as "IZO"). An etching solution for processing a film.
透明導電膜等所使用之氧化銦系被膜的濕式蝕刻之相關技術，已知有各種技術，從廉價且蝕刻速度佳的觀點而言，大多係將含有鹽酸的水溶液當作蝕刻液組成物使用。但是，鹽酸因為氯化氫的揮發與強腐蝕性，會有臭氣產生、及裝置或被蝕刻基材等的腐蝕劣化問題。又，除此之外，當使用鹽酸的情況，會有難以獲得氧化銦系被膜、與基材或其他層間之蝕刻選擇性的問題。Various techniques are known for wet etching of an indium oxide-based film used for a transparent conductive film or the like. From the viewpoint of inexpensiveness and high etching rate, an aqueous solution containing hydrochloric acid is often used as an etching liquid composition. . However, hydrochloric acid has a problem of odor generation and corrosion deterioration of a device or an etched substrate due to volatilization and strong corrosiveness of hydrogen chloride. Further, in addition to the above, when hydrochloric acid is used, there is a problem in that it is difficult to obtain an etching selectivity between the indium oxide-based film and the substrate or other layers.
為改善此種問題，就未含有鹽酸的氧化銦系被膜之蝕刻液組成物已進行檢討，並有各種報告。例如專利文獻1揭示：為了對由銀或銀合金構成的金屬膜與透明導電膜利用單液施行蝕刻，而含有銅離子、硝酸及氟化合物作為必要成分的組成物。另，作為該必要成分的氟化化合物係例示氟化銨，作為任意成分則揭示了甲酸、醋酸、草酸、檸檬酸等羧酸。In order to improve such a problem, an etchant composition of an indium oxide-based film containing no hydrochloric acid has been reviewed, and various reports have been made. For example, Patent Document 1 discloses a composition in which a metal film made of silver or a silver alloy and a transparent conductive film are etched by a single liquid, and copper ions, nitric acid, and a fluorine compound are contained as essential components. Further, the fluorinated compound as the essential component is exemplified by ammonium fluoride, and as an optional component, a carboxylic acid such as formic acid, acetic acid, oxalic acid or citric acid is disclosed.
再者，專利文獻2揭示含有多元羧酸與氫氟酸鹽的ITO蝕刻液組成物。多元羧酸係例示草酸、檸檬酸，而氟化物鹽係揭示氟化鈉、氟化鉀、氟化銨。Further, Patent Document 2 discloses an ITO etching solution composition containing a polyvalent carboxylic acid and a hydrofluoric acid salt. The polycarboxylic acid is exemplified by oxalic acid and citric acid, and the fluoride salt is disclosed by sodium fluoride, potassium fluoride or ammonium fluoride.
[專利文獻1]日本專利特開2009-206462號公報[Patent Document 1] Japanese Patent Laid-Open Publication No. 2009-206462
[專利文獻2]日本專利特開2010-67823號公報[Patent Document 2] Japanese Patent Laid-Open Publication No. 2010-67823
然而，上述所揭示之蝕刻液組成物的蝕刻速度慢，且蝕刻選擇性亦尚嫌不足。However, the etching rate of the above-described etching liquid composition is slow, and the etching selectivity is also insufficient.
緣是，本發明係為了解決上述問題而完成，其目的在於提供經抑制臭氣產生及裝置或被蝕刻基材等的腐蝕劣化，特別係對氧化銦系被膜呈現充分蝕刻速度與蝕刻選擇性的蝕刻液組成物。The present invention has been made to solve the above problems, and an object thereof is to provide corrosion deterioration which suppresses odor generation and a device or an etched substrate, and the like, and particularly exhibits sufficient etching speed and etching selectivity for an indium oxide film. Etching liquid composition.
本發明者等為解決上述問題經深入鑽研，結果發現藉由將2-羥基乙磺酸與氟化化合物依特定比例併用，便可解決上述問題，遂完成本發明。The inventors of the present invention have intensively studied to solve the above problems, and as a result, have found that the above problems can be solved by using 2-hydroxyethanesulfonic acid in combination with a fluorinated compound in a specific ratio, and the present invention has been completed.
即，本發明的金屬氧化物被膜之蝕刻液組成物係由含有下述成分的水溶液所構成：(A)2-羥基乙磺酸或其鹽依2-羥基乙磺酸換算為5~20質量%；以及(B)從氫氟酸、氟化銨、氟化鉀、氟化鈉及氟化鋰所構成群組中選擇之至少1種氟化化合物0.05~5質量%。That is, the etching liquid composition of the metal oxide film of the present invention is composed of an aqueous solution containing the following components: (A) 2-hydroxyethanesulfonic acid or a salt thereof is converted into 5 to 20 masses in terms of 2-hydroxyethanesulfonic acid. And (B) at least one fluorinated compound selected from the group consisting of hydrofluoric acid, ammonium fluoride, potassium fluoride, sodium fluoride, and lithium fluoride, 0.05 to 5% by mass.
根據本發明，可提供對氧化銦系被膜具有充分蝕刻速度與蝕刻選擇性的蝕刻液組成物。According to the present invention, it is possible to provide an etching liquid composition having a sufficient etching rate and etching selectivity for an indium oxide-based film.
本發明的金屬氧化物被膜之蝕刻液組成物(以下亦簡稱「蝕刻液組成物」)係以：(A)2-羥基乙磺酸或其鹽依2-羥基乙磺酸換算為5~20質量%；以及(B)從氫氟酸、氟化銨、氟化鉀、氟化鈉及氟化鋰所構成群組中選擇之至少1種氟化化合物0.05~5質量%作為必要成分並含有。且，視需要在不致阻礙本發明效果的範圍內，亦可含有添加劑。本發明的蝕刻液組成物較佳係含有上述(A)、(B)成分及視需要使用的添加劑，其餘則為水。The etching liquid composition of the metal oxide film of the present invention (hereinafter also referred to as "etching liquid composition") is characterized in that: (A) 2-hydroxyethanesulfonic acid or a salt thereof is converted into 5 to 20 in terms of 2-hydroxyethanesulfonic acid. And (B) at least one fluorinated compound selected from the group consisting of hydrofluoric acid, ammonium fluoride, potassium fluoride, sodium fluoride, and lithium fluoride, 0.05 to 5% by mass as an essential component and containing . Further, an additive may be contained as long as it does not impair the effects of the present invention. The etching liquid composition of the present invention preferably contains the above-mentioned components (A) and (B) and additives as needed, and the others are water.
作為本發明蝕刻液組成物的(A)成分係2-羥基乙磺酸之鹽的情況之例，可舉例如鈉鹽、鉀鹽、鋰鹽、銨鹽等的水溶性鹽。通常(A)成分係可使用2-羥基乙磺酸。其含有量係依2-羥基乙磺酸換算為5~20質量%、較佳為5~15質量%。若(A)成分的含有量低於上述範圍的下限，便無法獲得充分的蝕刻速度。另一方面，即便(A)成分的含有量多於上述範圍的上限，仍無法提升蝕刻速度，反而導致發生對裝置構件造成腐蝕等不良情況。The example of the case where the component (A) of the etching liquid composition of the present invention is a salt of 2-hydroxyethanesulfonic acid may, for example, be a water-soluble salt such as a sodium salt, a potassium salt, a lithium salt or an ammonium salt. Usually, the (A) component can be 2-hydroxyethanesulfonic acid. The content thereof is 5 to 20% by mass, preferably 5 to 15% by mass in terms of 2-hydroxyethanesulfonic acid. If the content of the component (A) is less than the lower limit of the above range, a sufficient etching rate cannot be obtained. On the other hand, even if the content of the component (A) is more than the upper limit of the above range, the etching rate cannot be increased, and conversely, corrosion of the device member occurs.
本發明之蝕刻液組成物中，(B)成分的氟化化合物係選擇自氫氟酸、氟化銨、氟化鉀、氟化鈉及氟化鋰所構成群組中，該等係可為1種、亦可混合使用2種以上。其中，氟化鉀係從安全性、衛生性的觀點而言屬較佳。(B)之含有量係0.05~5質量%、較佳係0.1~2質量%。又，若(B)之含有量少於上述範圍的下限，則無法獲得充分的蝕刻速度。另一方面，若(B)之含有量多於上述範圍的上限，會有對裝置或基材的腐蝕性變大之不良情況發生。In the etching liquid composition of the present invention, the fluorinated compound of the component (B) is selected from the group consisting of hydrofluoric acid, ammonium fluoride, potassium fluoride, sodium fluoride, and lithium fluoride, and the One type or two or more types may be used in combination. Among them, potassium fluoride is preferred from the viewpoint of safety and hygiene. The content of (B) is 0.05 to 5% by mass, preferably 0.1 to 2% by mass. Further, if the content of (B) is less than the lower limit of the above range, a sufficient etching rate cannot be obtained. On the other hand, if the content of (B) is more than the upper limit of the above range, there is a problem that corrosion of the device or the substrate becomes large.
再者，本發明的蝕刻液組成物中，除上述(A)成分與(B)成分之外，在不致阻礙本發明效果的範圍內，可配合周知添加劑。該添加劑係可舉例如蝕刻液組成物的安定化劑、各成分的可溶化劑、消泡劑、pH調整劑、比重調整劑、黏度調整劑、濕潤性改善劑、螯合劑、界面活性劑等，使用該等時的濃度，一般係在0.001質量%~10質量%的範圍內。Further, in the etching liquid composition of the present invention, in addition to the components (A) and (B) described above, a known additive can be blended insofar as the effects of the present invention are not inhibited. Examples of the additive include a stabilizer for an etching liquid composition, a solubilizing agent for each component, an antifoaming agent, a pH adjuster, a specific gravity adjusting agent, a viscosity adjusting agent, a wettability improving agent, a chelating agent, a surfactant, and the like. The concentration at the time of use is generally in the range of 0.001% by mass to 10% by mass.
本發明的蝕刻液組成物係在對金屬氧化物被膜施行蝕刻時使用。被蝕刻對象的金屬氧化物係可舉例如氧化矽、氧化鋁、氧化鋅、氧化釔、氧化銦、ITO、IZO、鋁-鋅氧化物(AZO)等。本發明的蝕刻液組成物係於該等之中，特別對氧化銦、ITO、IZO等含有氧化銦的氧化銦系被膜顯示良好蝕刻速度。又，對該等氧化銦系被膜特別顯示良好蝕刻選擇性。The etching liquid composition of the present invention is used when etching a metal oxide film. Examples of the metal oxide to be etched include cerium oxide, aluminum oxide, zinc oxide, cerium oxide, indium oxide, ITO, IZO, and aluminum-zinc oxide (AZO). The etching liquid composition of the present invention is such that it exhibits a good etching rate particularly for an indium oxide-based film containing indium oxide such as indium oxide, ITO or IZO. Further, these indium oxide-based coating films particularly exhibit good etching selectivity.
因為本發明的蝕刻液組成物具有上述特性，因而適用於太陽電池、顯示元件、觸控面板或照明器具等所使用之屬於透明導電膜的ITO被膜、IZO被膜之蝕刻。Since the etching liquid composition of the present invention has the above-described characteristics, it is suitable for etching of an ITO film or an IZO film which is a transparent conductive film used in a solar cell, a display element, a touch panel, or a lighting fixture.
在使用本發明之蝕刻液組成物將被膜予以除去時，只要使被加工基材浸漬於上述本發明蝕刻液組成物中、或對被加工基材噴灑本發明蝕刻液組成物等即可。浸漬條件係依照構件的形狀與膜厚等而有所差異，故只要配合該等適當選擇即可，但例如若溫度屬低溫則蝕刻效率會變差，所以較佳係依10~80℃、更佳係依20~60℃實施。When the film is removed using the etching liquid composition of the present invention, the substrate to be processed may be immersed in the above-described etching liquid composition of the present invention, or the etching liquid composition of the present invention may be sprayed onto the substrate to be processed. The immersion conditions differ depending on the shape of the member, the film thickness, and the like. Therefore, it is only necessary to appropriately select such a suitable one. However, if the temperature is low, the etching efficiency is deteriorated, so that it is preferably 10 to 80 ° C or more. Jiashi is implemented at 20~60°C.
利用上述浸漬、噴灑等施行的蝕刻時間並無特別的限定，只要施行直到除去被膜為止的時間即可。若被膜係通常所使用之被膜厚度的膜厚0.01~500μm，則蝕刻只要施行數秒~十數分鐘便可。又，因為本發明蝕刻液組成物的蝕刻選擇性良好，因而即便在被膜的蝕刻結束後仍施行過剩時間的處理，亦不會有基材等遭腐蝕化的問題。特別係對氧化銦系被膜顯示更良好的蝕刻選擇性。The etching time to be performed by the above-described immersion, spraying, or the like is not particularly limited as long as the time until the film is removed is performed. When the film thickness of the film thickness generally used for the film system is 0.01 to 500 μm, the etching may be performed for several seconds to several ten minutes. Moreover, since the etching selectivity of the etching liquid composition of the present invention is good, even if the treatment is performed for an excessive period of time after the etching of the film is completed, there is no problem that the substrate or the like is corroded. In particular, the indium oxide-based film exhibits better etching selectivity.
以下，利用實施例與比較例針對本發明進行詳細說明，惟本發明並不因該等而受限制。Hereinafter, the present invention will be described in detail by way of examples and comparative examples, but the invention is not limited thereto.
將表1所記載濃度的2-羥基乙磺酸、以及表1所記載的氟化化合物調製為含有括號內所記載濃度的蝕刻液組成物No.1~No.10。另外，其餘全部為水。在經調溫為30℃的各個蝕刻液中，浸漬著經在PET薄膜上利用濺鍍形成膜厚125μm之ITO膜的基材，測定直到ITO膜被除去為止的時間。The 2-hydroxyethanesulfonic acid having the concentration shown in Table 1 and the fluorinated compound described in Table 1 were prepared to include etching solution compositions No. 1 to No. 10 having the concentrations described in parentheses. In addition, the rest are all water. In each of the etching liquids adjusted to a temperature of 30 ° C, a substrate on which a ITO film having a film thickness of 125 μm was formed by sputtering on a PET film was immersed, and the time until the ITO film was removed was measured.
表1：實施例的各蝕刻液之主組成與蝕刻速度Table 1: Main composition and etching rate of each etching solution of the examples
調製由經溶解表2所記載溶質之水溶液所構成的比較用蝕刻液組成物A~L。施行與上述實施例同樣的操作，測定直到ITO膜被除去為止的時間。The comparative etching liquid compositions A to L composed of the aqueous solution of the solute described in Table 2 were prepared. The same operation as in the above examples was carried out, and the time until the ITO film was removed was measured.
表2：比較例的各蝕刻液之主組成與蝕刻速度Table 2: Main composition and etching rate of each etching solution of the comparative example
從蝕刻液No.1~10、與比較用蝕刻液組成物A的比較，確認本發明蝕刻液可獲得與鹽酸同等級以上的ITO蝕刻速度。又，從各自含有氟化化合物0.1質量%的蝕刻液No.1、4、10與蝕刻液C、D的比較，得知本發明蝕刻液相較於將2-羥基乙磺酸改變為硫酸、硝酸的情況，可賦予同等級或同等級以上的ITO蝕刻速度。由該等結果可確認到本發明蝕刻液能改善習知蝕刻液中構成問題之臭氣產生、對裝置與被蝕刻基材等的腐蝕劣化、蝕刻選擇性等問題，且為蝕刻速度優異的蝕刻液。From the etching liquid Nos. 1 to 10 and the comparative etching liquid composition A, it was confirmed that the etching liquid of the present invention can obtain an ITO etching rate of the same grade or higher as that of hydrochloric acid. Further, from the comparison of the etching liquids No. 1, 4, and 10 containing 0.1% by mass of the fluorinated compound and the etching liquids C and D, it was found that the etching liquid phase of the present invention was changed to sulfuric acid by changing the 2-hydroxyethanesulfonic acid. In the case of nitric acid, it is possible to impart an ITO etching rate of the same grade or higher. From these results, it was confirmed that the etching liquid of the present invention can improve the problem of odor generation in the conventional etching solution, corrosion deterioration of the device and the substrate to be etched, etching selectivity, and the like, and is excellent in etching rate. liquid.
再者，由含有2-羥基乙磺酸10質量%與氟化化合物0.5質量%的蝕刻液No.6、與分別含有氟化化合物0.5質量%的比較用蝕刻液E、F、G進行比較，可確認本發明蝕刻液相較於將2-羥基乙磺酸改變為其他有機酸的情況，可賦予同等級以上的ITO蝕刻速度。Further, the etching liquid No. 6 containing 10% by mass of 2-hydroxyethanesulfonic acid and 0.5% by mass of the fluorinated compound was compared with the etching liquids E, F, and G for comparison containing 0.5% by mass of the fluorinated compound, respectively. It was confirmed that the etching liquid phase of the present invention can be imparted to the ITO etching rate of the same grade or higher as compared with the case where the 2-hydroxyethanesulfonic acid is changed to another organic acid.
再者，由蝕刻液No.1~10與比較用蝕刻液H、I、J、K、L的比較(例如No.3與I的比較)，可確認到本發明蝕刻液相較於將氟化化合物改變為氯化化合物的情況，可賦予優異蝕刻速度。Further, by comparison of the etching liquid Nos. 1 to 10 with the comparative etching liquids H, I, J, K, and L (for example, comparison of No. 3 and I), it was confirmed that the etching liquid phase of the present invention is more fluorine-containing. When the compound is changed to a chlorinated compound, an excellent etching rate can be imparted.
針對上述實施例1所記載之蝕刻液No.6、與比較例1所記載之蝕刻液F，施行對鋁及鈦的腐蝕試驗。腐蝕試驗係將各基材的測試片(5cm×2.5cm×厚度1mm)在40℃蝕刻液中浸漬7小時，依浸漬後的質量減少程度施行評價。結果如表3所示。Corrosion tests on aluminum and titanium were carried out on the etching liquid No. 6 described in the first embodiment and the etching liquid F described in the comparative example 1. In the corrosion test, the test piece (5 cm × 2.5 cm × thickness 1 mm) of each substrate was immersed in an etching solution at 40 ° C for 7 hours, and evaluated according to the degree of mass reduction after immersion. The results are shown in Table 3.
表3：對鋁及鈦的腐蝕試驗Table 3: Corrosion tests on aluminum and titanium
由上述可確認到本發明蝕刻液No.6相較於將2-羥基乙磺酸改變為草酸的情況，對鋁及鈦的腐蝕性較小。From the above, it was confirmed that the etching liquid No. 6 of the present invention is less corrosive to aluminum and titanium than the case where 2-hydroxyethanesulfonic acid is changed to oxalic acid.
使用上述實施例1所記載之蝕刻液No.6及No.7，針對50nm氧化釔膜、30nm氧化矽膜的各被膜施行蝕刻試驗。具體而言係將各個膜基材浸漬於45℃蝕刻液中，浸漬15分鐘。結果確認到各個膜均被除去。An etching test was performed on each of the 50 nm yttrium oxide film and the 30 nm yttrium oxide film using the etching liquid No. 6 and No. 7 described in the above Example 1. Specifically, each film substrate was immersed in an etching solution at 45 ° C and immersed for 15 minutes. As a result, it was confirmed that each film was removed.
Claims (4)
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| TWI488943B (en) * | 2013-04-29 | 2015-06-21 | Chi Mei Corp | Etching paste composition and the application thereof |
| JP6261926B2 (en) | 2013-09-18 | 2018-01-17 | 関東化學株式会社 | Metal oxide etchant composition and etching method |
| JP6350008B2 (en) * | 2014-06-20 | 2018-07-04 | 三菱瓦斯化学株式会社 | Etching solution and etching method of oxide containing at least indium, gallium, zinc and silicon |
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