TW201910539A - Oxide sintered body and sputtering target - Google Patents
Oxide sintered body and sputtering target Download PDFInfo
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Abstract
Description
本發明係有關氧化物燒結體及濺鍍靶，詳而言之，係有關一種可得到在可見光區域具有高透射率及低電阻之薄膜的濺鍍靶，以及可製作如此之靶的氧化物燒結體。 The present invention relates to an oxide sintered body and a sputtering target, and in particular, it relates to a sputtering target capable of obtaining a thin film having high transmittance and low resistance in a visible light region, and an oxide sintering method capable of producing such a target body.
隨著以液晶為中心之顯示裝置的發展而對透明導電膜的需求增加。透明導電膜被要求高透明性，進而亦要求低電阻。由於高透明性及低電阻的需求，廣泛地使用ITO膜作為透明導電膜。就ITO透明導電膜的形成方法而言，從操作性的簡便度之觀點而言，一般的方法係將ITO濺鍍靶進行濺鍍而成膜。 With the development of liquid crystal-centric display devices, the demand for transparent conductive films has increased. Transparent conductive films are required to have high transparency and further low resistance. Due to the requirements of high transparency and low resistance, ITO films are widely used as transparent conductive films. As for the method for forming the ITO transparent conductive film, a general method is to form a film by sputtering an ITO sputtering target in terms of ease of operation.
尤其在最近，隨著液晶之彩色化、元件之精細化及主動矩陣方式之採用，需要透明性更高，且電阻低的高性能之ITO透明導電膜。 Especially recently, with the colorization of liquid crystals, the refinement of components, and the use of active matrix methods, high-performance ITO transparent conductive films with higher transparency and low resistance are required.
專利文獻1中記載一種包含1至20重量%之氧化錫及0.05至5重量%之氧化鈦的高透射率、低電阻的透明導電膜，以及濺鍍靶，又記載可藉由在300℃進行熱處理亦即退火處理，而可達成透明導電膜的高透射率化、低電阻化。 Patent Document 1 describes a high-transmittance, low-resistance transparent conductive film containing 1 to 20% by weight of tin oxide and 0.05 to 5% by weight of titanium oxide, and a sputtering target. It is also described that it can be performed at 300 ° C. Heat treatment, that is, annealing treatment, can achieve high transmittance and low resistance of the transparent conductive film.
專利文獻2中記載一種透明導電膜之製造方法，係將包含氧化銦、氧化錫及鈦等之氧化物的濺鍍靶進行濺鍍，再將所得之銦錫氧化物薄膜藉由熱處理使其結晶化之方法。在該方法中，藉由將經濺鍍而得之非晶質的銦錫氧化物薄膜以200℃以上之熱處理使其結晶，而可降低薄膜之比電阻且提高導電特性。 Patent Document 2 describes a method for manufacturing a transparent conductive film, which comprises sputtering a sputtering target including oxides of indium oxide, tin oxide, and titanium, and crystallizing the obtained indium tin oxide film by heat treatment. Method of transformation. In this method, the amorphous indium tin oxide thin film obtained by sputtering is crystallized by a heat treatment at 200 ° C. or higher, thereby reducing the specific resistance of the thin film and improving the conductive characteristics.
然而，必須在200℃以上之高溫進行熱處理的方法，要在會於200℃以上的時候變形的樹脂製的薄膜上製作透明導電膜的情況下則無法應用。 However, a method that requires heat treatment at a high temperature of 200 ° C or higher cannot be applied when a transparent conductive film is produced on a resin film that will deform at 200 ° C or higher.
[專利文獻1]日本特開平4-277408號公報 [Patent Document 1] Japanese Patent Laid-Open No. 4-277408
[專利文獻2]日本專利第5726752號公報 [Patent Document 2] Japanese Patent No. 5726752
本發明之目的係提供一種能夠使薄膜成膜之濺射靶濺射靶，該薄膜即使不經過高溫熱處理亦可得到透明性高且電阻低的透明導電膜。 An object of the present invention is to provide a sputtering target capable of forming a thin film, and the thin film can obtain a transparent conductive film having high transparency and low resistance even without being subjected to high-temperature heat treatment.
本發明之氧化物燒結體，其構成元素為In、Sn、Ti及O，其中，In之含有比率以In2O3計為88.0至98.2質量%、Sn之含有比率以SnO2計為1.0至8.0質量%、Ti之含有比率以TiO2計為0.8至4.0質量%。 In the oxide sintered body of the present invention, the constituent elements are In, Sn, Ti, and O. Among them, the content ratio of In is 88.0 to 98.2% by mass as In 2 O 3 , and the content ratio of Sn is 1.0 to SnO 2 . 8.0% by mass, and the content ratio of Ti is 0.8 to 4.0% by mass as TiO 2 .
上述氧化物燒結體，其比電阻係以5.0×10-4Ω cm以下為佳，相對密度係以95%以上為佳。 The oxide sintered body preferably has a specific resistance of 5.0 × 10 -4 Ω cm or less, and a relative density of 95% or more.
本發明之濺鍍靶材係包含上述氧化物燒結體。 The sputtering target material of this invention contains the said oxide sintered compact.
本發明之濺鍍靶係將上述濺鍍靶材與基材接合而成者。 The sputtering target of the present invention is obtained by joining the above-mentioned sputtering target to a substrate.
本發明之透明導電膜中，In之含有比率以In2O3計為88.0至98.2質量%、Sn之含有比率以SnO2計為1.0至8.0質量%、Ti之含有比率以TiO2計為0.8至4.0質量%。 In the transparent conductive film of the present invention, the content ratio of In is 88.0 to 98.2% by mass as In 2 O 3 , the content ratio of Sn is 1.0 to 8.0% by mass as SnO 2 , and the content ratio of Ti is 0.8 as TiO 2 To 4.0% by mass.
本發明之透明導電膜的製造方法，係藉由將上述濺鍍靶進行濺鍍而成膜，將成膜得到之薄膜在110至145℃進行加熱處理。 The manufacturing method of the transparent conductive film of the present invention is to form a film by sputtering the above-mentioned sputtering target, and heat-treat the obtained thin film at 110 to 145 ° C.
藉由本發明之氧化物燒結體，可得到能夠使薄膜成膜之濺射靶，該薄膜即使不經過高溫熱處理亦可得到透明性高之透明導電膜、甚至是電阻低的透明導電。 With the oxide sintered body of the present invention, a sputtering target capable of forming a thin film can be obtained, and the thin film can obtain a transparent conductive film with high transparency and even a transparent conductive film with low resistance even without undergoing high-temperature heat treatment.
第1圖係顯示在實施例15中，經濺鍍而得之薄膜以及藉由將該薄膜在125℃進行熱處理而得的透明導電膜在波長300nm至800nm的範圍內之光透射率之圖。 FIG. 1 is a graph showing the light transmittance of a thin film obtained by sputtering in Example 15 and a transparent conductive film obtained by heat-treating the thin film at 125 ° C. in a wavelength range of 300 nm to 800 nm.
第2圖係顯示在實施例15及比較例1、3中，藉由將經濺鍍而得之薄膜在125℃進行熱處理而得的透明導電膜在波長300nm至800nm的範圍內之光透射率之圖。 Figure 2 shows the light transmittance of a transparent conductive film obtained by heat-treating a thin film obtained by sputtering at 125 ° C in Example 15 and Comparative Examples 1 and 3 at a wavelength of 300 nm to 800 nm. Figure.
本發明之氧化物燒結體，其構成元素為In、Sn、Ti及O，In之含有比率以In2O3計為88.0至98.2質量%、Sn之含有比率以SnO2計為1.0至8.0質量%、Ti之含有比率以TiO2計為0.8至4.0質量%。 The oxide sintered body of the present invention includes In, Sn, Ti, and O as constituent elements. The content ratio of In is 88.0 to 98.2% by mass as In 2 O 3 , and the content ratio of Sn is 1.0 to 8.0 as SnO 2 . The content ratios of% and Ti are 0.8 to 4.0% by mass as TiO 2 .
上述氧化物燒結體中，In之含有比率以In2O3計為88.0至98.2-質量%，以90.0至97.0質量%為佳，以91.5至96.0質量%更佳，以93.0至95.5質量%又更佳；Sn之含有比率以SnO2計為1.0至8.0質量%，以2.0至7.0質量%為佳，以2.7至6.0質量%更佳，以3.0至5.0質量%又更佳；Ti之含有比率以TiO2計為0.8至4.0質量%，以1.0至3.0質量%為佳，以1.3至2.5質量%更佳，以1.5至2.0質量%又更佳。當然，如本發明之氧化物燒結體中，理所當然可包含源自原料等之無可避免的雜質，本發明之氧化物燒結體中亦有包含無可避免的雜質之情形。本發明之氧化物燒結體中之無可避免的雜質可列舉如：Fe、Cr、Ni、Si、W、Zr等，該等之含量一般各為100ppm以下。 In the above oxide sintered body, the content of In is 88.0 to 98.2% by mass as In 2 O 3 , preferably 90.0 to 97.0% by mass, more preferably 91.5 to 96.0% by mass, and 93.0 to 95.5% by mass. more preferably; the content ratio of Sn in terms of SnO 2 mass%, 1.0 to 8.0, to preferably 2.0 to 7.0 mass%, more preferably at 2.7 to 6.0 mass%, 3.0%, and more preferably 5.0 mass; the content ratio of Ti TiO 2 is 0.8 to 4.0% by mass, more preferably 1.0 to 3.0% by mass, more preferably 1.3 to 2.5% by mass, and even more preferably 1.5 to 2.0% by mass. Of course, as the oxide sintered body of the present invention, it is a matter of course that unavoidable impurities derived from raw materials and the like may be included, and the oxide sintered body of the present invention may contain unavoidable impurities. Examples of the unavoidable impurities in the oxide sintered body of the present invention include Fe, Cr, Ni, Si, W, and Zr. The content of each of these is generally 100 ppm or less.
另外，本發明中，所謂的構成元素係指氧化物燒結體或透明導電膜中除了無可避免之雜質以外的構成元素之意，各構成元素之含有比率係指在氧化物燒結體或透明導電膜全體中所佔之各構成元素的含有比率之意。 In addition, in the present invention, the so-called constituent elements refer to constituent elements other than unavoidable impurities in the oxide sintered body or the transparent conductive film, and the content ratio of each constituent element refers to the oxide sintered body or the transparent conductive film. The content ratio of each constituent element in the entire film is intended.
上述氧化物燒結體之比電阻係以5.0×10-4Ω cm以下為佳，以4.8×10-4Ω cm以下更佳，以4.5×10-4Ω cm以下又更佳。藉此可使用廉價的DC電源進行濺射，可提高成膜速度，並且可抑制異常放電的發生。 The specific resistance of the oxide sintered body is preferably 5.0 × 10 -4 Ω cm or less, more preferably 4.8 × 10 -4 Ω cm or less, and even more preferably 4.5 × 10 -4 Ω cm or less. Thereby, sputtering can be performed using an inexpensive DC power source, the film-forming speed can be increased, and the occurrence of abnormal discharge can be suppressed.
上述氧化物燒結體之相對密度係以95%以上為佳，以98%以上更佳，以99%以上又更佳。相對密度為95%以上時，不會生結塊或電弧，可有效率地進行濺鍍。相對密度之上限並無特別限制，可超出100%。上述相對密度係基於阿基米德所測得之數值。 The relative density of the oxide sintered body is preferably 95% or more, more preferably 98% or more, and even more preferably 99% or more. When the relative density is 95% or more, no caking or arcing occurs, and sputtering can be performed efficiently. The upper limit of the relative density is not particularly limited and may exceed 100%. The above relative densities are based on values measured by Archimedes.
上述氧化物燒結體係可藉由例如以下所示之方法製造。 The above-mentioned oxide sintering system can be produced by, for example, the method shown below.
首先，將原料粉末混合。原料粉末一般為In2O3粉末、SnO2粉末及TiO2粉末。In2O3粉末、SnO2粉末及TiO2粉末係以使所得之燒結體中的In、Sn及Ti的含量分別成為上述範圍內之方式混合。而且，將原料粉末混合而得之混合粉末中的In2O3粉末、SnO2粉末及TiO2粉末之含量比係分別與上述氧化物燒結體中之以In2O3計之含量比、以SnO2計之Sn含量比及以TiO2計之Ti含量比為一致。 First, the raw material powder is mixed. The raw material powder is generally In 2 O 3 powder, SnO 2 powder, and TiO 2 powder. The In 2 O 3 powder, SnO 2 powder, and TiO 2 powder are mixed so that the contents of In, Sn, and Ti in the obtained sintered body fall within the above ranges, respectively. In addition, the content ratios of the In 2 O 3 powder, the SnO 2 powder, and the TiO 2 powder in the mixed powder obtained by mixing the raw material powders are respectively the content ratios in terms of In 2 O 3 and The Sn content ratio in terms of SnO 2 is consistent with the Ti content ratio in terms of TiO 2 .
由於各原料粉末一般係粒子呈現凝聚者，因此以事先進行粉碎而混合、或一面混合一面進行粉碎者為佳。 Since each raw material powder generally has particles agglomerated, it is preferable to perform pulverization and mixing in advance, or pulverization while mixing.
原料粉末之粉碎方法或混合方法並無特別限制，例如可將原料粉末饋入罐中並以球磨機進行粉碎或混合。 The method for pulverizing or mixing the raw material powder is not particularly limited. For example, the raw material powder may be fed into a tank and pulverized or mixed with a ball mill.
所得之混合粉末可直接成型而作成成型體並予以燒結，但亦可依所需在混合粉末中添加黏合劑進行成型而作成成型體。此黏合劑可使用在習知的粉末冶金法中要得到成型體時使用的黏合劑，例如聚乙烯醇、丙烯酸乳液黏合劑等。而且，亦可在混合粉末中添加分散介質而 調製成漿體，再將該漿體進行噴霧乾燥而製作顆粒，並使該顆粒成型。 The obtained mixed powder can be directly molded into a molded body and sintered, but a binder can be added to the mixed powder to form the molded body as required. This adhesive can be used in the conventional powder metallurgy method to obtain a molded body, such as polyvinyl alcohol, acrylic emulsion adhesive, and the like. Further, a dispersion medium may be added to the mixed powder to prepare a slurry, and the slurry may be spray-dried to produce pellets, and the pellets may be formed.
成型方法係可使用以往粉末冶金法中所採用的方法，例如冷噴塗(cold spray)及CIP(冷均壓：cold isostatic pressing)等。 The molding method can be a method used in the conventional powder metallurgy method, such as cold spray and cold isostatic pressing (CIP).
而且，可預先將混合粉末暫時壓製以製作臨時成型體，並且對將其粉碎而得的粉碎粉末進行正式壓製，藉此製作成型體。 In addition, the mixed powder may be temporarily pressed in advance to produce a temporary formed body, and the pulverized powder obtained by pulverizing the mixed powder may be formed into a pressed body.
而且，亦可使用滑鑄法等濕式成型法等製而製作型體。 In addition, a molded body can also be produced using a wet molding method such as a slip casting method.
所得的成型體係可依所需藉由以往粉末冶金法中所採用的方法進行脫脂。成型體之密度一般為50至75%。 The obtained molding system can be degreased by a method adopted in the conventional powder metallurgy method as required. The density of the molded body is generally 50 to 75%.
接著，將所得之成型體進行燒製而製作氧化物燒結體。燒製時所使用的燒製爐只要係在冷卻時可控制冷卻速度者即可，並無特別限制，亦可使用粉末冶金時一般所使用的燒製爐。燒製環境係以氧環境為適合。 Next, the obtained molded body is fired to produce an oxide sintered body. The firing furnace used for firing is not particularly limited as long as it can control the cooling rate during cooling, and a firing furnace generally used in powder metallurgy can also be used. The firing environment is suitable for an oxygen environment.
從高密度及防裂的觀點來看，升溫速度一般為100至500℃/h。燒製溫度為1300至1600℃，以1400至1600℃為佳。燒製溫度在上述範圍內時，可得到高密度之氧化物燒結體。在上述燒製溫度的滯留時間(retention time)一般為3至30h，以5至20h為佳，滯留時間在上述範圍內時，容易得到高密度之氧化物燒結體。 From the viewpoint of high density and crack prevention, the heating rate is generally 100 to 500 ° C / h. The firing temperature is 1300 to 1600 ° C, preferably 1400 to 1600 ° C. When the firing temperature is within the above range, a high-density oxide sintered body can be obtained. The retention time at the firing temperature is generally 3 to 30 hours, preferably 5 to 20 hours. When the retention time is within the above range, a high-density oxide sintered body is easily obtained.
冷卻溫度一般為300℃/hr以下，以50℃/hr以下為佳。 The cooling temperature is generally below 300 ° C / hr, preferably below 50 ° C / hr.
本發明之濺鍍靶材係包含上述氧化物燒結 體。具體而言，將上述氧化物燒結體因應所需切取成所要的形狀，並施予進行研磨等之加工，藉此可得到濺鍍靶材。 The sputtering target of the present invention includes the above-mentioned oxide sintered body. Specifically, the above-mentioned oxide sintered body is cut into a desired shape as needed, and subjected to processing such as grinding, thereby obtaining a sputtering target.
關於該濺鍍靶材之組成及比電阻、相對密度等之物性值，係與上述氧化物燒結體之組成、比電阻、相對密度等為相同。 The physical properties of the sputtering target, such as the composition, specific resistance, and relative density, are the same as the composition, specific resistance, and relative density of the oxide sintered body.
藉由將上述濺鍍靶材與基材接合而可得到濺鍍靶。基材一般為Cu、Al、Ti或不鏽鋼製者。接合材係可使用以往ITO靶材在接合時所使用的接合材，例如In金屬。接合方法亦與以往之ITO靶材的接合方法相同。 A sputtering target can be obtained by joining the said sputtering target and a base material. The substrate is generally made of Cu, Al, Ti or stainless steel. As the bonding material, a conventional bonding material used for bonding the ITO target, such as In metal, can be used. The bonding method is also the same as that of the conventional ITO target.
藉由將上述濺鍍靶進行濺鍍而可使薄膜成膜。濺鍍係可根據使用一般的ITO濺鍍靶之濺鍍的條件進行。 A thin film can be formed by sputtering the sputtering target. The sputtering system can be performed according to sputtering conditions using a general ITO sputtering target.
依如此方式而得的薄膜一般為非晶質者。藉由將該薄膜進行熱處理亦即退火，可使環結晶化，並可得到光透射率高且比電阻低的透明導電膜。就光透射率而言，特別是在短波長區域例如300至380nm波長區域的光透射率可得到顯著地提高。 The thin film obtained in this way is generally amorphous. By heat-treating, that is, annealing, the thin film, the ring can be crystallized, and a transparent conductive film having high light transmittance and low specific resistance can be obtained. In terms of light transmittance, the light transmittance can be significantly improved, particularly in a short wavelength region, such as a wavelength region of 300 to 380 nm.
該熱處理所需的溫度為110℃至145℃，以115℃至140℃為佳，以120℃至135℃更佳。如上所述，以往習知之為了使ITO薄膜高透射率化、低電阻化所進行的熱處理，需要200℃以上的溫度。相對於此，為了使藉由將本發明之濺鍍靶進行濺鍍而得的薄膜高透射率化、低電阻化所進行的熱處理之溫度，可設在110至145℃之低溫。因此，若使用本發明之濺鍍靶，即使要在會於200℃以上 的時候引起變形等之樹脂製的薄膜等之上製作透明導電膜的情況下，也不會引起薄膜等之變形等，而可製作具有光透射率高及低電阻的透明導電膜。另一方面，在超出145℃之溫度下進行熱處理時，無法得到充分的高透射率化及低電阻化，反而會有比起以往的ITO膜(In2O3：SnO2=90：10(質量比))透射率變低且比電阻變高之傾向，因而不佳。 The temperature required for this heat treatment is 110 ° C to 145 ° C, preferably 115 ° C to 140 ° C, and more preferably 120 ° C to 135 ° C. As described above, the heat treatment conventionally known for increasing the transmittance and reducing the resistance of the ITO film requires a temperature of 200 ° C. or higher. In contrast, the temperature of the heat treatment for increasing the transmittance and reducing the resistance of the thin film obtained by sputtering the sputtering target of the present invention can be set to a low temperature of 110 to 145 ° C. Therefore, if the sputtering target of the present invention is used, even if a transparent conductive film is to be formed on a resin film or the like that causes deformation at a temperature of 200 ° C or higher, the film or the like will not be deformed. A transparent conductive film having high light transmittance and low resistance can be produced. On the other hand, when heat treatment is performed at a temperature exceeding 145 ° C, sufficient high transmittance and low resistance cannot be obtained, and there is a possibility that compared with the conventional ITO film (In 2 O 3 : SnO 2 = 90: 10 ( Mass ratio)) The transmittance tends to be low and the specific resistance tends to be high, which is not good.
上述熱處理所需的時間一般為0.1至2小時，以0.5至1小時為佳。上述熱處理可在大氣中進行。 The time required for the heat treatment is generally 0.1 to 2 hours, and preferably 0.5 to 1 hour. The heat treatment may be performed in the atmosphere.
對於藉由將本發明之濺鍍靶進行濺鍍而得的薄膜，可藉由施予上述熱處理而提高光透射率及比電阻。 The thin film obtained by sputtering the sputtering target of the present invention can improve the light transmittance and specific resistance by applying the heat treatment.
藉由在上述溫度施予熱處理，在可見光之波長區域(例如380至750nm)之波長區域中，更特別是在短波長區域(例如300至380nm)中，尤其可使光透射率變得比以往習知的ITO薄膜(In2O3：SnO2=90：10(質量比))更高。 By applying heat treatment at the above-mentioned temperature, in the wavelength region of the visible light wavelength region (for example, 380 to 750 nm), and more particularly in the short wavelength region (for example, 300 to 380 nm), the light transmittance can be made higher than ever The conventional ITO film (In 2 O 3 : SnO 2 = 90: 10 (mass ratio)) is higher.
依如此方式而得的透明導電膜係具有In、Sn、Ti及O作為構成元素，例如：In之含有比率以In2O3計為88.0至98.2質量%，以90.0至97.0質量%為佳，以91.5至96.0質量%更佳，以93.0至95.5質量%又更佳；Sn之含有比率以SnO2計為1.0至8.0質量%，以2.0至7.0質量%為佳，以2.7至6.0質量%更佳，以3.0至5.0質量%又更佳；Ti之含有比率以TiO2計為0.8至4.0質量%，以1.0至3.0質量%為佳，以1.3至2.5質量%更佳，以1.5至2.0質量%又更佳。該透明導電膜係如上所述，具有高的光透射率，並可具有低電阻。 The transparent conductive film obtained in this way has In, Sn, Ti, and O as constituent elements. For example, the content ratio of In is 88.0 to 98.2% by mass as In 2 O 3 , and preferably 90.0 to 97.0% by mass. 91.5 to 96.0% by mass is more preferable, and 93.0 to 95.5% by mass is even better; the content ratio of Sn is 1.0 to 8.0% by mass as SnO 2 , 2.0 to 7.0% by mass is preferable, and 2.7 to 6.0% by mass is more Jia, 3.0 and more preferably 5.0 mass%; the content ratio of Ti in terms of TiO 2 is from 0.8 to 4.0 mass%, 1.0 to 3.0 mass%, preferably, more preferably to 1.3 to 2.5 mass%, to 1.5 to 2.0 mass % Is even better. As described above, the transparent conductive film has high light transmittance and low resistance.
下述實施例及比較例中使用之測定方法顯示如下。 The measurement methods used in the following examples and comparative examples are shown below.
氧化物燒結體之相對密度係根據阿基米德法測定。具體而言，將氧化物燒結體之空氣中質量除以體積(氧化物燒結體之水中質量/測量溫度的水比重)，以根據下述式(X)得到的理論密度ρ(g/cm3)的百分比值作為相對密度(單位：%)。 The relative density of the oxide sintered body was measured according to the Archimedes method. Specifically, the mass in air of the oxide sintered body is divided by the volume (mass in water of the oxide sintered body / water specific gravity at the measurement temperature) to obtain a theoretical density ρ (g / cm 3 according to the following formula (X) ) As the relative density (unit:%).
[數1]ρ=((C1/100)/ρ 1+(C2+100)/ρ 2+…+(Ci/100)/ρ i)-1 (X)(式中之C1至Ci係分別表示氧化物燒結體之構成物質的含量(質量%)，ρ 1至ρ i係表示對應於C1至Ci之各構成物質的密度(g/cm3)。) [Number 1] ρ = ((C1 / 100) / ρ 1+ (C2 + 100) / ρ 2 +… + (Ci / 100) / ρ i) -1 (X) (where C1 to Ci in the formula are respectively It represents the content (mass%) of constituent materials of the oxide sintered body, and ρ 1 to ρ i represent the density (g / cm 3 ) of each constituent material corresponding to C1 to Ci.)
下述實施例及比較例中，由於氧化物燒結體之製造中使用的物質(原料)係In2O3、SnO2、TiO2，因此可藉由將例如下述C1、ρ 1、C2、ρ 2、C3、ρ 3應用於式(X)而計算出理論密度ρ。 In the following examples and comparative examples, since the substance (raw material) used in the production of the oxide sintered body is In 2 O 3 , SnO 2 , and TiO 2 , for example, the following C1, ρ1, C2, and C2 can be used. ρ2, C3, ρ3 are applied to formula (X) to calculate the theoretical density ρ.
C1：氧化物燒結體中使用的In2O3原料之質量% C1: mass% of In 2 O 3 raw material used in oxide sintered body
ρ 1：In2O3之密度(7.18g/cm3) ρ 1: Density of In 2 O 3 (7.18g / cm 3 )
C2：氧化物燒結體中使用的SnO2原料之質量% C2: mass% of SnO 2 raw material used in oxide sintered body
ρ 2：SnO2之密度(6.95g/cm3) ρ 2: Density of SnO 2 (6.95g / cm 3 )
C3：氧化物燒結體中使用的TiO2原料之質量% C3: mass% of TiO 2 raw material used in oxide sintered body
ρ 3：TiO2之密度(4.26g/cm3) ρ 3: Density of TiO 2 (4.26g / cm 3 )
氧化物燒結體之比電阻係使用三菱化學公司製造之Loresta(註冊商標)HP MCP-T410(串聯四探針TYPE ESP)，將探針抵接在加工後之燒結體表面，並以AUTO RANGE模式測定。測定點係設為氧化物燒結體之中央附近及4個角落共計5處，並以各測定值之平均值作為該燒結體的容積電阻值。 The specific resistance of the oxide sintered body uses Loresta (registered trademark) HP MCP-T410 (series four-probe TYPE ESP) manufactured by Mitsubishi Chemical Corporation, and the probe is abutted against the surface of the sintered body after processing, and in the AUTO RANGE mode Determination. The measurement points were set at five locations near the center and four corners of the oxide sintered body, and the average value of each measurement value was used as the volume resistance value of the sintered body.
膜的光透射率係使用日立高科技公司製造之紫外-可見光近紅外分光光度計UH4150測定。測定條件係設定為掃描速度：600nm/min、波長區域：200至2600nm。首先，在裝置中設置未進行成膜之基礎玻璃基板並測定基線，然後測定各個成膜試樣的透射率。 The light transmittance of the film was measured using an ultraviolet-visible near-infrared spectrophotometer UH4150 manufactured by Hitachi High-Tech. The measurement conditions were set to a scanning speed of 600 nm / min and a wavelength region of 200 to 2600 nm. First, a base glass substrate on which no film formation has been performed is set in the apparatus, a baseline is measured, and then the transmittance of each film formation sample is measured.
透明導電膜之薄膜比電阻係使用共和理研公司製造之四點探針測量儀K-705RS測定。 The specific resistance of the thin film of the transparent conductive film was measured using a four-point probe measuring instrument K-705RS manufactured by Kyowa Riken.
使用球磨機將In2O3粉末、SnO2粉末及TiO2粉末以表1所示之比率進行混合，調製成混合粉末。 Using a ball mill, In 2 O 3 powder, SnO 2 powder, and TiO 2 powder were mixed at a ratio shown in Table 1 to prepare a mixed powder.
在上述混合粉末中，添加相對於混合粉末為6質量%之已稀釋至4質量%的聚乙烯醇，使用乳缽使聚乙烯醇充分塗於粉末，並通過5.5網孔的篩網。將所得粉末以200kg/cm2之條件進行臨時壓製，將所得臨時成型體以乳缽粉碎。將所得粉碎粉充填至壓製用的模具中，並在1t/cm2之壓製壓力下成型60秒鐘，得到成型體。 To the mixed powder, 6% by mass of polyvinyl alcohol diluted to 4% by mass relative to the mixed powder was added, and the polyvinyl alcohol was fully applied to the powder using a mortar, and passed through a 5.5-mesh sieve. The obtained powder was temporarily pressed under the conditions of 200 kg / cm2, and the obtained temporarily formed body was pulverized in a mortar. The obtained pulverized powder was filled into a mold for pressing, and was molded under a pressing pressure of 1 t / cm 2 for 60 seconds to obtain a molded body.
將所得成型體放入燒結爐中，以10L/min的速度使氧氣流入爐內，將燒製環境變為氧氣流環境，且以升溫速度設為350℃/h、燒結溫度設為1550℃、在燒結溫度的滯留時間設為9小時的方式進行燒結。 The obtained compact was placed in a sintering furnace, and oxygen was flowed into the furnace at a rate of 10 L / min. The firing environment was changed to an oxygen flow environment. Sintering was performed so that the residence time of the sintering temperature was 9 hours.
然後，以降溫速度100℃/h冷卻，得到氧化物燒結體。 Then, it cooled at the cooling rate of 100 degreeC / h, and obtained the oxide sintered compact.
接著，將所得之氧化物燒結體進行切削加工，得到表面粗糙度Ra為1.0μm、寬度210mm、長度710mm、厚度6mm的濺鍍靶材。此外，切削加工係使用# 170的磨石。 Next, the obtained oxide sintered body was subjected to cutting processing to obtain a sputtering target having a surface roughness Ra of 1.0 μm, a width of 210 mm, a length of 710 mm, and a thickness of 6 mm. In addition, the cutting process uses a # 170 millstone.
將上述氧化物燒結體之相對密度及比電阻以上述方法測定。將結果顯示於表1。 The relative density and specific resistance of the oxide sintered body were measured by the methods described above. The results are shown in Table 1.
而且，在各實施例及比較例中，證實在調製各原料粉末時所測量之各元素的含有率係與所得氧化物燒結體中之各元素的含有率相等。氧化物燒結體中之各元素的含有率係例如可藉由ICP-AES(Inductively Coupled Plasma Atomic Emission Spectroscopy：感應耦合電漿原子發射光譜法)測定。 Moreover, in each Example and the comparative example, it was confirmed that the content rate of each element measured when preparing each raw material powder is equal to the content rate of each element in the obtained oxide sintered body. The content rate of each element in the oxide sintered body can be measured, for example, by ICP-AES (Inductively Coupled Plasma Atomic Emission Spectroscopy).
將上述濺鍍靶材以In焊料與銅製底板進行接合而製造濺射靶。 The sputtering target was bonded to a copper substrate with In solder to produce a sputtering target.
使用上述濺鍍靶，在以下條件下進行濺鍍，而於玻璃基板上使膜厚100nm之薄膜成膜。 Using the sputtering target, sputtering was performed under the following conditions to form a thin film having a thickness of 100 nm on a glass substrate.
裝置：真空機器工業股份有限公司製造之EX-3013M(DC磁控濺鍍裝置) Device: EX-3013M (DC magnetron sputtering device) manufactured by Vacuum Machinery Industry Co., Ltd.
極限真空度：未達1.0×10-4Pa Ultimate vacuum degree: less than 1.0 × 10 -4 Pa
濺鍍氣體：Ar/O2混合氣體 Sputtering gas: Ar / O 2 mixed gas
濺鍍氣體壓力：0.4Pa Sputtering gas pressure: 0.4Pa
氧流量：0至2.0sccm Oxygen flow: 0 to 2.0 sccm
基板：玻璃基板(Corning公司製造之EAGLE XG(註冊商標)) Substrate: glass substrate (EAGLE XG (registered trademark) manufactured by Corning)
基板溫度：室溫 Substrate temperature: room temperature
濺鍍功率密度：3W/cm2 Sputtering power density: 3W / cm 2
另外，在各實施例及比較例中，證實濺鍍靶材所使用之氧化物燒結體中的各元素之含有率係與成膜得到的透明導電膜中之各元素的含有率相等。透明導電膜中之各元素的含有率係例如可藉由ICP-AES(Inductively Coupled Plasma Atomic Emission Spectroscopy：感應耦合電漿原子發射光譜法)測定。 Moreover, in each Example and the comparative example, it was confirmed that the content rate of each element in the oxide sintered body used for a sputtering target is equal to the content rate of each element in the transparent conductive film obtained by film formation. The content rate of each element in the transparent conductive film can be measured, for example, by ICP-AES (Inductively Coupled Plasma Atomic Emission Spectroscopy).
所得之薄膜在大氣中、125℃熱處理1小時，製造透明導電膜。 The obtained thin film was heat-treated in the air at 125 ° C for 1 hour to produce a transparent conductive film.
將上述薄膜及透明導電膜在波長350nm及550nm之光透射率、透明導電膜的比電阻以上述方法測定。將光透射率及比電阻之結果顯示於表1。 The light transmittance of the thin film and the transparent conductive film at wavelengths of 350 nm and 550 nm, and the specific resistance of the transparent conductive film were measured by the methods described above. The results of light transmittance and specific resistance are shown in Table 1.
在比電阻方面，與屬於以往之ITO薄膜的比較例1所得之透明導電膜(In2O3：SnO2=90：10(質量比))的比電阻4.8×10-4Ω cm(以下稱為基準比電阻)相比並進行評定，將比電阻未達基準比電阻之1.0倍的透明導電膜評定為「A」、比電阻為基準比電阻之1.0倍以上且未達1.1倍的透明導電膜評定為「B」、比電阻為基準比電阻之1.1倍以上且未達1.2倍的透明導電膜評定為「C」、比電阻為基準比電阻之1.2倍以上的透明導電膜評定為「D」。 In terms of specific resistance, the specific resistance is 4.8 × 10 -4 Ω cm (hereinafter referred to as the transparent conductive film (In 2 O 3 : SnO 2 = 90: 10 (mass ratio)) obtained in Comparative Example 1 which is a conventional ITO thin film. (Referred to as the specific resistance) and evaluated, the transparent conductive film whose specific resistance is less than 1.0 times the reference specific resistance is rated as "A", and the specific resistance is 1.0 times or more and less than 1.1 times the reference specific resistance of the transparent conductive film. The transparent conductive film with a film rating of "B", a specific resistance of 1.1 times or more and less than 1.2 times the reference specific resistance is rated as "C", and a transparent conductive film with a specific resistance of 1.2 times or more the reference specific resistance is rated as "D"".
而且，在實施例15中，經濺鍍而得之薄膜及藉由將該薄膜在125℃進行熱處理而得之透明導電膜在波長300nm至800nm的範圍內的光透射率係顯示於第1圖，在實施例15及比較例1、3中，將經濺鍍而得之薄膜在125℃進行熱處理而得之透明導電膜在波長300nm至800nm的範圍內的光透射率係顯示於第2圖。第1圖中，「as-depo」意指未進行熱處理。 Further, in Example 15, the light transmittance of a thin film obtained by sputtering and a transparent conductive film obtained by heat-treating the thin film at 125 ° C in a wavelength range of 300 nm to 800 nm is shown in Fig. 1 In Example 15 and Comparative Examples 1 and 3, the light transmittance of a transparent conductive film obtained by heat-treating a thin film obtained by sputtering at 125 ° C. in a wavelength range of 300 nm to 800 nm is shown in FIG. 2. . In Fig. 1, "as-depo" means that no heat treatment has been performed.
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