TW201638364A - ITO sputtering target material - Google Patents
ITO sputtering target material Download PDFInfo
- Publication number
- TW201638364A TW201638364A TW105102324A TW105102324A TW201638364A TW 201638364 A TW201638364 A TW 201638364A TW 105102324 A TW105102324 A TW 105102324A TW 105102324 A TW105102324 A TW 105102324A TW 201638364 A TW201638364 A TW 201638364A
- Authority
- TW
- Taiwan
- Prior art keywords
- sno
- ito
- target
- phase
- sputtering target
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
- Inorganic Chemistry (AREA)
Abstract
Description
本發明係關於ITO濺鍍靶材,更詳而言之,係關於結合時難以產生龜裂,可有效率地成膜之ITO濺鍍靶材。 The present invention relates to an ITO sputtering target, and more specifically, to an ITO sputtering target which is difficult to generate cracks upon bonding and which can form a film efficiently.
ITO(銦錫氧化物,Indium-Tin-Oxide)膜因係具有高光透過性及導電性,故被廣泛利用於平面顯示器之透明電極、觸控面板等。透明電極用ITO膜通常以SnO2換算含有10質量%左右之Sn,但使用於觸控面板用之ITO膜係隨著與膜之熱處理的關係,Sn之含量以SnO2換算計使用2.5至8.0質量%左右者。 ITO (Indium-Tin-Oxide) film is widely used in transparent electrodes and touch panels of flat panel displays because of its high light transmittance and conductivity. The ITO film for a transparent electrode usually contains about 10% by mass of Sn in terms of SnO 2 , but the ITO film used for the touch panel has a relationship with the heat treatment of the film, and the content of Sn is 2.5 to 8.0 in terms of SnO 2 . The mass is about %.
ITO膜一般係藉由ITO濺鍍靶材之濺鍍所形成。ITO濺鍍靶材一般係與Cu製之支撐板結合(bonding)而被使用。因此,形成觸控面板用之ITO膜時,一般係將可實現目的之膜阻抗的Sn含量之ITO濺鍍靶材結合於Cu製之支撐板而進行濺鍍。 The ITO film is generally formed by sputtering of an ITO sputtering target. The ITO sputtering target is generally used in conjunction with a support plate made of Cu. Therefore, when forming an ITO film for a touch panel, an ITO sputtering target which can achieve a Sn content of a target film impedance is generally bonded to a support plate made of Cu to perform sputtering.
但,已知Sn之含量以SnO2換算計少於10質量%之ITO濺鍍靶材係脆弱且易龜裂。尤其是在Sn之含量以SnO2換算計成為3.5質量%以下時,易龜裂之傾向變 得顯著,在製造靶上變成很大之障礙。已知此係在此等之ITO濺鍍靶材中,製造過程之燒製時原因為容易殘留殘留應力,更且靶材之強度低。因此,此等之ITO濺鍍靶材係結合於Cu製等之支撐板時易產生龜裂。 However, it is known that the content of Sn is less than 10% by mass in terms of SnO 2 , and the ITO sputtering target is fragile and easily cracked. In particular, when the content of Sn is 3.5% by mass or less in terms of SnO 2 , the tendency to crack easily becomes remarkable, and it becomes a big obstacle in manufacturing a target. It is known that in such ITO sputtering targets, the reason for the firing of the manufacturing process is that residual stress is easily left, and the strength of the target is low. Therefore, these ITO sputtering targets are susceptible to cracking when they are bonded to a support plate made of Cu or the like.
進而,濺鍍Sn之含量以SnO2換算計少於10質量%之ITO濺鍍靶材時,抑制小節粒(nodule)之發生亦為課題之一。此小節粒之發生係可藉提高靶材之密度來改善。但,提高靶材之密度時,殘留應力變大,產生易龜裂之問題。 Further, when the content of the sputtered Sn is less than 10% by mass in terms of SnO 2 , the occurrence of nodule is also one of the problems. The occurrence of this small particle can be improved by increasing the density of the target. However, when the density of the target is increased, the residual stress becomes large, and the problem of cracking easily occurs.
又,降低燒製溫度而使燒製密度低至97%時,可得到殘留應力小,難以龜裂,且結晶組織亦小之ITO靶材,但於靶材中針孔增加,其為原因,而產生濺鍍時之小節粒增加的問題。亦即,使ITO靶材難以龜裂及抑制小節粒係有補償之關係。 Further, when the firing temperature is lowered and the firing density is as low as 97%, an ITO target having a small residual stress and being difficult to be cracked and having a small crystal structure can be obtained, but pinholes are increased in the target, which is a cause. There is a problem of an increase in the number of small particles at the time of sputtering. That is, it is difficult to crack the ITO target and suppress the relationship between the small granules.
特開平10-147862號公報中係關於一種小節粒發生少之錫含量為3至12重量%之氧化銦/氧化錫燒結體,並敘述有關結晶之平均粒徑或錫原子之最大凝集徑,但對於靶材之龜裂絲毫無任何言及。 Japanese Laid-Open Patent Publication No. Hei 10-147862 relates to an indium oxide/tin oxide sintered body having a small tin content of 3 to 12% by weight, and describes the average particle diameter of the crystal or the maximum agglomerating diameter of the tin atom, but There is nothing to say about the cracked wire of the target.
又,於特開2010-255022號公報中係記載有關相對於氧化銦之氧化錫的含量以質量比計為1.5%以上3.5%以下之ITO燒結體中,燒結體之結晶相為單相,以及平均結晶粒徑與燒結體之彎曲強度(70MPa以上)之關係。但,由此燒結體所構成之ITO靶材,龜裂之抑制並不充分。 In the ITO sintered body in which the content of tin oxide in indium oxide is 1.5% or more and 3.5% or less by mass ratio, the crystal phase of the sintered body is a single phase, and The relationship between the average crystal grain size and the bending strength (70 MPa or more) of the sintered body. However, the ITO target composed of the sintered body is not sufficiently suppressed in cracking.
[專利文獻1]日本特開平10-147862號公報 [Patent Document 1] Japanese Patent Laid-Open No. Hei 10-147862
[專利文獻2]日本特開2010-255022號公報 [Patent Document 2] Japanese Patent Laid-Open Publication No. 2010-255022
本發明之目的在於提供一種ITO濺鍍靶材,其係在Sn之含量以SnO2換算計為2.8至3.5質量%之ITO濺鍍靶材中,結合時難以產生龜裂,且濺鍍時之小節粒的發生量少。 An object of the present invention is to provide an ITO sputtering target which is 2.8 to 3.5% by mass in terms of Sn in terms of SnO 2 in an ITO sputtering target, which is less likely to be cracked when combined, and is sputtered. The amount of small pellets is small.
本發明人係為達成前述目的,經專心研究之結果,發現一種ITO濺鍍靶材,係Sn之含量以SnO2換算計為2.8至3.5質量%,其中,靶材係具有於In2O3固溶有SnO2之相及In4Sn3O12相之二相,靶材之相對密度為98%以上,因靶材之應變鬆弛所產生之變化長度每1m為50μm以下時,可達成前述目的。進一步,發現為得到其等之物性,必須以60℃/hr以下進行燒製成形體後之冷卻。 The inventors of the present invention have found that an ITO sputtering target material has a content of Sn of 2.8 to 3.5% by mass in terms of SnO 2 in order to achieve the above object, wherein the target is in In 2 O 3 . When the phase of the SnO 2 phase and the two phases of the In 4 Sn 3 O 12 phase are solid-solved, the relative density of the target is 98% or more, and the change length due to the strain relaxation of the target is 50 μm or less per 1 m. purpose. Further, it has been found that in order to obtain physical properties thereof, it is necessary to cool the body after firing at 60 ° C / hr or less.
亦即,本發明之ITO濺鍍靶材,係Sn之含量以SnO2換算為2.8至3.5質量%,其中,具有於In2O3固溶有SnO2之相及In4Sn3O12相之二相,相對密度為98%以上,應變鬆弛所產生之變化長度每1m為50μm以下。 That is, the ITO sputtering target of the present invention has a content of Sn of 2.8 to 3.5% by mass in terms of SnO 2 , and has a phase in which SnO 2 is dissolved in In 2 O 3 and an In 4 Sn 3 O 12 phase. In the two phases, the relative density is 98% or more, and the variation length due to strain relaxation is 50 μm or less per 1 m.
前述ITO濺鍍靶材係以應變鬆弛所產生之變化長度每1m為40μm以下為較佳。 It is preferable that the ITO sputtering target has a variation length due to strain relaxation of 40 μm or less per 1 m.
前述ITO濺鍍靶材係抗彎強度為13.0kgf/mm2以上較佳,14.0kgf/mm2以上為更佳。 The ITO sputtering target has a flexural strength of preferably 13.0 kgf/mm 2 or more, more preferably 14.0 kgf/mm 2 or more.
另一發明係一種前述ITO濺鍍靶材之製造方法,包含下列步驟:從含有平均粒徑為0.5μm以上之SnO2原料粉末的ITO製造用原料所製作之成形體以燒製爐在1500至1600℃之燒製溫度下燒製,在燒製爐內之溫度從前述燒製溫度達到700至1100℃之溫度範圍,使燒製爐內之溫度以60℃/hr以下之降溫速度降低,藉此冷卻所得之燒製體。 Another invention is a method for producing the ITO sputtering target, comprising the steps of: forming a shaped body from a raw material for ITO production containing a SnO 2 raw material powder having an average particle diameter of 0.5 μm or more, in a firing furnace at 1500 to Firing at a firing temperature of 1600 ° C, the temperature in the firing furnace is from the above-mentioned firing temperature to a temperature range of 700 to 1100 ° C, so that the temperature in the firing furnace is lowered at a cooling rate of 60 ° C / hr or less. This cooled the resulting fired body.
本發明之ITO濺鍍靶材係具有Sn之含量以SnO2換算計為2.8至3.5質量%之極易產生龜裂之組成,同時結合時難以龜裂,且濺鍍中小節粒之產生少,故可有效率地使ITO薄膜成膜。本發明之ITO濺鍍靶材的製造方法係可極有效率地製造前述靶材。 The ITO sputtering target of the present invention has a Sn content of 2.8 to 3.5% by mass in terms of SnO 2 , which is extremely susceptible to cracking, and is difficult to be cracked when combined, and the generation of small particles in sputtering is small. Therefore, the ITO film can be efficiently formed into a film. The method for producing an ITO sputtering target of the present invention can produce the aforementioned target extremely efficiently.
1‧‧‧應變量規 1‧‧‧ variable gauge
2‧‧‧配線 2‧‧‧Wiring
3‧‧‧靶材斷片 3‧‧‧ Target fragment
第1圖係以應變鬆弛所產生之變化長度的測定方法之說明圖。 Fig. 1 is an explanatory view showing a method of measuring the length of change caused by strain relaxation.
本發明之ITO濺鍍靶材(以下,亦稱為ITO靶材)係Sn之含量以SnO2換算計為2.8至3.5質量%之ITO靶材,且具有於In2O3中固溶有SnO2之相及In4Sn3O12相之二相,相對密度為98%以上,以應變鬆弛所產生之變化長 度每1m為50μm以下。本發明之ITO濺鍍靶材係結合時難以龜裂,且於濺鍍中小節粒之產生很少。 The ITO sputtering target (hereinafter also referred to as ITO target) of the present invention is an ITO target having a content of Sn of 2.8 to 3.5% by mass in terms of SnO 2 and having SnO dissolved in In 2 O 3 . The phase of 2 and the two phases of the In 4 Sn 3 O 12 phase have a relative density of 98% or more, and the length of change due to strain relaxation is 50 μm or less per 1 m. The ITO sputtering target of the present invention is difficult to crack when combined, and the generation of small particles in sputtering is small.
如前述,Sn之含量以SnO2換算計為2.8至3.5質量%之以往的ITO靶材係易產生殘留應力且強度低,故脆弱且易龜裂。製造ITO靶材時,若降低燒製溫度而使靶材之相對密度設為97%或其以下,則殘留應力變小,不易龜裂,但濺鍍時之小節粒會增加。若使ITO靶材之相對密度設為98%以上,則濺鍍時之小節粒變少,但殘留應力變大或容易龜裂。亦即,在Sn之含量以SnO2換算計為2.8至3.5質量%之以往的ITO靶材中係無法使龜裂困難性及抑制小節粒併存。 As described above, the conventional ITO target having a content of Sn of 2.8 to 3.5% by mass in terms of SnO 2 is likely to cause residual stress and low strength, so that it is fragile and easily cracked. When the ITO target is produced, when the firing temperature is lowered and the relative density of the target is 97% or less, the residual stress is small and cracking is unlikely, but the small particles at the time of sputtering increase. When the relative density of the ITO target is 98% or more, the small particles at the time of sputtering are reduced, but the residual stress is increased or cracking is likely to occur. In other words, in the conventional ITO target in which the content of Sn is 2.8 to 3.5% by mass in terms of SnO 2 , the cracking difficulty and the suppression of the small particles are not able to coexist.
本發明係在Sn之含量以SnO2換算計為2.8至3.5質量%之ITO靶材中,成功地使龜裂困難性及抑制小節粒併存。龜裂困難性及抑制小節粒之併存係初次藉由ITO靶材具有於In2O3中固溶有SnO2之相、及Sn之含量較於In2O3中固溶有SnO2之相更多之相的In4Sn3O12相之二相的方式來實現。 In the present invention, in the ITO target having a Sn content of 2.8 to 3.5% by mass in terms of SnO 2 , the cracking difficulty and the suppression of the small particles are successfully coexisted. Difficulty and cracking suppressed coexist based measure of the initial particles by ITO target having an In 2 O 3 in a solid solution phase of SnO 2, and the Sn content than the In 2 O 3 in a solid solution phase having minute SnO 2 of More phases of the In 4 Sn 3 O 12 phase are achieved in a two-phase manner.
ITO之製造通常係藉由製作由In2O3粉與SnO2粉之混合粉製作成形體,並燒製此成形體來進行。在此燒製中,SnO2會逐漸固溶於In2O3中。此時,例如Sn之含量以SnO2換算計為10%之ITO中,SnO2不完全固溶於In2O3,故於In2O3中固溶有SnO2之相的母相之外,可形成為富有Sn之相的In4Sn3O12相。其結果,SnO2之含量以SnO2換算計為10%之ITO係具有母相及In4Sn3O12相之二相。另 一方面,Sn之含量以SnO2換算計為2.8至3.5質量%之以往的ITO中,係Sn量少,且SnO2可完全固溶於In2O3中,故未形成In4Sn3O12相。其結果,SnO2之含量以SnO2換算計為2.8至3.5質量%之以往的ITO,係僅由於In2O3中固溶有SnO2之相之單一相所構成。 The production of ITO is usually carried out by producing a molded body from a mixed powder of In 2 O 3 powder and SnO 2 powder, and firing the molded body. In this firing, SnO 2 is gradually dissolved in In 2 O 3 . In this case, for example, the content of Sn in terms of SnO 2 to 10% of the ITO, SnO 2 is not completely dissolved in the In 2 O 3, In 2 O 3 it is in a solid solution phases other than the mother phase of SnO 2 of It can be formed into an In 4 Sn 3 O 12 phase rich in Sn phase. As a result, SnO 2 content of SnO 2 in terms of 10% based ITO having a two-phase matrix phase and In 4 Sn 3 O 12 phase of. On the other hand, in the conventional ITO in which the content of Sn is 2.8 to 3.5% by mass in terms of SnO 2 , the amount of Sn is small, and SnO 2 is completely dissolved in In 2 O 3 , so that In 4 Sn 3 is not formed. O 12 phase. As a result, SnO 2 content of SnO 2 in terms of 2.8 to 3.5 mass% of the conventional ITO, Department of In 2 O 3 since only the single phase solid solution of SnO 2 phase composed of.
本發明人係藉由採用後述之製造方法,SnO2之含量以SnO2換算計為2.8至3.5質量%,同時具有於In2O3中固溶有SnO2之相及In4Sn3O12相之二相,進而相對密度為98%以上,成功地製造屬於殘留應力之指標的應變鬆弛所產生之變化長度每1m為50μm以下之ITO靶材。其結果,在SnO2之含量為2.8至3.5質量%之ITO靶材中,可使龜裂困難性及抑制小節粒併存。 The present invention is based by a manufacturing method described later after use, the content of SnO 2 to SnO 2 of 2.8 to 3.5 in terms of% by mass, while in the In 2 O 3 having a solid solution of SnO 2 and Phase In 4 Sn 3 O 12 The two phases, and the relative density of 98% or more, succeeded in producing an ITO target having a change length of strain relaxation which is an index of residual stress of 50 μm or less per 1 m. As a result, in the ITO target having a content of SnO 2 of 2.8 to 3.5% by mass, cracking difficulty and suppression of small particles can be prevented.
使SnO2之含量為2.8至3.5質量%之ITO靶材設為具有於In2O3固溶有SnO2之相及In4Sn3O12相之二相的構造,藉此,可使龜裂困難度及抑制小節粒併存之理由係未必很明確,但可認為如此之構造中,In4Sn3O12相存在於在In2O3固溶有SnO2之相的粒界,因此並非增強於In2O3固溶有SnO2之相相互的結合之楔體作用所致。其結果,咸認為,前述具有二相之ITO靶材係可藉由使其高密度化,實現小節粒之抑制,另一方面,即使產生殘留應力,其若為一定值以下,亦非不可獲得難以龜裂之特性。例如Sn之含量以SnO2換算計為10%之ITO,一般係具有較SnO2之含量為2.8至3.5質量%之ITO更難以龜裂之性質,前者之ITO係如前述,由In2O3中固溶有SnO2之相及In4Sn3O12 相之二相所構成,In4Sn3O12相發揮如前述作用之故。 The ITO target having a content of SnO 2 of 2.8 to 3.5% by mass is a structure having a phase in which SnO 2 is dissolved in In 2 O 3 and a phase of In 4 Sn 3 O 12 phase, whereby the turtle can be made The reasons for the difficulty of cracking and the inhibition of the coexistence of small particles are not necessarily clear, but it is considered that in such a structure, the In 4 Sn 3 O 12 phase exists in the grain boundary of the phase in which SnO 2 is solid-dissolved in In 2 O 3 , and thus is not It is enhanced by the action of the wedge of In 2 O 3 solid solution in which the phases of SnO 2 are bonded to each other. As a result, it is considered that the ITO target having two phases can be suppressed by the density of the ITO target, and on the other hand, even if residual stress is generated, if it is a certain value or less, it is not available. It is difficult to crack the characteristics. For example, ITO having a content of Sn of 10% in terms of SnO 2 is generally more resistant to cracking than ITO having a content of SnO 2 of 2.8 to 3.5% by mass. The former ITO is as described above, and is made of In 2 O 3 . The two phases of the SnO 2 phase and the In 4 Sn 3 O 12 phase are dissolved in the solid solution, and the In 4 Sn 3 O 12 phase functions as described above.
本發明之ITO靶材係Sn之含量以SnO2換算計為2.8至3.5質量%。具體的Sn之含量係藉由由此靶材所得之膜所要求的物性而從前述範圍內來決定。 The content of the ITO target system Sn of the present invention is 2.8 to 3.5% by mass in terms of SnO 2 . The specific content of Sn is determined from the above range by the physical properties required for the film obtained from the target.
本發明之ITO靶材之相對密度係98%以上,更佳係98.5%以上,再更佳係99.0%以上。相對密度為98%以上時,於濺鍍時可抑制小節粒之發生,可良好的濺鍍。 The relative density of the ITO target of the present invention is 98% or more, more preferably 98.5% or more, still more preferably 99.0% or more. When the relative density is 98% or more, the occurrence of small particles can be suppressed at the time of sputtering, and good sputtering can be performed.
本發明之ITO靶材之因應變鬆弛所產生之變化長度係每1m為50μm以下,以每1m為40μm以下為較佳。因應變鬆弛所產生之變化長度係意指ITO靶材具有之殘有應力實質上全部被釋放之時,其釋放前之ITO靶材之長度與釋放後之ITO靶材之長度之差。因應變鬆弛所產生之變化長度係成為殘留應力之指標的物性值。因應變鬆弛所產生之變化長度係可使用應變量規來測定。ITO靶材以應變鬆弛所產生之變化長度之測定方法係在實施例中詳述。本發明之ITO靶材係如前述,具有於In2O3中固溶有SnO2之相及In4Sn3O12相之二相,故即使存在殘留應力,亦不易龜裂,但存在以應變鬆弛所產生之變化長度每1m為超過50μm之很大的殘留應力時,在其後之加工或結合步驟產生龜裂之機率變高。 The ITO target of the present invention has a variation length due to strain relaxation of 50 μm or less per 1 m, and preferably 40 μm or less per 1 m. The length of change due to strain relaxation means the difference between the length of the ITO target before release and the length of the released ITO target when the residual stress of the ITO target is substantially completely released. The length of change due to strain relaxation is a physical property value that is an indicator of residual stress. The length of change due to strain relaxation can be determined using a strain gauge. The method for determining the length of change of the ITO target by strain relaxation is detailed in the examples. As described above, the ITO target of the present invention has two phases of a phase in which SnO 2 is dissolved and a phase of In 4 Sn 3 O 12 in In 2 O 3 , so that even if residual stress is present, cracking is not easy, but there is When the length of change due to strain relaxation is a large residual stress exceeding 50 μm per 1 m, the probability of occurrence of cracks in the subsequent processing or bonding step becomes high.
本發明之ITO靶材係以抗彎強度為13.0kgf/mm2以上為較佳,以14.0kgf/mm2以上為更佳。本發明之TTO靶材滿足此條件時,可更有效地防止龜裂之發 生。 The ITO target of the present invention preferably has a flexural strength of 13.0 kgf/mm 2 or more, more preferably 14.0 kgf/mm 2 or more. When the TTO target of the present invention satisfies this condition, the occurrence of cracks can be more effectively prevented.
本發明之ITO靶材的形狀及大小無特別限制,即使為任何形狀及大小之ITO靶材,若滿足上述條件,可達成本發明之目的。形狀係可舉例如平板形及圓筒形等。 The shape and size of the ITO target of the present invention are not particularly limited, and even if the ITO target of any shape and size satisfies the above conditions, it can achieve the object of the invention. The shape may be, for example, a flat plate shape or a cylindrical shape.
以下,詳述有關本發明之ITO靶材之製造方法。 Hereinafter, a method of producing the ITO target of the present invention will be described in detail.
本發明之ITO靶材之製造方法係包含下列步驟:從含有平均粒徑為0.5μm以上之SnO2原料粉末的ITO製造用原料所製作之成形體在1500至1600℃之溫度範圍下燒製,再以60℃/hr以下之降溫速度冷卻所得到之燒製體。藉由此製造方法,可製造上述之ITO靶材。 The method for producing an ITO target of the present invention comprises the steps of: firing a molded body obtained from a raw material for ITO production containing a SnO 2 raw material powder having an average particle diameter of 0.5 μm or more at a temperature ranging from 1,500 to 1,600 ° C, The obtained fired body was further cooled at a temperature decreasing rate of 60 ° C / hr or less. By the above manufacturing method, the above ITO target can be produced.
ITO製造用之原料係包含SnO2粉末,通常含有In2O3粉末及SnO2粉末。將原料粉末之In2O3粉末與SnO2粉末以SnO2粉末之含量成為2.8至3.5質量%之目的組成的方式進行混合而製作混合粉末。各原料粉末之粒子通常會凝集,故較佳為於事前進行粉碎而混合,或一邊進行混合一邊粉碎。 The raw material for ITO production contains SnO 2 powder, and usually contains In 2 O 3 powder and SnO 2 powder. The In 2 O 3 powder of the raw material powder and the SnO 2 powder were mixed so that the content of the SnO 2 powder was 2.8 to 3.5% by mass to prepare a mixed powder. Since the particles of the respective raw material powders are usually aggregated, it is preferably pulverized and mixed beforehand or pulverized while being mixed.
In2O3粉末之平均粒徑通常為0.2至1.5μm,較佳為0.4至1.0μm。SnO2粉末之平均粒徑為0.5μm以上,較佳係0.5μm至5.0μm,更佳係0.6μm至2.0μm。本發明之ITO靶材之製造方法中,為得到於In2O3具有SnO2固溶之相及In4Sn3O12相之二相之ITO靶材,SnO2粉之平均粒徑必須為0.5μm以上。若SnO2粉之平均粒徑為0.5μm以上,於燒製時形成富Sn之相的In4Sn3O12相。認為此係 SnO2粉之平均粒徑為0.5μm以上時,前述成形體之燒製過程中,SnO2未完全固溶於In2O3,而未完全固溶之SnO2形成In4Sn3O12相之故。另一方面,若SnO2粉之平均粒徑小於0.5μm,未形成In4Sn3O12相。認為此係SnO2粉之平均粒徑未達0.5μm時,在前述成形體之燒製過程中,SnO2易固溶於In2O3,SnO2之至少大部分被固溶於In2O3之故。因此,必須意圖使用0.5μm以上之具有大的平均粒徑之SnO2粉末。又,上述平均粒徑係以雷射繞射散射式粒度分布測定法所得之累積體積50容量%中的體積累積粒徑D50。 The average particle diameter of the In 2 O 3 powder is usually from 0.2 to 1.5 μm, preferably from 0.4 to 1.0 μm. The SnO 2 powder has an average particle diameter of 0.5 μm or more, preferably 0.5 μm to 5.0 μm, more preferably 0.6 μm to 2.0 μm. In the method for producing an ITO target of the present invention, in order to obtain an ITO target having two phases of a SnO 2 solid solution phase and an In 4 Sn 3 O 12 phase in In 2 O 3 , the average particle diameter of the SnO 2 powder must be 0.5 μm or more. When the average particle diameter of the SnO 2 powder is 0.5 μm or more, an In 4 Sn 3 O 12 phase in which a Sn-rich phase is formed is formed at the time of firing. When this system that the average particle diameter of SnO 2 powder was 0.5μm or more, the formed body of the firing process, not completely dissolved in the SnO 2 In 2 O 3, without forming a complete solid solution of SnO 2 In 4 Sn 3 O 12 phase. On the other hand, if the average particle diameter of the SnO 2 powder is less than 0.5 μm, the In 4 Sn 3 O 12 phase is not formed. It is considered that when the average particle diameter of the SnO 2 powder is less than 0.5 μm, SnO 2 is easily dissolved in In 2 O 3 during the firing of the formed body, and at least a majority of the SnO 2 is dissolved in In 2 O. 3 reasons. Therefore, it is necessary to use a SnO 2 powder having a large average particle diameter of 0.5 μm or more. Further, the above average particle diameter is a volume cumulative particle diameter D50 in a cumulative volume of 50% by volume obtained by a laser diffraction scattering type particle size distribution measurement method.
於原料粉末之粉碎方法或混合方法無特別限制,例如,可將原料粉末置入於缽中,藉由球磨機進行粉碎或混合。 The pulverization method or the mixing method of the raw material powder is not particularly limited. For example, the raw material powder may be placed in a crucible and pulverized or mixed by a ball mill.
混合粉末係亦可直接成形而為成形體,再進行燒結,但依需要,可於混合粉末中加入黏結劑而成形為成形體。此黏結劑係可使用在公知之粉末冶金法中得到成形體時所使用之黏結劑、例如聚乙烯醇、丙烯酸乳化液黏結劑等。又,所得之成形體係亦可依需要在公知之粉末冶金法中所採用之方法來脫脂。成形方法亦可於公知之粉末冶金法中所採用之方法,例如適用澆鑄成形。成形體之密度通常為50至75%。 The mixed powder may be directly molded into a molded body and then sintered. However, if necessary, a binder may be added to the mixed powder to form a molded body. As the binder, a binder which is used in obtaining a molded body in a known powder metallurgy method, for example, a polyvinyl alcohol, an acrylic emulsion binder or the like can be used. Further, the obtained molding system can be degreased as needed in a known powder metallurgy method. The forming method can also be carried out by a method known in the powder metallurgy method, for example, casting molding. The density of the shaped body is usually from 50 to 75%.
將所得之成形體燒製而為燒製體,再進行冷卻而得到燒結體。使用於燒製之燒製爐只要在冷卻時可控制冷卻速度即可,並無特別限制,可為一般使用於粉末 冶金之燒製爐。燒製環境係適用氧氣環境。 The obtained molded body is fired to be a fired body, and further cooled to obtain a sintered body. The firing furnace used in the firing is not particularly limited as long as it can control the cooling rate during cooling, and can be generally used for powders. Metallurgical firing furnace. The firing environment is suitable for the oxygen environment.
昇溫速度係從高密度化及防止龜裂之觀點,通常為100至500℃/小時。燒製溫度係1500至1600℃,較佳係1520至1580℃。若燒製溫度為前述範圍內,可得到高密度之燒結體。在前述燒製溫度之保持時間通常為3至30小時,較佳係5至20小時。若保持時間為前述範圍內,易得到高密度之燒結體。 The rate of temperature rise is usually from 100 to 500 ° C / hour from the viewpoint of high density and prevention of cracking. The firing temperature is 1500 to 1600 ° C, preferably 1520 to 1580 ° C. When the firing temperature is within the above range, a sintered body having a high density can be obtained. The holding time at the aforementioned firing temperature is usually from 3 to 30 hours, preferably from 5 to 20 hours. If the holding time is within the above range, a sintered body of high density is easily obtained.
燒製結束之後,燒製爐內之溫度係從前述燒製溫度達到700至1100℃之溫度範圍為止,例如達到800℃為止,使燒製爐內之溫度以60℃/hr以下,較佳係以30℃/hr以下來降低,冷卻所得之燒製體。以此範圍之降溫速度進行冷卻,可減少燒結體之應變鬆弛所產生之變化長度,可使每1m設為50μm以下。其後之燒製爐內之溫度之下降速度係只要可為防止燒製體之龜裂等即可,無特別限制,例如可設為50至150℃/hr。 After the completion of the firing, the temperature in the firing furnace is from a temperature range of 700 to 1100 ° C, for example, 800 ° C, and the temperature in the firing furnace is 60 ° C / hr or less. The obtained fired body was cooled by lowering at 30 ° C / hr or less. By cooling at a temperature drop rate in this range, the length of change in strain relaxation of the sintered body can be reduced, and it can be made 50 μm or less per 1 m. The rate of decrease in the temperature in the firing furnace is not particularly limited as long as it can prevent cracking of the fired body, and can be, for example, 50 to 150 ° C / hr.
將如此作法所得之ITO燒結體依需要而切出所希望之形狀,藉由進行研削等得到本發明之ITO靶材。 The ITO sintered body obtained in this manner is cut into a desired shape as needed, and the ITO target of the present invention is obtained by grinding or the like.
本發明之ITO靶材通常係結合於支撐板而使用。支撐板通常係Cu、Al、Ti或不銹鋼製。結合材係可使用以往之ITO靶材之結合所使用的結合材、例如In金屬。結合方法亦與以往之ITO靶材之結合方法同樣。例如,將本發明之ITO靶材及支撐板加熱至結合材會融解之溫度例如約200℃,於靶材及支撐板之各別之結合面塗布結合材,貼合各別之結合面而壓接兩者之後,冷卻。或是,於 本發明之ITO靶材及支撐板之各別之結合面塗佈結合材,貼合各別之結合面,而將靶材及支撐板加熱至結合劑會融解之溫度例如約200℃之後,進行冷卻。 The ITO target of the present invention is usually used in combination with a support sheet. The support plate is usually made of Cu, Al, Ti or stainless steel. The bonding material can use a bonding material such as In metal used in combination with a conventional ITO target. The bonding method is also the same as the conventional ITO target. For example, the ITO target and the support plate of the present invention are heated until the temperature at which the bonding material melts, for example, about 200 ° C, and the bonding materials are applied to the respective bonding faces of the target and the supporting plate, and the respective bonding faces are pressed to be pressed. After the two, cool down. Or, in The bonding surface of the ITO target and the support plate of the present invention is coated with a bonding material to adhere to the respective bonding faces, and the target and the supporting plate are heated until the bonding agent melts at a temperature of, for example, about 200 ° C. cool down.
在下述實施例及比較例所得之ITO靶材之評估方法表示於以下。 The evaluation methods of the ITO targets obtained in the following examples and comparative examples are shown below.
1.相對密度 Relative density
ITO靶材之相對密度係依據阿基米德法進行測定。具體上係使靶材之空中重量除以體積(靶材之水中重量/量測溫度中之水比重),依據下述式(X)之相對於理論密度ρ(g/cm3)之百分率的值設為相對密度(單位:%)。 The relative density of the ITO target was measured according to the Archimedes method. Specifically, the air weight of the target is divided by the volume (the weight of the water in the target / the specific gravity of the water in the measured temperature), and the percentage relative to the theoretical density ρ (g/cm 3 ) according to the following formula (X) The value is set to relative density (unit: %).
ρ=((C1/100)/ρ1+(C2/100)/ρ2+‧‧‧+(Ci/100)/ρi)-1 (X) (式中C1至Ci係分別表示靶材之構成物質的含量(重量%),ρ 1至ρ i係表示對應於C1至Ci之各構成物質之密度(g/cm3)。) ρ=((C1/100)/ρ1+(C2/100)/ρ2+‧‧‧+(Ci/100)/ρi) -1 (X) (wherein C1 to Ci represent the content of the constituent materials of the target, respectively (wt%), ρ 1 ρ i lines to indicate corresponding to the density of the constituent substances of C1 to Ci (g / cm 3).)
2.原料粉末之平均粒徑 2. Average particle size of raw material powder
原料粉末之平均粒徑係使用日機裝股份公司製雷射繞射散射式粒度分布測定裝置(HRA 9320-X100)而測定。溶劑係使用水,以測定物質之折射率2.20測定。 The average particle diameter of the raw material powder was measured using a laser diffraction scattering type particle size distribution measuring apparatus (HRA 9320-X100) manufactured by Nikkiso Co., Ltd. The solvent was measured using water using a refractive index of 2.20.
3.抗彎強度測定 3. Determination of bending strength
抗彎強度係依據JIS-R-1601而測定。 The flexural strength was measured in accordance with JIS-R-1601.
4.靶材之組織(結晶相)之特定 4. Specificity of the target structure (crystalline phase)
藉電子顯微鏡觀察觀察於In2O3中SnO2固溶之相。又,有關In4Sn3O12相之特定係藉歐傑電子分光法調查Sn之分布來進行。 The phase in which SnO 2 was dissolved in In 2 O 3 was observed by an electron microscope. Further, the specificity of the In 4 Sn 3 O 12 phase is carried out by investigating the distribution of Sn by the Auger electron spectroscopy.
確認出於In2O3中固溶有SnO2之相及In4Sn3O12相時係評估為「二相」,僅確認出於In2O3中固溶有SnO2之相時係評估為「單一相」。 It was confirmed that the phase in which SnO 2 was dissolved in In 2 O 3 and the In 4 Sn 3 O 12 phase were evaluated as "two phases", and only when the phase in which SnO 2 was dissolved in In 2 O 3 was confirmed. The assessment is "single phase".
5.靶材之應變鬆弛所產生之變化長度(1量規法2線式) 5. The length of change caused by the strain relaxation of the target (1 gauge method 2-wire type)
於經清潔之靶材表面以專用之接着劑貼黏應變量規(N 11-FA-2-120-VSE 1、公稱電阻值120Ω、量規率2.0/日本Avionics公司製),以鑽石鋸齒機器切割靶材。切割係如第1圖所示,以安裝有配線2之應變量規1為中心,與應變量規1之4邊平行之方向上,以獲得20×20mm大小之靶材斷片3的方式進行。藉由靶材之切割釋放應變所產生之靶材的長度變化以連接有配線2之數據記錄器(遠端掃描器DC6100/日本Avionics公司製)測定。測定係在室溫(25℃)下進行。 Apply a variable gauge to the surface of the cleaned target with a special adhesive (N 11-FA-2-120-VSE 1, nominal resistance 120Ω, gauge rate 2.0/Avionics, Japan), with diamond sawtooth machine Cutting the target. As shown in Fig. 1, the cutting system is performed so as to obtain the target piece 3 of 20 × 20 mm in the direction parallel to the four sides of the strain gauge 1 centering on the strain gauge 1 on which the wiring 2 is attached. The change in the length of the target produced by the release of the strain by the cutting of the target was measured by a data recorder (remote scanner DC6100/manufactured by Avionics, Japan) to which the wiring 2 was connected. The measurement was carried out at room temperature (25 ° C).
6.結合時之靶材的龜裂 6. Cracking of the target when combined
為結合靶材具有充分面積之Cu製平板狀支撐板藉下列之方法結合靶材。將靶材及支撐板加熱至160℃,於靶材及基材之各別的結合面塗佈In焊料作為結合材,貼合各別之結合面而壓接兩者之後,進行冷卻。以目視觀察結合時靶材有無龜裂。確認出龜裂時係評估為「有」,未確認出 時評估為「無」。 A plate-shaped support plate made of Cu having a sufficient area in combination with the target is combined with the target by the following method. The target and the support plate were heated to 160 ° C, and In solder was applied as a bonding material to the respective bonding faces of the target and the substrate, and the respective bonding faces were bonded to each other to be pressed, and then cooled. The target was visually observed for cracking at the time of bonding. When the crack was confirmed, it was evaluated as "Yes" and was not confirmed. The time is evaluated as "None."
7.小節粒之發生量評估 7. Evaluation of the occurrence of small pellets
將結合時未產生龜裂之ITO靶以線切刀切割成小節粒評估用之大小,以下述條件濺鍍。照相攝影濺鍍後之靶材的表面,藉攝影從所得之圖像使用圖像解析軟體(粒子解析版3日鐵住金Technology股份公司製)而求出小節粒之面積。從所得之小節粒之面積,藉由靶材表面之小節粒面積之相對於靶材表面之面積的比率(%)評估小節粒之產生量。 The ITO target which was not cracked at the time of bonding was cut into a small particle size by a wire cutter, and sputtered under the following conditions. The surface of the target material after the photolithography was imaged, and the area of the small particle was obtained from the obtained image by image analysis software (particle analysis version, manufactured by Tiejinjin Technology Co., Ltd.). From the area of the obtained small pellets, the amount of small pellets was evaluated by the ratio (%) of the area of the small particles on the surface of the target with respect to the area of the surface of the target.
濺鍍係使用DC磁子濺鍍來進行。 Sputtering is performed using DC magneto-sputtering.
背壓:7.0×10-5[Pa] Back pressure: 7.0×10 -5 [Pa]
Ar分壓:4.0×10-1[Pa] Ar partial pressure: 4.0 × 10 -1 [Pa]
O2分壓:4.0×10-5[Pa] O 2 partial pressure: 4.0 × 10 -5 [Pa]
電力:300[W](1.6W/cm2) Electricity: 300 [W] (1.6 W / cm 2 )
靶尺寸:直徑203.2mm、厚度6mm Target size: diameter 203.2mm, thickness 6mm
將事先以球磨機進行粉碎所得之平均粒徑為0.6μm之In2O3粉末、及平均粒徑為0.8μm之SnO2粉末以SnO2粉末之含量成為3.0質量%之方式調配,作為黏結劑之丙烯酸乳化液黏結劑相對於陶瓷原料粉末加入0.3質量%、作為分散劑之聚羧酸銨相對於陶瓷原料粉末加入0.5質量%、及作為分散劑之水相對於陶瓷原料粉末加入20質量%,並進 行混合而調製膏漿。將此膏漿流入石膏模中,然後,進行排水而獲得縱350mm、橫1000mm、厚度10mm之平板狀之成形體。 In 2 O 3 powder having an average particle diameter of 0.6 μm obtained by pulverizing in a ball mill in advance, and SnO 2 powder having an average particle diameter of 0.8 μm were blended so as to have a content of SnO 2 powder of 3.0% by mass, as a binder. The acrylic emulsion binder is added to the ceramic raw material powder in an amount of 0.3% by mass, the polycarboxylate as a dispersing agent is added to the ceramic raw material powder in an amount of 0.5% by mass, and the water as a dispersing agent is added in an amount of 20% by mass based on the ceramic raw material powder, and Mixing is carried out to prepare a paste. This slurry was poured into a plaster mold, and then drained to obtain a flat molded body having a length of 350 mm, a width of 1000 mm, and a thickness of 10 mm.
其次,將此成形體乾燥後,燒製而製作燒製體。燒製係於氧氣環境中以升溫速度300℃/小時、燒製溫度1550℃進行10小時。其後,藉由燒製爐內之溫度達到800℃為止使燒製爐內之溫度以30℃/hr之速度下降以進行冷卻燒製體之後,藉由燒製爐內之溫度至成為室溫為止使燒製爐內之溫度以100℃/hr之速度下降以進行冷卻,製得燒結體。 Next, the molded body is dried and then fired to prepare a fired body. The firing was carried out in an oxygen atmosphere at a heating rate of 300 ° C / hour and a firing temperature of 1550 ° C for 10 hours. Thereafter, the temperature in the firing furnace is lowered at a rate of 30 ° C/hr by the temperature in the firing furnace to reach a temperature of 30 ° C to cool the fired body, and then the temperature in the furnace is heated to room temperature. The temperature in the firing furnace was lowered at a rate of 100 ° C / hr to cool, and a sintered body was obtained.
進一步,將所得之燒結體切削加工,獲得表面粗度Ra為0.7μm之縱280mm、橫750mm、厚度6mm之平板狀ITO靶材。加工係使用# 170之磨石。 Further, the obtained sintered body was subjected to a cutting process to obtain a flat ITO target having a surface roughness Ra of 0.7 μm and a longitudinal direction of 280 mm, a width of 750 mm, and a thickness of 6 mm. The processing system uses a #170 millstone.
所得之ITO靶材的Sn之含量係以SnO2換算計為3.0質量%,確認出與原料之Sn含量相同。 The content of Sn in the obtained ITO target was 3.0% by mass in terms of SnO 2 , and it was confirmed that the content of Sn was the same as that of the raw material.
對於此ITO靶材,進行上述評估。 For this ITO target, the above evaluation was performed.
除了使用平均粒徑為1.3μm之SnO2粉末取代平均粒徑為0.8μm之SnO2粉末以外,其餘係與實施例1同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 1 except that the SnO 2 powder having an average particle diameter of 1.3 μm was used instead of the SnO 2 powder having an average particle diameter of 0.8 μm.
除了使用平均粒徑為0.6μm之SnO2粉末取代平均粒徑為0.8μm之SnO2粉末以外,其餘係與實施例1同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 1 except that the SnO 2 powder having an average particle diameter of 0.6 μm was used instead of the SnO 2 powder having an average particle diameter of 0.8 μm.
除使燒製後至800℃之冷卻速度設為50℃/hr以外,其餘係與實施例1同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 1 except that the cooling rate to 800 ° C after firing was set to 50 ° C / hr.
除了以SnO2粉末之含量成為2.8質量%之方式調配以外,其餘係與實施例1同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 1 except that the content of the SnO 2 powder was 2.8% by mass.
除了以SnO2粉末之含量成為2.8質量%之方式調配以外,其餘係與實施例2同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 2 except that the content of the SnO 2 powder was 2.8% by mass.
除了以SnO2粉末之含量成為2.8質量%之方式調配以外,其餘係與實施例3同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 3 except that the content of the SnO 2 powder was 2.8% by mass.
除了以SnO2粉末之含量成為2.8質量%之方式調配以外,其餘係與實施例4同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 4 except that the content of the SnO 2 powder was 2.8% by mass.
除了以SnO2粉末之含量成為3.5質量%之方式調配以外,其餘係與實施例1同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 1 except that the content of the SnO 2 powder was adjusted to 3.5% by mass.
除了以SnO2粉末之含量成為3.5質量%之方式調配以外,其餘係與實施例2同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 2 except that the content of the SnO 2 powder was adjusted to 3.5% by mass.
除了以SnO2粉末之含量成為3.5質量%之方式調配以外,其餘係與實施例3同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 3 except that the content of the SnO 2 powder was adjusted to 3.5% by mass.
除了以SnO2粉末之含量成為3.5質量%之方式調配以外,其餘係與實施例4同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 4 except that the content of the SnO 2 powder was adjusted to 3.5% by mass.
除了使用平均粒徑為0.4μm之SnO2粉末取代平均粒徑為0.8μm之SnO2粉末以外,其餘係與實施例1同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 1 except that the SnO 2 powder having an average particle diameter of 0.4 μm was used instead of the SnO 2 powder having an average particle diameter of 0.8 μm.
除使燒製後至800℃之冷卻速度設為150℃/hr以外,其餘係與實施例1同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 1 except that the cooling rate to 800 ° C after firing was 150 ° C / hr.
除使燒製溫度設為1450℃以外,其餘係與實施例1同樣地進行製造、評估。 The production and evaluation were carried out in the same manner as in Example 1 except that the firing temperature was changed to 1,450 °C.
將評估結果表示於表1中。在表1之比較例1及2中係靶材於結合時完全龜裂,故未進行小節粒發生量之評估。 The evaluation results are shown in Table 1. In Comparative Examples 1 and 2 of Table 1, the target was completely cracked at the time of bonding, so that the amount of small particle generation was not evaluated.
1‧‧‧應變量規 1‧‧‧ variable gauge
2‧‧‧配線 2‧‧‧Wiring
3‧‧‧靶材斷片 3‧‧‧ Target fragment
Claims (5)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015-092830 | 2015-04-30 | ||
JP2015092830 | 2015-04-30 |
Publications (2)
Publication Number | Publication Date |
---|---|
TW201638364A true TW201638364A (en) | 2016-11-01 |
TWI660056B TWI660056B (en) | 2019-05-21 |
Family
ID=57199250
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
TW105102324A TWI660056B (en) | 2015-04-30 | 2016-01-26 | Ito sputtering target material and method for producing the same |
Country Status (5)
Country | Link |
---|---|
JP (1) | JPWO2016174877A1 (en) |
KR (1) | KR20170142169A (en) |
CN (1) | CN107250426A (en) |
TW (1) | TWI660056B (en) |
WO (1) | WO2016174877A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
TWI815291B (en) * | 2021-04-05 | 2023-09-11 | 日商Jx金屬股份有限公司 | Sputtering target and manufacturing method |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111440000B (en) * | 2020-04-24 | 2022-04-29 | 河北恒博新材料科技股份有限公司 | Preparation method of large-size rotary ceramic target |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3591610B2 (en) * | 1994-11-10 | 2004-11-24 | 日立金属株式会社 | ITO sintered body for forming transparent conductive film |
JP2000233969A (en) * | 1998-12-08 | 2000-08-29 | Tosoh Corp | Production of ito sputtering target and transparent electrically conductive film |
JP4642327B2 (en) * | 2003-06-03 | 2011-03-02 | Jx日鉱日石金属株式会社 | ITO sputtering target and manufacturing method thereof |
JP2007008752A (en) * | 2005-06-29 | 2007-01-18 | Mitsui Mining & Smelting Co Ltd | Indium oxide-tin oxide powder, sputtering target using it, and method of manufacturing indium oxide-tin oxide powder |
JP2009040621A (en) * | 2007-08-06 | 2009-02-26 | Mitsui Mining & Smelting Co Ltd | Ito sintered body and ito sputtering target |
JP2009040620A (en) * | 2007-08-06 | 2009-02-26 | Mitsui Mining & Smelting Co Ltd | Ito sintered body and ito sputtering target |
JP5218032B2 (en) * | 2008-12-25 | 2013-06-26 | 東ソー株式会社 | Method for producing sintered body for transparent conductive film |
JP5309975B2 (en) * | 2008-12-25 | 2013-10-09 | 東ソー株式会社 | Sintered body for transparent conductive film, sputtering target and method for producing the same |
JP5206983B2 (en) * | 2009-04-22 | 2013-06-12 | 住友金属鉱山株式会社 | ITO sputtering target and manufacturing method thereof |
CN101580379B (en) * | 2009-06-29 | 2012-05-16 | 北京航空航天大学 | Nb-doped nano indium tin oxide powder and method for preparing high density sputtering coating target thereof |
JP2012126937A (en) * | 2010-12-13 | 2012-07-05 | Sumitomo Metal Mining Co Ltd | Ito sputtering target and manufacturing method thereof |
CN102718499B (en) * | 2012-07-10 | 2014-02-26 | 国家钽铌特种金属材料工程技术研究中心 | Manufacturing method of ITO (Indium Tin Oxide) sputtering target comprising In4Sn3O12 phases |
JP5987105B2 (en) * | 2013-03-29 | 2016-09-06 | Jx金属株式会社 | ITO sputtering target and manufacturing method thereof |
JP5816394B1 (en) * | 2014-02-18 | 2015-11-18 | 三井金属鉱業株式会社 | ITO sputtering target material and manufacturing method thereof |
-
2016
- 2016-01-04 WO PCT/JP2016/050020 patent/WO2016174877A1/en active Application Filing
- 2016-01-04 JP JP2017515394A patent/JPWO2016174877A1/en active Pending
- 2016-01-04 CN CN201680011407.1A patent/CN107250426A/en active Pending
- 2016-01-04 KR KR1020177030294A patent/KR20170142169A/en unknown
- 2016-01-26 TW TW105102324A patent/TWI660056B/en active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
TWI815291B (en) * | 2021-04-05 | 2023-09-11 | 日商Jx金屬股份有限公司 | Sputtering target and manufacturing method |
Also Published As
Publication number | Publication date |
---|---|
KR20170142169A (en) | 2017-12-27 |
WO2016174877A1 (en) | 2016-11-03 |
TWI660056B (en) | 2019-05-21 |
CN107250426A (en) | 2017-10-13 |
JPWO2016174877A1 (en) | 2018-02-22 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP4846726B2 (en) | Sputtering target, transparent conductive film and transparent electrode | |
TWI594970B (en) | ITO sputtering target and manufacturing method thereof, and manufacturing method of ITO transparent conductive film and ITO transparent conductive film | |
TWI522332B (en) | Ito sputtering target material and method of manufacturing the same | |
JP6278229B2 (en) | Sputtering target for forming transparent oxide film and method for producing the same | |
JP2014105383A (en) | Cylindrical type sputtering target and manufacturing method of the same | |
KR20140041950A (en) | Amorphous composite oxide film,crystalline composite oxide film,process for producing amorphous composite oxide film,process for producing crystalline composite oxide film,and composite oxide sinter | |
JP2007176706A (en) | Oxide sintered compact, its production method, sputtering target and transparent electrically conductive film | |
TWI421357B (en) | Ito sputtering target and the manufacturing method thereof | |
TW201638364A (en) | ITO sputtering target material | |
JP2020164930A (en) | Ito sputtering target, method for manufacturing the same, ito transparent conductive film and method for manufacturing the same | |
JP7086080B2 (en) | Oxide sintered body and sputtering target | |
JP6267297B1 (en) | Sintered body, sputtering target and manufacturing method thereof | |
JP6453528B1 (en) | Sputtering target for transparent conductive film | |
JP7203088B2 (en) | Oxide sintered body, sputtering target and transparent conductive film | |
JP6722736B2 (en) | Sintered body and sputtering target | |
WO2015020029A1 (en) | Sputtering target and method for producing same | |
JP2007238365A (en) | Oxide sintered compact, its manufacturing method, sputtering target and transparent conductive film | |
JP5809542B2 (en) | Sputtering target material and manufacturing method thereof | |
TW202020179A (en) | Oxide sputtering target and method of manufacturing oxide sputtering target | |
JP2019137875A (en) | Sputtering target, and manufacturing method of sputtering target | |
JP2009227513A (en) | Method for manufacturing titanium oxide target having high density and low specific resistance |