200905003 * 九、發明說明： 【發明所屬之技術領域】 I發明係關於一種濺鍍靶(t a r g e t)，尤有關於 2時之麵吻则之華)_筆),（咐合金賤鑛 【先前技術】 近年來，作為液晶面板等之配線材料，鋁 系合金膜正受到目屬目。此A1系合金膜 冉A1) 雷P日，卜士梦Μ· , , ~ 彳有耐熱性與低 /手人而其中在紹中含有錄（以下稱叫之 者（參照專利文獻…）。有“之耐熱性、低電阻性 [專利文獻1]日本特開2003-089864號公報 [專利文獻2]曰本特開2〇〇扣2146〇6號公報 [專利文獻3]國際公開第2006/117954號公報 【發明内容】 [發明欲解決之問題] 作為該配線材料所使用之A1系 鍍而形成。藉由此濺轳^ 犋通吊係猎由濺 弧(_咱或飛濺(splash)之現象， 二::： :、u曰出在濺鍍時多會產生發 在使用由鑄造法所製造之Al系 月开/尤/、疋 會產生發弧現象。 ”口 '、、又巴時，已認為大多 ，由此鑄造法所製造<Al系合 有較大結晶粒徑之组婢处姐 无戣粑之性貝為.具 K構；及由於添加於#巴材之添加元 320083 5 200905003 :所產生的生成化合物被氧化而容易形成氧化物等之性 貝，故可推想發弧係由此等要因而產生者。 此叫朴剛）糊）系合金濺齡，係可藉由習知 之麵^造法來製造。铁而，斜於打旌s d '、、、而對於何種革巴材組織結構可充分抑 Δ 產生，而且，要以何種製造條件才可實現該種 1U系合金減鑛革巴，並未有提出具體方案之先前技二 本發明係有鑑於以上之情事而研創者，：種 經抑制產生發弧之A1抓Β系合金藏餘。R種 [解決問題之方案] 為了解決上述問題，本發明係一種A1抓Β系合 鑛革巴，係為含有Ni及Β，且析出有Al3Ni化合物者，盆特 徵為：相對於前述華化合物之全 ：粒 係為20"m以下。另外，本發明中之所謂内含 ^粒子之Al3Ni化合物相對於化合物之全析出量 ㈣㈣電子顯微鏡觀察革巴材表面或 央T *別疋義之Al3Nl化合物之全部個數，以百分比 來表不内含含B粒子之A_化合物之個數之比例者。 再者，本發明係有關於使用上述之ALB系合金濺 鑛革巴而藉由濺鏡法所形成之Al-Ni-B系合金膜。’、 【實施方式】 ’、 打：ΓΓ月本發明之最佳實施形態，惟本發明並不限定 於下述貫施形態。 本發明之Al-Ni-B系合金賤鐘把之特徵為：含有Ni 320083 6 200905003 及β ’且析出有A】 合物之全析出量，内含材中之獅化 '2%以上，而前述⑽化合物之平均;二合物之比例為 下。在系合金中，雖…仫係為2〇以m以 化合物之AI3Ni之性質隹 相中析出屬於金屬間 化合物之令，若内含含心^:,1；目中析出之湖i 發弧之產生就受到抑制。 子在有預定量，則 X 3有Νι及B作為添加元素之A 而言，在靶材之A丨相中，會 ^系δ金之情形 (例如Α1Β2粒子）。若藉由鑄造法製造m = 粒子 靶，則在預定條件下，就會以Μ 卜系合金濺鍍 為種核而產生Al3Ni化合物之 戶斤產生之含B粒子200905003 * IX, invention description: [Technical field of invention] I invention relates to a sputtering target, especially about the face kiss at 2 o'clock) _ pen), (咐 alloy antimony ore [previous technology] In recent years, as a wiring material such as a liquid crystal panel, an aluminum-based alloy film is attracting attention. This A1 alloy film 冉A1) Lei P, 士士梦Μ·, , 彳 has heat resistance and low/hands. In addition, it is described in the above-mentioned (hereinafter referred to as "the patent document"). There is a heat resistance and a low-resistance [Patent Document 1] Japanese Laid-Open Patent Publication No. 2003-089864 (Patent Document 2) [Patent Document 3] International Publication No. 2006/117954 [Disclosure] [The problem to be solved by the invention] It is formed by plating A1 which is used for the wiring material.轳^ 犋 吊 由 由 由 由 由 由 由 由 由 由 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅 溅/ You /, 疋 will produce arcing phenomenon. "口", and Ba Shi, have been considered mostly, thus cast The manufactured <Al series has a larger crystal grain size group, and the sister-in-law has a K-shaped structure; and since it is added to #巴材的元元320083 5 200905003: the resulting compound is produced Oxidation is easy to form a salt such as an oxide. Therefore, it is thought that the arc-forming system is caused by such an occurrence. This is called "Pang Gang" paste). The alloy splash age can be produced by a conventional method. Iron, oblique to sd ',, and for what kind of leather and buck material structure can fully inhibit Δ, and, under what manufacturing conditions can achieve this kind of 1U series alloy mining bar, not There are proposals for the prior art. The present invention has been developed in view of the above circumstances: the species is inhibited from producing arcing A1 scratching alloy deposits. R. [Solution to solve the problem] In order to solve the above problems, the present invention is an A1 grabbing gangue, which contains Ni and yttrium, and precipitates Al3Ni compound. The pot is characterized by: relative to the aforementioned Chinese compound. All: The granules are below 20"m. In addition, in the present invention, the total amount of the Al3Ni compound contained in the particles is compared with the total amount of the compound (4). (IV) Electron microscopic observation of the total number of Al3N1 compounds on the surface of the leather material or the central T*, which is expressed as a percentage. The ratio of the number of A-compounds containing B particles. Further, the present invention relates to an Al-Ni-B based alloy film formed by a sputtering method using the above-described ALB alloy splashing bar. The present invention is not limited to the following embodiments. The Al-Ni-B alloy beryllium of the present invention is characterized in that it contains Ni 320083 6 200905003 and β ' and precipitates a total amount of precipitated A compound, and the lionization in the inner material is '2% or more, and The average of the above (10) compounds; the ratio of the dimers is lower. In the alloy, although the lanthanum is 2 〇 in m, the compound of the AI3Ni of the compound is precipitated as an intermetallic compound, and if it contains a heart ^:, 1; Production is suppressed. When there is a predetermined amount, if X 3 has Νι and B as the additive element A, in the A 丨 phase of the target, δ gold is used (for example, Α1Β2 particles). If the m = particle target is produced by the casting method, under the predetermined conditions, the B-containing particles generated by the Al3Ni compound are generated by sputtering the alloy as a seed nucleus.
Al3Ni化合物形成。° =子2使内含含B粒子之 y. 3 β粒子之Al3Ni化合物呈有 在乾材之A1相中微細析出之傾向，推想 ς 之Al^i化合物若在八丨相中存在 3 3 3粒子 蟋合、# >佩 、里則革巴材整體之組 織曰進㈣細化，而使發弧之產生受到抑制。 广者，本發明之A1_Ni_B系合金賤錄，由於上之内 3率較而且組織微細，因此藏錢之際的發孤現象受到抑制 之結果，可獲得穩定之麟’進而可使均勻分散有β之 Al-Ni-B系合金膜成膜。此外，只要是B均句分散之从㈣ f合金膜，則於進行與ITO(IndiumTin〇xide，氧化鋼锡） 等透明電極之直接接合之際，即可降低其接合電阻。 _在本發明中，所§胃内含含B粒子之AlgNi化合物係指 含B粒子產生（被納入）在A13Ni化合物之中心部分之^ 320083 7 200905003 '態，包括：在八邮化合物之周邊部分產生含B粒子之狀 態、或在含B粒子與人咖化合物接觸之形態下所產生之 .狀態。換言之，不論其形態為何，均係顯示含辣子 、種形式與Al3NHb合物（粒子）接觸之狀態者。 ” 再者本么月之A1長-B系合金賤鑛乾中，相 =孽化合物之全析出量，内含含B粒子之： .9Π 乂上而削述A13Ni化合物之平均粒徑 (^^以下。若内含含B粒子之A1洲化合物之比例未 達2/。’則發弧現象之抑制效果就會變 之擊化合物相對於乾材中之_ = ::Π上限值雖無限制，惟由鱗造法之 咖下為較佳。另外，本發明中 ^ζ成本粒=Al3Ni compound is formed. ° = Sub 2 makes the Al3Ni compound containing y. 3 β particles containing B particles have a tendency to be finely precipitated in the A1 phase of the dry material, and it is assumed that the Al^i compound in the 丨 phase exists in the 丨 phase. The particle 蟋 , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , In the case of the A1_Ni_B alloy of the present invention, since the upper rate is 3 and the microstructure is fine, the lone phenomenon at the time of hiding money is suppressed, and a stable lining can be obtained, thereby uniformly dispersing β. The Al-Ni-B alloy film is formed into a film. Further, as long as it is a (four) f alloy film in which B average sentences are dispersed, the bonding resistance can be lowered when direct bonding to a transparent electrode such as ITO (Indium Tin Oxide) is performed. In the present invention, the AlgNi compound containing B particles in the stomach means that the B-containing particles are produced (incorporated) in the central portion of the A13Ni compound, and include: in the peripheral portion of the compound of the eight-mail compound. The state in which the B-containing particles are produced or in the form in which the B-containing particles are in contact with the human-coffee compound. In other words, regardless of the form, it is shown to be in a state in which a hot pepper is contained and the species is in contact with an Al3NHb compound (particle). In addition, this month's A1 long-B series alloy antimony ore, the total precipitation of phase = bismuth compound, containing B particles: .9 Π 乂 而 削 削 削 削 削 削 削 削 削 削 削 削 削If the ratio of the A1 compound containing B particles is less than 2/. 'The inhibition effect of the arcing phenomenon will change the _ = ::Π upper limit of the compound relative to the dry material, although there is no limit. However, it is preferable to use the scale method of the coffee. In addition, in the present invention, the cost of the grain =
Al3Ni化合物相對於八咖化 月円η Β粒子之 對於藉由掃描型電子㈣王析出量之比例，係相 ί 別定一化= : = ^ 含B粒子之Al3NUt合物之個數之=比來表不内含 此外，若AUNi化合物之平 有容易產生發弧之傾向。此A1N粒賴過2〇" m ’則會 内含含B粒子之彻化合物、^化合人物之平均粒徑係由 化合物之所有Al3Ni化合物來^内3含B粒子之Al3Ni 徑為W m以上之Al3NW_H^H、藉由粒 化合物之平均粒徑係以16“ m 者。再者， 有效地抑制發弧現象之故。 為較佳。此係因為可更 再者，對於AlsNi化合物之平 320083 8 200905003 ’均粒徑，並未特別限制下限值，惟由鑄造法之製造條件限 制來看，係以5 A m以上較為實用，若考慮製造成本，則 以13 // m以上為較佳。若考慮發弧現象之有效的抑制與製 -造條件之限制，則Al3Ni化合物之平均粒徑係以6// m至 16 μ m為更佐。丑& 4 , 另卜，右AlslSii化合物之粒徑未達5 // m， 則對於發弧不太有影響，因此在本發明中係以5/zm以上 粒徑之AlsNi化合物為對象。 f 另外，在本發明中，AhNi化合物、含b粒子（例如 I 子）之特別定義及其比例、該等平均粒徑係可藉由 !二鏡(SEM)及能量分散型x光分析裝置(EDX) :广之革巴材表面或革巴材剖面而特別定義。更具體 ”所二：率200倍之SEM觀察之視野(0.19mm2)下， 邮化合物之析出物且其直徑為一 算在Π)個視數者;在10個視野下進行此觀察’且計 【，化合物之含=子之 出物之長轴直：並算所有個數’來測量該析 切之本發明A1抓Β系合金 c以上之溫度 π谇7猎由以750 金。惟+ 來霄現預定組成之Al-Ni-B孚合 氓而配合鑄模材質、 川·《糸口 造溫度之各製造條件;；进且有^牛而適當調整包含鑄 卿Β系合金機…有上述組織結構之本發明 320083 9 200905003 < 上述之本發明Al-Ni-B系合金濺鍍靶係以Ni含量為 1.5at%以上、B含量為0.80at%以下為較佳。且以Ni含量 為1.5 at%至6 · Oat%為尤佳。再者，B含有量為係以0.10 at% 為較佳，且以0.20at%至0.80at%為尤佳。此係因為若為此 種組成之Al-Ni-B系合金濺鍍靶，則可成為對於液晶面板 等製程中之各項熱履歷具備優異耐熱特性之Al-Ni-B系合 金膜之故。另外，本發明之Al-Ni-B系合金濺鍍靶，從低 電阻特性之觀點來看，係以含有A1本身為75at%以上為 ί 宜。再者，本發明之Al-Ni-B系合金濺鍍靶不妨包含不可 避免之雜質，只要可達到本申請案發明之效果，亦可含有 其他之添加元素。 (實施例） 接下來說明本發明之實施例。在本實施例中，係製造 各種組成之Al-Ni系合金之濺鍍靶，且調查其濺鍍時發弧 之產生。 , 首先說明靶材之製造條件。在原料之熔解步驟中，係 k ' 使用閘流體（thyristor)式高頻加熱裝置（日本Thermonics(股） 製：公稱輸出50kW、振盪頻率3kHz)。由於第1表所示之 實施例1之合金組成係為Al-5.0at%Ni-0.4at%B，因此將經 考慮此组成比例之銘、鎳、之各原料投入至經預先加熱 之鋁坩堝，且設置於閘流體式高頻加熱裝置。原料之鋁係 使用從鑄錠（ingot)切出預定量者，而錄、硼之原料係使用 顆粒狀（pellet)者。再者，藉由將設置有鋁坩堝之空間減壓 而設在8Pa(以派藍尼真空儀（Pirani gauge)測量）之真空狀 10 320083 200905003 « 態，而開始原料之熔解加熱。坩堝内之原料雖藉由升溫至 1000°C(1273K)而全部熔解，惟再進一步進行升溫至1200 °C (1473K)。到達1200°C之後，在該溫度下保持30分鐘。 保持此溫度之後，以氬氣加壓至50000Pa，將鑄造溫 度調整至800°C (1073K)，並澆注於SUS製鑄膜（厚度 50 mm、縱長325mm、橫寬350mm之鑄錠製作用）。之後， 自然冷卻而獲得鑄錠。 所獲得之鑄錠在進行熱軋處理（壓下量2mm/軋次 € (pass)、溫度500°C )之後，作成厚度1 〇mm、縱長1625mm、 橫寬350mm之大小之軋製板。然後，將此軋製板表面進行 銑切加工（milling)，以製造尺寸為φ 203.2mmx8mm之革巴材 (實施例1)。另外，關於第1表所記載之實施例2至實施例 8、比較例1及比較例2、比較例6、比較例7之把材，基 本製造步驟係與上述相同，僅改變其合金組成或鑄造溫度 而製取。 / 此外，關於第1表所示之比較例3至比較例4之其他The ratio of the Al3Ni compound to the 咖 咖 円 円 Β 对于 藉 藉 藉 扫描 扫描 扫描 扫描 扫描 扫描 扫描 扫描 扫描 扫描 = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = In addition, the AUNi compound has a tendency to generate arcing. The A1N grain depends on 2〇" m ', which contains a compound containing B particles, and the average particle size of the compound is from all the Al3Ni compounds of the compound. The Al3Ni diameter of the B-containing particles is W m or more. Al3NW_H^H, the average particle size of the granular compound is 16" m. Furthermore, it is preferable to effectively suppress the arcing phenomenon. This is because it can be further, for the AlsNi compound flat 320083 8 200905003 'The average particle size is not particularly limited to the lower limit. However, it is more practical to use 5 A m or more depending on the manufacturing conditions of the casting method. If the manufacturing cost is considered, it is better to use 13 // m or more. Considering the effective inhibition of the arcing phenomenon and the limitation of the manufacturing conditions, the average particle size of the Al3Ni compound is more preferably from 6/m to 16 μm. Ugly & 4, another, right AlslSii compound When the particle diameter is less than 5 // m, it does not affect the arcing. Therefore, in the present invention, an AlsNi compound having a particle diameter of 5/zm or more is used. f Further, in the present invention, an AhNi compound, The specific definition of b particles (such as I) and their ratio, the average particle size can be borrowed Two-mirror (SEM) and energy-dispersive x-ray analyzer (EDX): specially defined for the surface of the leather or the material of the leather. More specific" two: 200 times the SEM observation field (0.19mm2 ), the precipitate of the physic compound and its diameter is calculated in Π) one visual number; this observation is carried out in 10 fields of view and the long axis of the compound containing the sub-substance is straight: All the numbers 'to measure the temperature of the A1 scratching alloy c above the cut-off of the present invention is 750 金. However, + is now the Al-Ni-B 氓 氓 预定 预定 氓 氓 配合 配合 配合 配合 配合 配合 配合 Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al Al The present invention of the above-mentioned structure is in the above-mentioned structure. The above-mentioned Al-Ni-B-based alloy sputtering target system preferably has a Ni content of 1.5 at% or more and a B content of 0.80 at% or less. It is particularly preferable that the Ni content is from 1.5 at% to 6 · Oat%. Further, the B content is preferably 0.10 at%, and particularly preferably 0.20 at% to 0.80 at%. In this case, the Al-Ni-B alloy sputtering target having such a composition can be used as an Al-Ni-B alloy film having excellent heat resistance characteristics for various heat history processes in a liquid crystal panel or the like. Further, the Al-Ni-B based alloy sputtering target of the present invention is preferably contained in an amount of 75 at% or more from the viewpoint of low resistance characteristics. Further, the Al-Ni-B alloy sputtering target of the present invention may contain unavoidable impurities, and may contain other additive elements as long as the effects of the invention of the present application can be attained. (Embodiment) Next, an embodiment of the present invention will be described. In the present embodiment, a sputtering target of an Al-Ni alloy of various compositions was produced, and the occurrence of arcing during sputtering was investigated. First, the manufacturing conditions of the target will be explained. In the melting step of the raw material, the k ' uses a thyristor type high-frequency heating device (made by Japan Thermonics: nominal output 50 kW, oscillation frequency 3 kHz). Since the alloy composition of the embodiment 1 shown in the first table is Al-5.0 at% Ni-0.4 at% B, the raw materials of the composition ratio, nickel, and the raw materials are considered to be put into the preheated aluminum crucible. And installed in a thyristor type high frequency heating device. The aluminum of the raw material is cut from a predetermined amount by ingot, and the raw material of the recorded or boron is pelletized. Further, the melting of the raw material was started by setting the vacuum of the aluminum crucible to 8 Pa (measured by a Pirani gauge) in a vacuum of 10 320083 200905003 « state. The raw materials in the crucible were all melted by heating to 1000 ° C (1273 K), but further heated to 1200 ° C (1473 K). After reaching 1200 ° C, it was kept at this temperature for 30 minutes. After maintaining this temperature, the pressure was adjusted to 50,000 Pa with argon gas, the casting temperature was adjusted to 800 ° C (1073 K), and cast into a cast film made of SUS (ingots having a thickness of 50 mm, a length of 325 mm, and a width of 350 mm). . After that, it is naturally cooled to obtain an ingot. The obtained ingot was subjected to hot rolling treatment (2 mm/roll (pass), temperature: 500 ° C), and a rolled plate having a thickness of 1 mm, a length of 1,625 mm, and a width of 350 mm was prepared. Then, the surface of the rolled plate was subjected to milling to produce a leather material having a size of φ 203.2 mm x 8 mm (Example 1). In addition, the basic manufacturing steps of the materials of the second to eighth embodiments, the comparative example 1 and the comparative example 2, the comparative example 6, and the comparative example 7 described in the first table are the same as described above, and only the alloy composition or the alloy composition thereof is changed. Prepared by casting temperature. / In addition, regarding the other of Comparative Example 3 to Comparative Example 4 shown in Table 1
I 組成之靶材，亦藉由與上述製造條件基本上相同之步驟進 行製造。惟以比較例4之情形而言，係以經考慮組成比例 而準備之鋁（鑄錠）、預先熔製之Ni-C合金（顆粒）作為原 料，並以1600°C進行溶解，在以與上述實施例l(Al-5.0at% Ni-0.4at%B)同樣之鑄造溫度製作出靶材。此外，以比較例 5之情形而言，係以經考慮其組成比例之鋁（鑄錠）、鎳（顆 粒）、鈥（顆粒）為原料，並以1200°C進行熔解，在以與上述 實施例l(Al-5.0at%Ni-0.4at%B)同樣之鑄造溫度製作出靶 11 320083 200905003 5 材。 再者，所獲得之各靶材係以下列方式調查濺鍍時之發 弧產生頻率。I巴材係接合（bonding)在銅製之背板（backing plate)，且裝設於多腔室型濺鍍裝置（TOKKI(股）製： MSL-464)。再者，此發弧測量係將因為濺鍍中之電弧放電 時之電壓降而使能量變化達1 〇Mj以上者計數為產生一次 發弧（測量裝置：微電弧監控器MAM Genesis、（股） LANDMARK TECHNOLOGY製）。另外，以發弧之指標而 ( 言，係使用以因濺鍍而在靶材厚度方向挖凹之深度除發弧 產生次數所得之發弧產生頻率（次/ mm)。藏鐘條件係如 下。設輸出為4000W、減壓度為0.5Pa、Ar流量為lOOsccm / min、放電時間為10小時。測量結果顯示於第2表。 此外，針對藉由各革巴材而成膜之Al-Ni系合金膜，亦 就與屬於透明電極之ITO之接合電阻進行了測量。與ITO 之接合電阻測量方法係如以下方式進行。 , 使用各組成之靶材，將濺鍍條件設為投入電力3.0W/ cm2、氬氣流量lOOccrn、氬氣壓力0.5Pa，使用濺鍍裝置 (TOKKI公司製：多腔室型濺鍍裝置MSL464)，將厚度2000 A之Al-Ni系合金膜形成於玻璃基板上。 再者，在Al-Ni系合金膜表面被覆阻劑（resist) (OFPR800 :東京應化工業（股）製），且配置20// m寬度電 路形成用圖案薄膜進行曝光處理，以包含濃度2.38%、液 溫 23°C 之氫氧化四曱錢（Tetramethyl ammonium hydroxide) 之鹼性顯影液（以下簡稱TMAH顯影液）進行顯影處理。顯 12 320083 200905003 影處理後，藉由磷酸系混酸蝕刻液（關東化學（股）公司製： 混酸餘刻劑（etchant)、組成（容量比磷酸：草酸：醋酸： 水=16 : 1 : 2 :卜液溫32。〇進行電路形成，且藉由二曱 基亞砜（以下稱DMS〇(dimethyl sulfoxide)剝離液進行阻劑 之去除’而形成20# m寬的電路。 接著，將形成有20# m寬之電路之基板，進行純水洗 淨、乾燥處理，而於其表面形成SiNx之絕緣層（厚度 Α ^ ο .ϊ-ί- (/71 Ζ.4Τ m 、 ，、 _.上 。 …〜~、”口/百、β /义呻 f k 人）。此絕緣層之成膜係使用濺鍍裝置，藉由投入電力 RF3.〇w/cm2、氬氣流4 9Geem、氮氣流量w⑽、塵力 〇.5pa、基板溫度300»c之濺鍍條件進行。 接下來，在絕緣層表面被覆正型阻劑（東京應化工業 ^公司製：TFR韻），且配置WO/zm見方之接 J孔開：用圖案薄膜而進行曝光處理，並藉由TMAH顯影 觸H影處理。然後’制CF4之乾絲刻氣體形成接 蜀孔：孔之形成條件训氣體之情形下， 、氧氣流量5咖、勤4施、輸出 :。在接觸孔形錢，藉由職〇剝離液進行阻劑^ 離液進=:'Γ剝離處理之各評估樣本係在將殘留之剝 進仃砘水洗淨之後，進行乾燥處理。 用IT::來，針對該阻劑之剝離處理已完成之各樣本，使 用1丁〇乾（组成In2〇3—1Gwt% 使 形成。透明_之=^及其周圍 板溫度7(TC、f A f ^ , 9 成係進仃濺鍍（基 氣流量〇.7CCnim .8W/cm、或氣流量80ccm、氧 堡力〇.37Pa)，而形成作為透明電極層之 320083 13 200905003 • 厚度1000 A之ITO膜。 再者，在此ΙΤΟ膜表面被覆阻劑（OFPR800 :東京應化 工業（股）公司製），且配置圖案薄膜進行曝光處理，並以濃 度2.38%、液溫23°C之ΤΜΑΗ顯影液進行顯影處理，並藉 由草酸系混合酸蝕刻液（關東化學（股）公司製ITO05N)進行 20μιη寬之電路之形成。於形成ITO膜電路之後，藉由剝 離液（DMSO 100wt%)將阻劑去除。 針對藉由以上之程序形成接觸孔，且經由接觸孔而直 f 接接合由Al-Ni系合金膜所構成之電路與透明電極層之評 估樣本，來測量其接觸電阻值。將其測量結果顯示於第2 表。此接觸電阻值之測量係根據如第1圖所示之四探針法 (four probe method)，將屬於評估樣本之元件在大氣中進行 25°C、30分鐘之退火處理後，進行各評估樣本之電阻值測 量。另外，此第1圖所示之四探針法係從熱處理後之評估樣 本之端子部分進行連續通電（3mA)，並進行測量其電阻者。 , 此外，將内含含B粒子之Al3Ni化合物相對於乾材中 之Al3Ni化合物之全析出量之比例、與Al3Ni化合物特別 定義如下。首先，針對所作成之各輕材，藉由掃描型電子 顯微鏡以倍率200倍進行觀察其中央部分之表面。第2圖 係顯示實施例1之代表性SEM觀察結果之概略圖。 第2圖所示之概略圖中，符號1之斜線所示之部分係 為靶材之A1相。此外，符號2所示之白色之析出物係為 Al3Ni粒子。再者，將符號3所示之析出物係為含B粒子（例 如AIB2粒子）。再者，將内部含有含B粒子、或與含B粒 14 320083 200905003 J 子接觸之狀態之Al3Ni化合物當作内含含B粒子之Al3Ni 並以符號2’表示。 關於内含含B粒子之Al3Ni化合物相對於革巴材中之 Al3Ni化合物之全析出量之比例，係將第2圖所示之SEM 觀察視野（〇.19mm2)之10個視野中所確認到之Al3Ni之析 出物之個數進行計數，且將其中以符號2’所示之内含含B 粒子之Al3Ni化合物之個數進行計數，而從該等個數算 出。此外，有關平均粒徑，係以作為析出物之長軸之部分 f 之長度作為各析出物之粒徑，並將在視野中所確認到之 Al3Ni之析出物且粒徑為5 // m以上之所有粒徑進行測量 而算出其平均。此外，藉由SEM與EDX確認結果，含B 粒子為A1B2。再者，以可藉由倍率200倍之SEM觀察而 測量之粒徑1# m以上者為對象，將内含含B粒子之粒徑 5// m以上之Al3Ni之個數進行計數。 第1表 組成 鑄造溫度(°C) 比例(％) Al3Ni平均粒徑〇 m) 實施例1 Al-5.0at%Ni-0.4at%B 800 5.6 15.3 實施例2 Al-5.0at%Ni-0.4at%B 750 3.9 13.1 實施例3 Al-3.2at%Ni-0.2at%B 800 2.5 7.6 實施例4 Al-1.5at%Ni-0.1at%B 800 2.3 6.4 實施例5 Al-1.5at%Ni-0.8at%B 800 7.2 6.1 實施例6 Al-6.0at%Ni-0.1at%B 800 2.0 18.5 實施例7 Al-6.0at%Ni-0.8at%B 800 6.6 16.2 實施例8 Al-1.2at%Ni-0.4at%B 800 8.3 5.7 比較例1 Al-5.0at%Ni-0.4at%B 700 1.8 20.3 比較例2 Al-5.0at%Ni-0.4at%B 950 4.1 24.7 比較例3 Al-5.0at%Ni 800 0 24.0 比較例4 Al-3.0at%Ni-0.3at%C 800 - 10.8 比較例5 Al-2.0at°/〇Ni-0.6at%Nd 800 - 7.7 比較例6 Al-5.0at°/〇Ni-0.05at°/〇B 800 0.9 20.7 比較例7 Al-7.0at%Ni-0.4at%B 800 1.1 25.2 15 320083 200905003 第2表 發弧頻率 (次 / mm) ITO接合電阻 (Ω 10 u m) 實施例1 2 1 貫施例2 貫施例3 -¾1 f：L· J%y\ A 5 *------- 2 3 4 實施例5 實施例6 3 31 8 ---^— 38 1 貫施例7 實施例 - 12 ZZHi-~ 50~' 比較例1 比較例2 比較例3 -逆 — 22 _30 ~~~---— 12 52 28 比較例4 3450 56 比旱父例5 比較例6 比較例7 ~~2Ϊ5 * — 320 38 ^-- ----—~-__ 1 ^ _表及第2表巾係囊總各實施例及各比較例之資 料加以顯示。第1本Λ , 貝 、中之比例之攔位係顯示内含含Β粒子 之入13沁化合物相對於靶 入 之比例值。由此第…结 3則匕.物之全析出量 R ,0/ 弟表及第2表可得知，在·比例為2.0%至 化合物之平均粒…8 5…”… 貝⑪歹'之乾材中，發弧現象明顯受到抑制。至於比較例 及比較例2,若與實施例！或2比較，則發弧頻率並未降 低。其理由據推測係由於Al3Ni化合物之粒徑較大所引 =，且由於在比較例i中禱造溫度較低，故於靖造前即在 坩堝内析出初晶AUNi(析出溫度約71〇。〇,並成長粗大化 320083 16 200905003 >里 所引ί之緣故。此外，亦可視為在比較例2 t由於鐘、告 曰曰 度過向而需要時間凝固，而於轉造後在禱模内析出之: AhNi成長粗大化所彳丨起之故。 知，之直接接合之接合電阻值之結果可 1猎由-施例…及實施例6、7、比較例6、 :至金=之㈣所絲者係為低接合電阻值，尤其實施例 盘 7係屬極低之接合電阻值。經由此發弧現象及 ^ 之接接合之接合電阻值之調查結果可知，在 f-N卜Β系合金賤鑛革巴中，係以见含量為i ^⑼以上為較 二/上所述，可預測在以實施们i 8之韻乾成膜之 情形下，膜中之B亦已均句地分散。 (產業上之可利用性） 依據本發明’由於抑制發弧之產生，因此可進行穩定 之峡’且可進行均勻之Α1·Νί_Β系合金膜之成膜。“ 【圖式簡單說明】 第1圖係為藉由四探針法之電阻值測量元件之概略 第2圖係為實施例1之乾材表面之SEM(SCanning electnm microscope，掃描電子顯微鏡）觀察照片之概略圖。 【主要元件符號說明】 1 A1相 2 AIgNi粒子 2’ 内含含B粒子之Al3Ni 3 含B粒子 320083The target composed of I is also manufactured by substantially the same steps as those described above. However, in the case of Comparative Example 4, aluminum (ingot) prepared in consideration of the composition ratio, and pre-melted Ni-C alloy (particles) were used as raw materials, and dissolved at 1600 ° C. The above Example 1 (Al-5.0 at% Ni-0.4 at% B) was cast at the same casting temperature to produce a target. Further, in the case of Comparative Example 5, aluminum (ingot), nickel (particles), and cerium (particles) which are considered to have a composition ratio are used as raw materials, and are melted at 1200 ° C, and are carried out in the same manner as described above. Example l (Al-5.0 at% Ni-0.4 at% B) The same casting temperature was used to produce the target 11 320083 200905003 5 material. Further, each of the obtained targets was investigated for the frequency of occurrence of arcing at the time of sputtering in the following manner. I was bonded to a copper backing plate and mounted on a multi-chamber type sputtering apparatus (manufactured by TOKKI Co., Ltd.: MSL-464). Furthermore, this arc measurement system will count the energy change up to 1 〇Mj or more due to the voltage drop during the arc discharge in the sputtering to generate a single arc (measuring device: micro-arc monitor MAM Genesis, (share) LANDMARK TECHNOLOGY). In addition, the arc generation frequency (times/mm) obtained by dividing the number of occurrences of arcing by the depth of the target in the thickness direction of the target by sputtering is used. The Tibetan clock condition is as follows. The output was 4000 W, the pressure reduction was 0.5 Pa, the Ar flow rate was lOOsccm / min, and the discharge time was 10 hours. The measurement results are shown in Table 2. In addition, the Al-Ni system formed by each of the leather materials was used. The alloy film was also measured for the bonding resistance of the ITO belonging to the transparent electrode. The bonding resistance measurement method with ITO was carried out as follows. Using the target of each composition, the sputtering condition was set to input power 3.0 W/ The cm2, the argon gas flow rate of 100 ccrn, and the argon gas pressure of 0.5 Pa were formed on a glass substrate by using a sputtering apparatus (manufactured by TOKKI Co., Ltd.: multi-chamber type sputtering apparatus MSL464) to form an Al-Ni alloy film having a thickness of 2000 A. The surface of the Al-Ni-based alloy film is coated with a resist (OFPR800: manufactured by Tokyo Ohka Kogyo Co., Ltd.), and a pattern film for 20//m width circuit formation is placed and exposed to a concentration of 2.38%. , tetrahydrogen hydroxide at a liquid temperature of 23 ° C (Tetrameth Alkylamine hydroxide (hereinafter referred to as TMAH developer) is developed. Display 12 320083 200905003 After the dye treatment, the phosphoric acid mixed acid etching solution (made by Kanto Chemical Co., Ltd.: mixed acid residual agent (etchant) ), composition (capacity ratio phosphoric acid: oxalic acid: acetic acid: water = 16: 1: 2: liquid temperature 32. 电路 circuit formation, and by dimercapto sulfoxide (hereinafter referred to as DMS 〇 (dimethyl sulfoxide) stripper The circuit of the resistor is removed to form a 20# m wide circuit. Next, a substrate having a circuit of 20# m width is formed, washed and dried by pure water, and an insulating layer of SiNx is formed on the surface thereof (thickness Α ^ ο .ϊ-ί- (/71 Ζ.4Τ m , , , _.上....~~, “mouth/hundred, β/呻呻fk person). The film formation of this insulating layer is performed by using a sputtering device. It is carried out by sputtering conditions of input electric power RF3.〇w/cm2, argon gas flow 49GEem, nitrogen gas flow rate w(10), dust force 〇.5pa, substrate temperature 300»c. Next, a positive resist is coated on the surface of the insulating layer (Tokyo Yinghua Industry Co., Ltd.: TFR rhyme), and configure WO/zm to see the J hole open: use The film is exposed and exposed to the H shadow by TMAH development. Then, the dry-cut gas of CF4 is formed to form the boring hole: in the case of the formation of the gas of the hole, the oxygen flow rate is 5, and the application is performed. , Output: In the contact hole shape, the resist is removed by the job stripping solution. ^Liquid in the =: 'The evaluation sample of the stripping treatment is dried after the residual stripped water is washed. . Using IT::, for each sample of the stripping treatment of the resist, use 1 〇 dry (composition of In2 〇 3-1 Gwt% to form. Transparent _ = = and its surrounding plate temperature 7 (TC, f A f ^ , 9 into the 仃 sputtering (base gas flow 〇 .7CCnim .8W / cm, or gas flow 80ccm, oxygen buckwheat 〇.37Pa), and formed as a transparent electrode layer 320083 13 200905003 • thickness 1000 A Further, the surface of the ruthenium film was coated with a resist (OFPR800: manufactured by Tokyo Ohka Kogyo Co., Ltd.), and a patterned film was placed for exposure treatment at a concentration of 2.38% and a liquid temperature of 23 °C. The developer was subjected to development treatment, and a circuit of 20 μm wide was formed by an oxalic acid mixed acid etching solution (ITO05N manufactured by Kanto Chemical Co., Ltd.). After the ITO film circuit was formed, the stripping solution (DMSO 100 wt%) was used. Resistor removal. The contact resistance was measured by forming a contact hole by the above procedure and directly bonding the evaluation sample of the circuit composed of the Al-Ni-based alloy film and the transparent electrode layer through the contact hole. The measurement results are shown in Table 2. This contact electricity The measurement of the value is based on the four probe method as shown in Fig. 1, and the components belonging to the evaluation sample are annealed at 25 ° C for 30 minutes in the atmosphere, and the resistance values of the respective evaluation samples are performed. In addition, the four-probe method shown in Fig. 1 is continuously energized (3 mA) from the terminal portion of the evaluation sample after heat treatment, and the resistance is measured. Further, Al3Ni containing B particles is contained. The ratio of the total amount of the compound to the total amount of the Al3Ni compound in the dry material and the Al3Ni compound are specifically defined as follows. First, the surface of the central portion is observed by a scanning electron microscope at a magnification of 200 times for each of the made light materials. Fig. 2 is a schematic view showing a representative SEM observation result of Example 1. In the schematic diagram shown in Fig. 2, the portion indicated by the hatching of symbol 1 is the A1 phase of the target. The white precipitates are Al3Ni particles. Further, the precipitates indicated by the symbol 3 are B-containing particles (for example, AIB2 particles). Further, the interior contains B-containing particles or B-containing particles 14 320083 200905003 J The Al3Ni compound in contact state is referred to as Al3Ni containing B particles and is represented by the symbol 2'. Regarding the ratio of the total precipitation amount of the Al3Ni compound containing the B particles to the Al3Ni compound in the leather material, 2 The number of precipitates of Al3Ni confirmed in 10 fields of view of the SEM observation field (〇.19 mm2) shown in Fig. 2, and the Al3Ni compound containing B particles contained therein as indicated by symbol 2' The number is counted and calculated from the number. In addition, the average particle diameter is the length of the part f which is the long axis of the precipitate as the particle diameter of each precipitate, and the precipitate of Al3Ni confirmed in the visual field has a particle diameter of 5 // m or more. All the particle diameters were measured to calculate the average. Further, by confirming the results by SEM and EDX, the B-containing particles were A1B2. In addition, the number of Al3Ni containing a particle diameter of 5/m or more containing B particles was counted for the particle diameter of 1# m or more which was measured by SEM observation at a magnification of 200 times. Table 1 Composition Casting Temperature (°C) Ratio (%) Al3Ni Average Particle Diameter 〇m) Example 1 Al-5.0at%Ni-0.4at%B 800 5.6 15.3 Example 2 Al-5.0at%Ni-0.4at %B 750 3.9 13.1 Example 3 Al-3.2 at% Ni-0.2 at% B 800 2.5 7.6 Example 4 Al-1.5 at% Ni-0.1 at% B 800 2.3 6.4 Example 5 Al-1.5 at% Ni-0.8 At% B 800 7.2 6.1 Example 6 Al-6.0 at% Ni-0.1 at% B 800 2.0 18.5 Example 7 Al-6.0 at% Ni-0.8 at% B 800 6.6 16.2 Example 8 Al-1.2 at% Ni- 0.4at%B 800 8.3 5.7 Comparative Example 1 Al-5.0at%Ni-0.4at%B 700 1.8 20.3 Comparative Example 2 Al-5.0at%Ni-0.4at%B 950 4.1 24.7 Comparative Example 3 Al-5.0at%Ni 800 0 24.0 Comparative Example 4 Al-3.0 at% Ni-0.3 at% C 800 - 10.8 Comparative Example 5 Al-2.0 at ° / 〇 Ni - 0.6 at % Nd 800 - 7.7 Comparative Example 6 Al-5.0 at ° / 〇 Ni -0.05 at ° / 〇 B 800 0.9 20.7 Comparative Example 7 Al-7.0 at% Ni-0.4 at% B 800 1.1 25.2 15 320083 200905003 Table 2 arc frequency (times / mm) ITO junction resistance (Ω 10 um) Example 1 2 1 Example 2 Example 3 - 3⁄41 f: L· J%y\ A 5 *------- 2 3 4 Example 5 Example 6 3 31 8 ---^— 38 1 Example 7 Example - 12 ZZHi-~ 50~' Comparative Example 1 Comparative Example 2 Comparative Example 3 - Inverse - 22 _30 ~~~---- 12 52 28 Comparative Example 4 3450 56 than Dry Father Example 5 Comparative Example 6 Comparative Example 7 ~~2Ϊ5 * — 320 38 ^-- --- --~-__ 1 ^ _ Table and the second table towel system are shown in the respective examples and comparative examples. The first block, the ratio of the shell to the middle, shows the ratio of the 13 沁 compound containing the ruthenium-containing particles to the target. Therefore, the third knot is 匕. The total amount of precipitation R, 0 / the younger table and the second table can be found, the ratio is 2.0% to the average particle of the compound... 8 5..."... In the dry material, the arcing phenomenon was remarkably suppressed. As for the comparative example and the comparative example 2, the arcing frequency was not lowered when compared with the example or the example 2. The reason was presumably because the particle size of the Al3Ni compound was large. Because of the lower temperature of the prayer in Comparative Example i, the primary crystal AUNi was precipitated in the crucible before the formation of Jing (the precipitation temperature was about 71 〇. 〇, and the growth was coarsened by 320083 16 200905003 > In addition, it can be considered that in Comparative Example 2, it takes time to solidify due to the passage of the clock and the warning, and it is precipitated in the prayer mold after the conversion: AhNi grows and coarsens. It is understood that the results of the direct bonding joint resistance values can be obtained from the example - and the examples 6 and 7, the comparative example 6, and the gold (4) are low junction resistance values, especially the embodiment disk. 7 is a very low junction resistance value. It can be seen from the investigation results of the arcing phenomenon and the junction resistance value of the junction. In the fN Β 贱 alloy 贱 革 巴 , , , , , , , , , i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i (Industrial Applicability) According to the present invention, since the generation of the arc is suppressed, the stable gorge can be performed and the film formation of the uniform Α1·Νί_Β alloy film can be performed. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic diagram of a resistance value measuring element by a four-probe method. Fig. 2 is a schematic view of an SEM (SCanning electnm microscope) observation of the surface of a dry material of Example 1. Fig. [Explanation of main component symbols] 1 A1 phase 2 AIgNi particle 2' contains Al3Ni 3 containing B particle 320083