TWI444491B - Pure aluminum or aluminum alloy sputtering target - Google Patents

Description

純鋁或鋁合金濺鍍靶Pure aluminum or aluminum alloy sputtering target

本發明係關於鋁基合金濺鍍靶，詳細地說，是有關於在使用濺鍍靶形成薄膜時，能夠消除在濺鍍的初期階段發生的問題(例如飛濺的個數的增加和所形成的薄膜的電阻的上升等)，可以縮短預濺鍍時間的鋁基合金濺鍍靶。The present invention relates to an aluminum-based alloy sputtering target, and more particularly to a problem in which an initial stage of sputtering can be eliminated when a thin film is formed using a sputtering target (for example, an increase in the number of splashes and formation) The increase in the resistance of the film, etc., can shorten the aluminum-based alloy sputtering target of the pre-sputtering time.

鋁由於電阻率低，容易加工等理由，在液晶顯示器(LCD：Liquid Crystal Display)、等離子體顯示器(PDP：Plasma Display Panel)、電致發光顯示器(ELD：Electro Luminescence Display)、場致發鍍顯示器(FED：Field Emission Display)、微機電系統(MEMS：Micro Electro Mechanical Systems)顯示器等的平板顯示器(FPD：Flat Panel Display)，觸控面板、電子紙等的領域被廣泛應用，被利用於佈線膜、電極膜、反鍍電極膜等的材料。Aluminum is a liquid crystal display (LCD: Liquid Crystal Display), a plasma display (PDP: Plasma Display Panel), an electroluminescence display (ELD: Electro Luminescence Display), a field emission display, etc. due to low resistivity and easy processing. (FED: Field Emission Display), flat panel display (FPD: Flat Panel Display) such as MEMS (Micro Electro Mechanical Systems) display, touch panel, electronic paper, etc., are widely used in wiring films. Materials such as electrode films and reverse plating electrode films.

例如，主動矩陣型的液晶顯示器具有TFT基板，該TFT基板具有：作為開關元件的薄膜電晶體(TFT：Thin Film Transistor)、由導電性氧化膜構成的像素電極及含有掃描線和信號線的佈線。在構成掃描線和信號線的佈線材料中，一般使用的是純Al或Al-Nd合金的鋁基合金膜。For example, an active matrix type liquid crystal display has a TFT substrate having a thin film transistor (TFT: Thin Film Transistor) as a switching element, a pixel electrode composed of a conductive oxide film, and a wiring including a scanning line and a signal line. . Among the wiring materials constituting the scanning lines and the signal lines, an aluminum-based alloy film of pure Al or Al-Nd alloy is generally used.

可是，在鋁基合金薄膜的形成中，一般會採用的是使用濺鍍靶的濺鍍法。所謂濺鍍法，就是在基板和與薄膜材料同樣的材料所構成的濺鍍靶(靶材)之間形成等離子體放電，使經由等離子體放電而離子化的氣體碰撞靶材，從而衝擊出靶材的原子，使之堆積在基板上而製造薄膜的方法。濺鍍法與真空蒸鍍法不同，其具有的優點是，能夠形成與靶材同組成的薄膜。特別是以濺鍍法形成的鋁合金膜，能夠使平衡狀態下不固溶的Nd等的合金元素固溶，作為薄膜發揮出優異的性能，因此在工業上是有效的薄膜製作方法，作為其原料的濺鍍靶材的開發正持續進行中。However, in the formation of an aluminum-based alloy film, a sputtering method using a sputtering target is generally employed. In the sputtering method, a plasma discharge is formed between a substrate and a sputtering target (target) made of the same material as the thin film material, and a gas ionized by plasma discharge collides with the target to impact the target. A method of producing a thin film by depositing atoms on a substrate. The sputtering method differs from the vacuum evaporation method in that it has the advantage of being able to form a film of the same composition as the target. In particular, an aluminum alloy film formed by a sputtering method is capable of solid-solving an alloying element such as Nd which is not dissolved in an equilibrium state, and exhibits excellent performance as a film. Therefore, it is an industrially effective film forming method. The development of sputtering targets for raw materials is continuing.

用於上述濺鍍法的鋁基合金濺鍍靶，例如通過噴射成形(spray forming)法和熔融鑄造法等所製造。在濺鍍的初期，一般會進行被稱為預濺鍍的操作。因為在濺鍍靶的使用初期，濺鍍靶表面的污垢會致使濺鍍不穩定，結果是所形成的薄膜的特性也不穩定，因此出於除去污垢等的目的而進行該預濺鍍。例如，在使用鋁基合金濺鍍靶形成薄膜時，在濺鍍的初期階段，飛濺(微細的熔融粒子)會大量發生，出現所形成的佈線薄膜的電阻上升等的問題，在現場要進行預濺鍍直至其穩定下來。但是，預濺鍍時間的增加帶來生產率的降低。The aluminum-based alloy sputtering target used in the above sputtering method is produced, for example, by a spray forming method, a melt casting method, or the like. At the beginning of sputtering, an operation called pre-sputtering is generally performed. In the initial stage of use of the sputtering target, the stain on the surface of the sputtering target causes the sputtering to be unstable, and as a result, the characteristics of the formed film are also unstable, so the pre-sputtering is performed for the purpose of removing dirt or the like. For example, when a film is formed using an aluminum-based alloy sputtering target, spatter (finely-molded particles) may be generated in a large amount in the initial stage of sputtering, and a problem such as an increase in resistance of the formed wiring film may occur, and a pre-preparation is required at the site. Sputter until it stabilizes. However, an increase in the pre-sputtering time leads to a decrease in productivity.

作為降低飛濺的方法，例如在日本專利第3410278號公報中，公開有一種以維氏硬度(Hv)計，將硬度控制在25以下的鋁基合金濺鍍靶。As a method of reducing the splash, for example, Japanese Patent No. 3410278 discloses an aluminum-based alloy sputtering target in which the hardness is controlled to 25 or less in terms of Vickers hardness (Hv).

另外，作為一種不是以鋁基合金濺鍍靶為對象，但卻是降低基於飛濺的現象的塊狀的異物的發生的方法，在日本專利2001-316808號公報中，公開有一種濺鍍面的最大高度Ry為10μm以下的Mo-W合金濺鍍靶。另外還公開，由於構成飛濺現象的原因的異常放電容易在相鄰的凸部間發生，因此將存在於濺鍍面的深度5μm以上的凹部的寬度作為粗糙度曲線的局部波峰的間隔，而較佳為控制在70μm以上。Further, as a method which does not target an aluminum-based alloy sputtering target, but is a method of reducing the occurrence of a block-shaped foreign matter based on a splash phenomenon, a sputtering surface is disclosed in Japanese Patent Laid-Open Publication No. 2001-316808. A Mo-W alloy sputtering target having a maximum height Ry of 10 μm or less. Further, it is also disclosed that the abnormal discharge which is caused by the splash phenomenon is likely to occur between adjacent convex portions, and therefore the width of the concave portion having a depth of 5 μm or more on the sputtering surface is used as the interval of the local peak of the roughness curve. Good control is above 70μm.

另外，雖然不是以鋁基合金濺鍍靶為對象，但在日本特開平10-158828號公報中公開有一種Ti濺鍍靶，其為了降低進行濺鍍中發生的微粒(微細的粉塵)，使被濺鍍的面成為具有規定曲率的凹面，並且對於該濺鍍面實施鏡面加工，將其算術平均粗糙度Ra控制在0.01μm以下。In addition, a titanium sputtering target is disclosed in Japanese Laid-Open Patent Publication No. Hei 10-158828, which is intended to reduce particles (fine dust) generated during sputtering. The surface to be sputtered has a concave surface having a predetermined curvature, and the sputter surface is mirror-finished to have an arithmetic mean roughness Ra of 0.01 μm or less.

本發明的目的在於，提供一種新穎的鋁基合金濺鍍靶，其能夠消除在濺鍍的初期階段發生的問題(飛濺的個數的增加、所形成的佈線薄膜的電阻的上升等)，可以縮短預濺鍍時間。An object of the present invention is to provide a novel aluminum-based alloy sputtering target capable of eliminating problems occurring in the initial stage of sputtering (increased number of spatters, increase in resistance of a formed wiring film, etc.) Shorten the pre-sputter time.

本發明包括以下的形態。The present invention includes the following aspects.

(1)一種鋁基合金濺鍍靶，其係以JIS B0601(2001)所規定的方法測量濺鍍面的表面粗糙度時，算術平均粗糙度Ra為1.50μm以下，以及最大高度Rz為10μm以下，並且，其特徵為將從粗糙度曲線的中心線至波峰或波谷的高度超過0.25×Rz的峰值高度分別設為為P或Q，於基準長度100mm內，依次計數P和Q時，P緊鄰其後出現的Q再到緊鄰該Q出現的P之間的間隔L的平均值為0.4mm以上。(1) An aluminum-based alloy sputtering target which has an arithmetic mean roughness Ra of 1.50 μm or less and a maximum height Rz of 10 μm or less when the surface roughness of the sputtering surface is measured by a method specified in JIS B0601 (2001) And it is characterized in that the peak height from the center line of the roughness curve to the peak or the trough exceeds 0.25×Rz is set to P or Q, respectively, and when P and Q are sequentially counted within the reference length of 100 mm, P is immediately adjacent. The average value of the interval L between the Q which appears thereafter and the P which appears immediately adjacent to the Q is 0.4 mm or more.

本發明的鋁基合金濺鍍靶，不僅被控制濺鍍面的表面粗糙度，而且還以使由L值代表的峰間隔的平均值(週期)延長的方式進行控制，所以能夠迅速地將濺鍍靶在使用初期階段發生的飛濺和由該濺鍍靶所形成的薄膜的電阻降低至規定水準。因此，如果使用本發明的濺鍍靶，則能夠縮短直至上述的飛濺或薄膜電阻穩定化所實施的預濺鍍時間。The aluminum-based alloy sputtering target of the present invention is controlled not only by controlling the surface roughness of the sputtering surface but also by extending the average value (period) of the peak interval represented by the L value, so that the sputtering can be quickly performed. The splash generated in the initial stage of use of the plating target and the electric resistance of the film formed by the sputtering target are lowered to a prescribed level. Therefore, if the sputtering target of the present invention is used, the pre-sputtering time which is performed up to the above-described spatter or sheet resistance stabilization can be shortened.

具體實施方式detailed description

本發明者們，為了提供一種能夠消除在濺鍍靶的使用初期階段發生的飛濺(初期飛濺)和由該濺鍍靶形成的薄膜的電阻上升這樣的問題，可以縮短預濺鍍時間的鋁基合金濺鍍靶而反復進行研究。其結果發現，如果所使用的鋁基合金濺鍍靶中，不僅適當控制濺鍍面的表面粗糙度(在本發明中為Ra和Rz)，而且以使由L值代表的峰間隔的平均值延長的方式進行控制時，則能夠達成預期的目的，從而完成了本發明。The inventors of the present invention have been able to eliminate the problem of splash (initial splash) occurring in the initial stage of use of the sputtering target and increase in resistance of the thin film formed by the sputtering target, thereby shortening the aluminum base of the pre-sputtering time. The alloy sputtering target was repeatedly studied. As a result, it was found that, in the aluminum-based alloy sputtering target to be used, not only the surface roughness of the sputtering surface (Ra and Rz in the present invention) but also the average value of the peak intervals represented by the L value is appropriately controlled. When the control is performed in an extended manner, the intended purpose can be achieved, and the present invention has been completed.

即，本發明的鋁基合金濺鍍靶，其特徵在於，以JIS B0601(2001)所規定的方法測量濺鍍面的表面粗糙度時，算術平均粗糙度Ra為1.50μm以下，以及最大高度Rz為10μm以下，並且，將從粗糙度曲線的中心線至波峰或波谷的高度超過(0.5×Rz)的峰值高度分別設為P或Q，於基準長度100mm內，依次計數P和Q時，P到緊鄰其後出現的Q再到緊鄰該Q後出現的P之間的間隔L的平均值為0.4mm以上。In other words, the aluminum-based alloy sputtering target of the present invention is characterized in that the arithmetic mean roughness Ra is 1.50 μm or less and the maximum height Rz when the surface roughness of the sputtering surface is measured by a method defined in JIS B0601 (2001). It is 10 μm or less, and the peak height from the center line of the roughness curve to the peak or the trough exceeds (0.5 × Rz), respectively, as P or Q, and when P and Q are sequentially counted within the reference length of 100 mm, P The average value of the interval L between the Q immediately after the occurrence and the P appearing immediately after the Q is 0.4 mm or more.

首先，本發明的鋁基合金濺鍍靶中，算術平均粗糙度Ra控制在1.50μm以下，以及最大高度Rz控制在10μm以下。通過將Ra控制在1.50μm以下，將Rz控制在10μm以下，能夠縮短使初期飛濺的個數和所形成的薄膜的電阻均降低化(穩定化)至一定水準的預濺鍍的時間(參照後述的實施例)。Ra和Rz的上限較佳為Ra：1.0μm，Rz：8.0μm，更佳的Ra和Rz的上限為Ra：0.8μm，Rz：6.0μm。還有Ra和Rz的下限，從上述觀點出發沒有特別限制，越小越好，但若考慮到機械加工和研磨加工的精度等，則大致以Ra：0.1μm，Rz：1.0μm為宜。First, in the aluminum-based alloy sputtering target of the present invention, the arithmetic mean roughness Ra is controlled to be 1.50 μm or less, and the maximum height Rz is controlled to be 10 μm or less. By controlling Ra to 1.50 μm or less and controlling Rz to 10 μm or less, it is possible to shorten the time for which the number of initial splashes and the resistance of the formed film are reduced (stabilized) to a certain level of pre-sputtering (see below). Example). The upper limit of Ra and Rz is preferably Ra: 1.0 μm, Rz: 8.0 μm, and more preferably Ra and Rz have an upper limit of Ra: 0.8 μm and Rz: 6.0 μm. In addition, the lower limit of Ra and Rz is not particularly limited, and it is preferably as small as possible. However, in consideration of the precision of machining and polishing, etc., Ra: 0.1 μm and Rz: 1.0 μm are preferable.

還有，也可以適宜組合Ra和Rz的上限和下限而形成其各自的範圍。Further, the upper limit and the lower limit of Ra and Rz may be appropriately combined to form their respective ranges.

此外，本發明的鋁基合金濺鍍靶，其特徵在於由L值代表的峰間隔的平均值被控制在0.4mm以上。如後述的實施例所示，只是控制Ra和Rz還得不到預期的特性，只有全部兼具這三個要件時，才能夠迅速實現初期飛濺和薄膜電阻的降低這兩個方面，才能夠縮短預濺鍍時間。Further, the aluminum-based alloy sputtering target of the present invention is characterized in that the average value of the peak intervals represented by the L value is controlled to be 0.4 mm or more. As shown in the later-described embodiment, only the control of Ra and Rz does not achieve the desired characteristics. Only when all three elements are combined, the initial splash and the reduction of the sheet resistance can be quickly achieved. Pre-sputter time.

一邊參照圖1(a)和圖1(b)，一邊對於本發明最具特徵的L值進行說明。圖1(a)和圖1(b)是針對濺鍍靶的濺鍍面，以JIS B0601(2001)所規定的方法進行測量時的粗糙度曲線的概略圖。L值是任意取基準長度100mm的粗糙度曲線，以如下方式進行計算時的值。夾隔粗糙度曲線的中心線，將峰方向的頂點稱為波峰(山的峰值)，將谷方向的底點稱為波谷(谷的峰值)，在本發明中，超過中心線+(0.25×Rz)的位置的波峰為P，超過中心線-(0.25×Rz)的波谷為Q。The L value which is the most characteristic of the present invention will be described with reference to Figs. 1(a) and 1(b). Fig. 1 (a) and Fig. 1 (b) are schematic diagrams showing a roughness curve when a sputtering target of a sputtering target is measured by a method defined in JIS B0601 (2001). The L value is a roughness curve arbitrarily taking a reference length of 100 mm, and the value at the time of calculation is performed as follows. The center line of the roughness curve is called the peak of the peak direction as the peak (peak of the mountain), and the bottom point of the valley direction is called the valley (the peak of the valley). In the present invention, the center line + (0.25 ×) The peak of the position of Rz) is P, and the valley exceeding the center line - (0.25 × Rz) is Q.

首先，參照圖1(a)。在上圖的粗糙度曲線中，基準長度為100mm，H表示中心線±(0.25×Rz)的位置。設高於(中心線+H)的波峰(山的峰值)為P，低於(中心線-H)的波谷(谷的峰值)為Q時，圖1(a)中從最左側依次為P1、Q1、P2、Q2、P3、…。在本發明中，峰間隔L值為P1→Q1→P2之間的距離，詳細地說就是從P1、Q1、P2的各點向中心線引垂線取交點(p1、q1、P2)時，p1-q1-p2之間的距離。於基準長度100m內，以上述方式求得峰間隔L值，計算其平均值。對於粗糙度曲線的任意3處進行同樣的操作，計算其平均值，得到L值的平均值。First, refer to FIG. 1(a). In the roughness curve of the above figure, the reference length is 100 mm, and H represents the position of the center line ± (0.25 × Rz). Let the peak above (center line +H) (peak of the mountain) be P, and the valley below (center line -H) (the peak of the valley) be Q, and P1 from the leftmost side in Fig. 1(a) , Q1, P2, Q2, P3, .... In the present invention, the peak interval L value is a distance between P1 → Q1 → P2, and in detail, when the intersection points (p1, q1, P2) are taken from the respective points of P1, Q1, and P2 toward the center line, p1 The distance between -q1-p2. The peak interval L value was obtained in the above manner within 100 m of the reference length, and the average value was calculated. The same operation was performed for any three of the roughness curves, and the average value was calculated to obtain an average value of the L values.

上述的圖1(a)是超過(中心線±H)的位置的P和Q交互輪流連續形成的例子，但粗糙度曲線例如如圖1(b)所示，有在P與Q之間存在未超過H的位置的波峰和波谷的情況。這時的L值的計算方法如下。以下，由P’表示未超過H的位置的波峰，由Q’表示未超過H的位置的波谷。Fig. 1(a) above is an example in which P and Q interactions exceeding the position of (center line ± H) are continuously formed, but the roughness curve is, for example, as shown in Fig. 1(b), exists between P and Q. The case of peaks and troughs where the position of H is not exceeded. The L value at this time is calculated as follows. Hereinafter, a peak of a position that does not exceed H is represented by P', and a valley of a position that does not exceed H is represented by Q'.

若參照圖1(b)，則以從最左側開始，順次連續形成有超過H的位置的波峰P1、超過H的位置的波峰P2、未超過H的位置的波峰P’1、未超過H的位置的波谷Q’1、超過H的位置的波峰P3、超過H的位置的波谷Q1、超過H的位置的波峰P4。這時，峰間隔L值為P1→Q1→P4之間的距離。Referring to Fig. 1(b), peaks P1 exceeding the position of H, peaks P2 exceeding the position of H, peaks P'1 of the position not exceeding H, and peaks not exceeding H are successively formed from the leftmost side. The valley of the position Q'1, the peak P3 of the position exceeding H, the valley Q1 of the position exceeding H, and the peak P4 of the position exceeding H. At this time, the peak interval L is a distance between P1 → Q1 → P4.

在圖1(b)中，P1後面出現的是P2，而超過H的波峰連續兩次顯示的情況時P2被忽視。在本發明中，波峰→波谷→波峰的順序受到重視。另外在本發明中，沒有超過H的波峰(P’)和沒有超過H的波谷(Q’)即使表現出來也被忽視。根據本發明者們的基礎實驗判明，以上述方式定義的峰間隔與初期飛濺的迅速的降低化和薄膜電阻的迅速的降低化有著密切的相關關係。In Fig. 1(b), P2 appears after P1, and P2 is ignored when the peak exceeding H is displayed twice in succession. In the present invention, the order of peaks → troughs → peaks is taken seriously. Further, in the present invention, no peaks (P') exceeding H and troughs (Q') not exceeding H are neglected even if they are expressed. According to the basic experiments of the present inventors, it has been found that the peak interval defined in the above manner is closely related to the rapid decrease of the initial splash and the rapid decrease of the sheet resistance.

如此計算出的L值的平均值以大為宜，較佳為0.5mm以上，更佳為0.6mm以上。但是，為了增大L值的平均值，機械加工和表面研磨加工所花費的加工時間就有可能過長，因此上限較佳為2.0mm，更佳為1.0mm。The average value of the L value thus calculated is preferably large, preferably 0.5 mm or more, more preferably 0.6 mm or more. However, in order to increase the average value of the L value, the processing time required for the machining and the surface grinding processing may be too long, so the upper limit is preferably 2.0 mm, more preferably 1.0 mm.

在本發明中，通過以上述方式控制L值的平均值，飛濺的降低和所形成的薄膜電阻的降低能夠迅速實現的理由其詳情尚不明確，但推測主要原因是由於峰間隔變寬，週期延長，致使濺鍍靶的表面積變小，因此存在於表面的Al氧化層變少，其結果是所形成的薄膜中的氧量也變少。薄膜中的氧量被認為會對預濺鍍的次數和時間產生很大的影響，但根據本發明時，藉由該氧量之降低，認為是使飛濺和成膜後的薄膜電阻會迅速地降低原因。In the present invention, the reason why the average value of the L value is controlled in the above manner, the decrease in the splash and the decrease in the formed sheet resistance can be quickly realized is not clear, but the main reason is that the peak interval is widened and the period is The elongation causes the surface area of the sputtering target to be small, so that the Al oxide layer existing on the surface is reduced, and as a result, the amount of oxygen in the formed film is also reduced. The amount of oxygen in the film is considered to have a great influence on the number and timing of pre-sputtering. However, according to the present invention, by the decrease in the amount of oxygen, it is considered that the film resistance after splashing and film formation is rapidly Reduce the cause.

以上對於本發明最具特徵的表面粗糙度和峰間隔的平均值進行了說明。The average of the surface roughness and the peak interval which are the most characteristic of the present invention has been described above.

此外，本發明的鋁基合金濺鍍靶之較佳維氏硬度(Hv)為26以上。例如在前述的日本特開平10-158828號公報中，通過使Hv在25以下來降低飛濺的發生，相對於此，在本發明中反而將Hv控制在26以上(大致為26～50Hv左右)，由此能夠容易地控制前述的表面粗糙度和L值的平均值，能夠降低飛濺等的發生。其理由詳情不明，但推測可能是如下原因：在日本特開2001-316808號公報中，是以缺乏加工性的Mo合金為物件，相對於此，在本發明中，如以下詳述，實質上是以純Al或合金元素的添加量非常少、約為2.0原子%左右的富有加工性的Al合金為物件，這種基體的合金的組成的不同表現為硬度的差異。Further, the aluminum-based alloy sputtering target of the present invention preferably has a Vickers hardness (Hv) of 26 or more. For example, in the above-mentioned Japanese Patent Publication No. Hei 10-158828, the occurrence of spatter is reduced by setting Hv to 25 or less. In contrast, in the present invention, Hv is controlled to be 26 or more (approximately 26 to 50 Hv). Thereby, the average value of the surface roughness and the L value described above can be easily controlled, and the occurrence of splashing or the like can be reduced. The reason for the reason is not known, but it is presumed that the reason is as follows: In the Japanese Patent Laid-Open Publication No. 2001-316808, a Mo alloy which lacks workability is used as an object, and in the present invention, as described in detail below, A processable Al alloy having a very small addition amount of pure Al or an alloy element and having a very small addition amount of about 2.0 atom% is an object, and the difference in composition of the alloy of such a matrix is represented by a difference in hardness.

本發明所使用的鋁基合金，除了純Al以外，還可以列舉如下：作為佈線薄膜用鋁基合金濺鍍靶被廣泛使用的含有Nd等元素的Al-Nd合金；含有稀土類元素(較佳為Nd、La、Y)的Al-稀土類元素合金；用於提供可以不經由障壁金屬層而直接與構成像素電極的導電性氧化膜直接接觸的直接接觸技術的Al-Ni合金；進一步含有Nd或Y等稀土類元素的Al-Ni-稀土類元素合金；含有Ta的Al-Ta合金等。較佳為Nd、Ni和Y等合金元素的量(合計量)大致為2.0原子%以下。在純Al和Al合金中，作為不可避免的雜質，例如含有在製造過程等之中不可避免混入的元素，例如有Fe、Si、Cu、C、O、N等。The aluminum-based alloy used in the present invention may be, in addition to pure Al, an Al-Nd alloy containing an element such as Nd which is widely used as an aluminum-based alloy sputtering target for wiring films, and contains a rare earth element (preferably). An Al- rare earth element alloy of Nd, La, Y); an Al-Ni alloy for providing a direct contact technique capable of directly contacting a conductive oxide film constituting a pixel electrode without passing through a barrier metal layer; further containing Nd Or an Al-Ni-rare earth element alloy of a rare earth element such as Y; an Al-Ta alloy containing Ta or the like. The amount (total amount) of the alloying elements such as Nd, Ni, and Y is preferably approximately 2.0 atom% or less. In the pure Al and the Al alloy, as an unavoidable impurity, for example, an element which is inevitably mixed in a manufacturing process or the like, for example, Fe, Si, Cu, C, O, N or the like is contained.

接下來，說明製造本發明的濺鍍靶的方法。Next, a method of manufacturing the sputtering target of the present invention will be described.

本發明規定的表面粗糙度和L值的平均值能夠通過下述方式實現：遵循常規方法加工成既定的形狀後，適當控制作為濺鍍面的精加工的機械加工的條件，再根據需要適當控制與該機械加工一起進行的表面研磨加工的條件。機械加工代表性的是進行使用銑床的銑磨加工，較佳為將轉數控制在大約2500～4500rpm(更佳為3000～4000rpm)，將切入量控制在0.02～0.2mm左右(更優選為0.05～0.15mm)，將送給速度控制為大約400～1800mm/min(更佳為大約600～1000mm/min)。還有，關於上述轉數、切如量、送給速度各條件，也可以為適宜將其上限和下限加以組合而成的範圍。The average value of the surface roughness and the L value prescribed by the present invention can be achieved by appropriately controlling the conditions of the finishing machining as the sputtered surface after being processed into a predetermined shape according to a conventional method, and appropriately controlling as needed The conditions of the surface grinding process performed together with the machining. Mechanical processing is typically performed by milling using a milling machine. Preferably, the number of revolutions is controlled to be about 2,500 to 4,500 rpm (more preferably 3,000 to 4,000 rpm), and the amount of cutting is controlled to be about 0.02 to 0.2 mm (more preferably 0.05). ～0.15 mm), the feed speed is controlled to be about 400 to 1800 mm/min (more preferably about 600 to 1000 mm/min). Further, the respective conditions of the number of revolutions, the amount of cut, and the feed rate may be a range in which the upper limit and the lower limit are appropriately combined.

另外，表面研磨加工是在上述的機械加工後再根據需所進行，較佳為使用適當的粒度的磨石進行研磨，以便容易獲得預期的表面性狀。具體來說，較佳為使用塗布有磨石的粒度編號(磨粒)大致為200～1200的磨粒的不織布等，直到磨削至預期的性狀。更佳的磨粒的下限大致為400。在本發明中，最佳為使用大致800左右的磨粒進行研磨。還有，磨石的粒度(磨粒)是磨粒編號越大，磨粒越細。Further, the surface grinding process is carried out as needed after the above-described mechanical processing, and it is preferred to use a grindstone of an appropriate particle size for grinding to easily obtain a desired surface property. Specifically, it is preferred to use a non-woven fabric or the like coated with abrasive grains having abrasive grains having a particle size number (abrasive grain) of approximately 200 to 1200 until grinding to a desired property. The lower limit of the preferred abrasive particles is approximately 400. In the present invention, it is preferable to perform grinding using abrasive grains of approximately 800 or so. Also, the particle size (abrasive grain) of the grindstone is such that the larger the grindstone number, the finer the abrasive grains.

在本發明中所具有的特徵在於，如上述通過適當控制機械加工或表面研磨加工，從而控制表面性狀，其以外的製造步驟未特別限定，能夠採用在鋁基合金濺鍍靶的製造通常所使用的步驟。具體來說，能夠採用公知的噴鍍成形和熔融鑄造法等。本發明所使用的噴鍍成形法沒有特別限定，但例如能夠參照日本特開2009-35766號公報、日本特開2008-240141號公報、日本特開2008-127632號公報、日本特開2007-247006號公報、日本特開2005-82855號公報等的記載。為了降低製造成本，較佳為採用熔融鑄造法。In the present invention, the surface properties are controlled by appropriately controlling the machining or the surface polishing, and the other manufacturing steps are not particularly limited, and can be generally used in the production of an aluminum-based alloy sputtering target. A step of. Specifically, a known spray coating method, a melt casting method, or the like can be employed. The thermal spraying method to be used in the present invention is not particularly limited. For example, JP-A-2009-35766, JP-A-2008-240141, JP-A-2008-127632, and JP-A-2007-247006 Japanese Laid-Open Patent Publication No. 2005-82855, and the like. In order to reduce the manufacturing cost, it is preferred to use a melt casting method.

[實施例][Examples]

以下，列舉實施例更具體地說明本發明，但本發明不受下述實施例限定，在能夠符合本發明的宗旨的範圍內可以適當加以變更實施，這些均包含在本發明的技術範圍內。The present invention is not limited by the following examples, but the present invention is not limited to the following examples, and may be appropriately modified and implemented within the scope of the present invention, and these are all included in the technical scope of the present invention.

實施例1Example 1

準備表1所示的組成的鋁基合金(餘量：Al和不可避免的雜質)，按以下的方法製作濺鍍靶。An aluminum-based alloy having the composition shown in Table 1 (balance: Al and unavoidable impurities) was prepared, and a sputtering target was produced in the following manner.

其中Al-Nd合金是使用噴鍍成形法製造鑄塊，進行熱處理、熱加工(軋製)，該噴鍍成形法是在惰性氣氛中的反應室內對Al合金熔液流噴送高壓的惰性氣體而進行噴霧化，使急冷至半熔融狀態、半凝固狀態、固相狀態的粒子堆積，從而得到既定形狀的原形材(預成型坯)的方法。另外，純Al通過DC鑄造法鑄成厚100mm的鑄塊後，以400℃進行4小時均熱處理，接著在室溫下以75%的壓下量進行冷加工後，以200℃進行熱處理，在室溫下以40%的壓下量進行冷軋。The Al-Nd alloy is produced by a spray forming method, and is subjected to heat treatment and hot working (rolling). The spray forming method is to spray a high-pressure inert gas to the Al alloy melt stream in a reaction chamber in an inert atmosphere. In the case of atomization, particles which are quenched to a semi-molten state, a semi-solidified state, and a solid phase state are deposited to obtain a prototype (preform) having a predetermined shape. In addition, pure Al was cast into a 100 mm thick ingot by DC casting, and then subjected to a soaking treatment at 400 ° C for 4 hours, followed by cold working at a room temperature of 75%, followed by heat treatment at 200 ° C. Cold rolling was carried out at a temperature of 40%.

接著，切斷如此得到的Al-Nd合金和純Al的軋製板，以表1所示的加工條件，對軋製板的表面進行機械加工或進行機械加工和表面研磨加工，得到濺鍍靶的各試料。Next, the thus obtained Al-Nd alloy and pure Al rolled sheet were cut, and the surface of the rolled sheet was machined or machined and surface-polished to obtain a sputtering target under the processing conditions shown in Table 1. Each sample.

使用如此得到的試料，進行表面粗糙度的算術平均粗糙度(Ra)和最大高度(Rz)的測量。上述算術平均粗糙度(Ra)和最大高度(Rz)的測量使用Mitutoyo製表面粗糙度測量儀SJ-301進行測量。評價長度為100mm。此外，基於前述的方法計算L值的平均值。Using the sample thus obtained, measurement of arithmetic mean roughness (Ra) and maximum height (Rz) of surface roughness was performed. The above arithmetic mean roughness (Ra) and maximum height (Rz) were measured using a Mitutoyo surface roughness measuring instrument SJ-301. The evaluation length is 100 mm. Further, the average value of the L values is calculated based on the aforementioned method.

另外，使用上述濺鍍靶的各試料形成薄膜，評價直至薄膜滿足規定的條件的濺鍍時間。Further, a film was formed using each of the samples of the sputtering target, and the sputtering time until the film satisfies the predetermined conditions was evaluated.

具體來說，通過DC磁控管濺鍍法，進行預濺鍍和濺鍍下的成膜。預濺鍍時，在靶與基板之間***擋板而不在基板上成膜，濺鍍時移開擋板而在基板上進行成膜。預濺鍍條件和濺鍍條件的詳情如下，除濺鍍功率不同以外其他均相同。Specifically, film formation under pre-sputtering and sputtering is performed by DC magnetron sputtering. In the case of pre-sputtering, a baffle is inserted between the target and the substrate without forming a film on the substrate, and the baffle is removed during sputtering to form a film on the substrate. Details of the pre-sputtering conditions and sputtering conditions are as follows, except that the sputtering power is different.

濺鍍裝置(通用)：Sputtering device (general):

股份有限公司島津製作所製“sputtering system HSR-542S”"sputtering system HSR-542S" manufactured by Shimadzu Corporation

預濺鍍條件Pre-sputter condition

背壓：0.43×10^-3 Pa以下Back pressure: 0.43×10 ^-3 Pa or less

Ar氣壓：0.67PaAr pressure: 0.67Pa

濺鍍功率：800WSputtering power: 800W

濺鍍條件Sputtering conditions

背壓：0.43×10^-3 Pa以下Back pressure: 0.43×10 ^-3 Pa or less

Ar氣壓：0.67PaAr pressure: 0.67Pa

濺鍍功率：300WSputtering power: 300W

極間距離：100mmDistance between poles: 100mm

基板溫度：室溫Substrate temperature: room temperature

基板：玻璃基板(尺寸：直徑6英寸)Substrate: Glass substrate (size: 6 inches in diameter)

詳細地說，就是使用上述濺鍍靶的各試料，以上述條件進行預濺鍍5分鐘後，再以上述條件進行濺鍍而形成薄膜(膜厚300nm)，以此作為一套操作而反復進行，以如下方式分別測量(1)飛濺個數達到基準值以下的預濺鍍時間，和(2)形成的薄膜的電阻(佈線電阻)相對於正常值達到+15%以下的預濺鍍時間。Specifically, each of the samples of the sputtering target was subjected to pre-sputtering for 5 minutes under the above conditions, and then sputtering was performed under the above conditions to form a thin film (thickness: 300 nm), which was repeated as a set of operations. The pre-sputtering time of (1) the number of spatters below the reference value is measured as follows, and (2) the pre-sputtering time of the formed film (resistance of the wiring) is +15% or less with respect to the normal value.

(1)飛濺個數達到基準值以下的預濺鍍時間的評價方法(1) Evaluation method of pre-sputtering time in which the number of spatters is below the reference value

對於以上述濺鍍條件形成的薄膜，按以下的條件測量發生的飛濺(初期飛濺)的個數。With respect to the film formed under the above-described sputtering conditions, the number of occurrences of spatter (initial splash) was measured under the following conditions.

使用粒子計數器(股份有限公司topcon製：晶片表面檢查裝置WM-3)，計測在上述薄膜的表面確認到的粒子的位置座標、尺寸(平均粒徑)和個數。在此，尺寸為3μm以上的視為粒子。其後對該薄膜表面進行光學顯微鏡觀察(倍率：1000倍)，形狀為半球形的視為飛濺，計測每單位面積中的飛濺的個數。在本實施例中，反復進行預濺鍍和濺鍍，直至如此得到的初期飛濺的發生數達到8個/cm² 以下。在本實施例中，初期飛濺的發生數達到8個/cm² 以下的預濺鍍時間在60分鐘以下的試料為合格。The position coordinates, size (average particle diameter) and number of particles confirmed on the surface of the film were measured using a particle counter (manufactured by Topcon Co., Ltd.: Wafer Surface Inspection Apparatus WM-3). Here, a particle having a size of 3 μm or more is regarded as a particle. Thereafter, the surface of the film was observed under an optical microscope (magnification: 1000 times), and the shape of the hemisphere was regarded as a splash, and the number of spatters per unit area was measured. In the present embodiment, pre-sputtering and sputtering are repeated until the number of occurrences of the initial splash thus obtained reaches 8/cm ² or less. In the present embodiment, the sample having a pre-sputtering time of 8 pieces/cm ² or less and having a pre-sputtering time of 60 minutes or less was acceptable.

(2)薄膜的電阻相對於正常值達到+15%以下的預濺鍍時間的測量方法(2) Method for measuring the pre-sputtering time of the film resistance with respect to the normal value of +15% or less

對於以上述濺鍍條件所形成的薄膜，設想在實際步驟中受到的熱過程而進行以320℃保持30分鐘的熱處理後，加工成線寬100μm的條紋圖案(stripe pattern)形狀，通過濕刻蝕加工成線寬100μm、線長10mm的佈線電阻測量用圖案狀。濕刻蝕使用H₃ PO₄ :HNO₃ :H₂ O=75:5:20的混合液。對於加工成圖案狀的薄膜，通過四探針法在室溫下測量電阻率值。For the film formed under the above-described sputtering conditions, it is assumed that the heat treatment subjected to the actual step is performed at 320 ° C for 30 minutes, and then processed into a stripe pattern shape having a line width of 100 μm, by wet etching. It was processed into a pattern for measuring the wiring resistance of a line width of 100 μm and a line length of 10 mm. A wet liquid was used for the wet etching using a mixture of H ₃ PO ₄ :HNO ₃ :H ₂ O=75:5:20. For the film processed into a pattern, the resistivity value was measured at room temperature by a four-probe method.

反復進行預濺鍍和濺鍍，直至如此得到的電阻率值相對於正常值(A1-2.0原子%Nd合金為4.6μΩ‧cm，純Al為3.2μΩ‧cm)達到+15%以下。在本實施例中，電阻率值達到正常值+15%以下的預濺鍍時間在60分鐘以下的試料為合格。The pre-sputtering and sputtering were repeated until the resistivity value thus obtained reached +15% or less with respect to the normal value (4.6 μΩ·cm for A1-2.0 at% of Nd alloy and 3.2 μΩ·cm for pure Al). In the present embodiment, the sample having a pre-sputtering time of a resistivity value of +15% or less and a pre-sputtering time of 60 minutes or less was acceptable.

這些測量結果顯示在表1中。These measurements are shown in Table 1.

另外，為了參考，在圖2(a)中顯示試料No.7(比較例)的濺鍍面的表面粗糙度曲線，在圖2(b)中顯示試料No.2(本發明例)的濺鍍面的表面粗糙度曲線。Further, for reference, the surface roughness curve of the sputter surface of Sample No. 7 (Comparative Example) is shown in Fig. 2(a), and the splash of Sample No. 2 (Example of the present invention) is shown in Fig. 2(b). Surface roughness curve of the plated surface.

首先，以本發明的推薦條件進行加工的試料No.1~6，表面性狀(Ra、Rz、峰間隔L的平均值)得到適當的控制，因此在使用純Al濺鍍靶和Al-Nd濺鍍靶的任意一種的情況下，都能夠縮短至飛濺個數降低的預濺鍍時間和至電阻穩定化的預濺鍍時間兩方面。First, in the samples No. 1 to 6 which were processed under the recommended conditions of the present invention, the surface properties (average values of Ra, Rz, and peak interval L) were appropriately controlled, and therefore, a pure Al sputtering target and Al-Nd sputtering were used. In the case of any of the plating targets, it is possible to shorten both the pre-sputtering time in which the number of splashes is reduced and the pre-sputtering time in which the resistance is stabilized.

相對於此，表1的No.7是使用Al-Nd濺鍍靶只進行銑磨加工的例子，因為銑磨加工時的轉數過高，所以Ra、Rz、峰間隔L的平均值全部超出本發明的範圍，至飛濺個數降低的預濺鍍時間和至電阻穩定化的預濺鍍時間這兩方均長。On the other hand, No. 7 in Table 1 is an example in which only the milling process is performed using the Al-Nd sputtering target, and since the number of revolutions during the milling process is too high, the average values of Ra, Rz, and the peak interval L are all exceeded. The scope of the present invention ranges from the pre-sputtering time in which the number of splashes is reduced to the pre-sputtering time in which the resistance is stabilized.

表1的No.8和No.9是使用純Al濺鍍靶進行銑磨加工(No.8)、銑磨加工和表面研磨加工兩方面(No.9)的例子。其中No.8因為銑磨加工時的轉數過高，雖然Ra和Rz良好，但是峰間隔L的平均值變短，至薄膜的電阻穩定化的預濺鍍時間變長。No.9雖然銑磨加工條件適當，但表面研磨加工時的磨粒過粗，因此儘管峰間隔L的平均值良好，但Ra和Rz變大，至飛濺個數降低的預濺鍍時間變長。No. 8 and No. 9 of Table 1 are examples of milling (No. 8), milling processing, and surface polishing processing (No. 9) using a pure Al sputtering target. Among them, No. 8 has a high number of revolutions during the milling process, and although Ra and Rz are good, the average value of the peak interval L is shortened, and the pre-sputtering time for stabilizing the resistance of the film becomes long. In No. 9, although the milling processing conditions are appropriate, the abrasive grains during surface grinding are too thick. Therefore, although the average value of the peak interval L is good, Ra and Rz become large, and the pre-sputtering time which decreases the number of splashes becomes long. .

參照特定的實施方式對於本申請進行了詳細的說明，但在不脫離本發明的精神和範圍的情況下能夠施加各種變更和修改，這一點對於從業者來說應該清楚。The present invention has been described in detail with reference to the preferred embodiments thereof, and various changes and modifications can be made without departing from the spirit and scope of the invention.

本申請基於2009年12月18日申請的日本專利申請(專利申請2009-287650)，其內容在此作為參照引入。The present application is based on a Japanese patent application (Patent Application No. 2009-287650) filed on Dec.

圖1(a)和圖1(b)是用於說明本發明所規定的L值(峰間隔)的模擬圖。Fig. 1 (a) and Fig. 1 (b) are simulation diagrams for explaining the L value (peak interval) prescribed by the present invention.

圖2(a)表示實施例1的試料No.7(比較例)的濺鍍面的表面粗糙度曲線，圖2(b)表示實施例1的試料No.2(本發明例)的濺鍍面的表面粗糙度曲線。2(a) shows the surface roughness curve of the sputter surface of Sample No. 7 (Comparative Example) of Example 1, and FIG. 2(b) shows the sputtering of Sample No. 2 (Example of the present invention) of Example 1. Surface roughness curve of the surface.

Claims (1)

一種純鋁或鋁合金濺鍍靶，其特徵係以JIS B0601(2001)所規定的方法測量濺鍍面的表面粗糙度時，算術平均粗糙度Ra為1.50μm以下，以及最大高度Rz為10μm以下，並且，將從粗糙度曲線的中心線至波峰或波谷的高度超過0.25×Rz的峰值高度分別設為P或Q，於基準長度100mm內，依次計數P和Q時，P到緊鄰其後出現的Q再到緊鄰該Q後出現的P之間的間隔L的平均值為0.4mm以上。 A pure aluminum or aluminum alloy sputtering target characterized in that the arithmetic mean roughness Ra is 1.50 μm or less and the maximum height Rz is 10 μm or less when the surface roughness of the sputtering surface is measured by a method specified in JIS B0601 (2001). And, the peak height from the center line of the roughness curve to the peak or trough height exceeding 0.25 × Rz is set to P or Q, respectively. When P and Q are sequentially counted within the reference length of 100 mm, P appears immediately after it. The average value of the interval L between the Q and the P appearing immediately after the Q is 0.4 mm or more.