TW202216436A - Laminated structure, and method for manufacturing laminated structure - Google Patents
Laminated structure, and method for manufacturing laminated structure Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 86
- 239000010936 titanium Substances 0.000 claims abstract description 86
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 42
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 26
- 238000004544 sputter deposition Methods 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000010408 film Substances 0.000 description 34
- 238000002474 experimental method Methods 0.000 description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 230000015572 biosynthetic process Effects 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 13
- 238000009864 tensile test Methods 0.000 description 11
- 229910052786 argon Inorganic materials 0.000 description 8
- 239000012535 impurity Substances 0.000 description 6
- 229920001721 polyimide Polymers 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 150000003609 titanium compounds Chemical class 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 238000012546 transfer Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
Description
本發明係關於依序層積第1鈦層、鋁層、第2鈦層之層積構造體及層積構造體之製造方法。The present invention relates to a laminated structure in which a first titanium layer, an aluminum layer, and a second titanium layer are sequentially laminated, and a method for producing the laminated structure.
此種層積構造體,在顯示器、智能手機或電子紙等電子裝置,作為開關元件(薄膜電晶體)之源極/汲極電極使用(例如參照專利文獻1)。另一方面,伴隨著近年的具有可撓性的電子裝置的開發,對具有比較高硬度的鈦層的層積體構造,要求高的耐屈曲性。Such a laminated structure is used as source/drain electrodes of switching elements (thin film transistors) in electronic devices such as displays, smartphones, and electronic paper (for example, see Patent Document 1). On the other hand, with the development of flexible electronic devices in recent years, high buckling resistance is required for a laminate structure having a titanium layer having a relatively high hardness.
一般而言,層積構造體之鈦層或鋁層,在真空氛圍中藉由濺鍍法一貫地成膜(例如參照專利文獻1)。例如,在成膜鈦層或鋁層時,使鈦製或者鋁製的靶與基材對向配置的真空室內真空排氣到特定壓力後,對真空室內導入稀有氣體(例如氬氣),對靶投入具有負的電位之直流電力形成電漿,在電漿中藉由電離的稀有氣體的離子濺射靶,使由靶飛散的濺射粒子附著、堆積於基材,以所要的膜厚(例如,第1鈦層50nm,鋁層500nm,第2鈦層50nm)形成鈦層或鋁層。此時,對靶的施加電力、稀有氣體的氣體導入量或成膜中的真空室內的全壓等各種濺鍍條件,要考慮生產性或膜厚分布而設定(例如,施加電力20~40kW,全壓0.2~1.0Pa)。Generally, the titanium layer or the aluminum layer of the laminated structure is uniformly formed by sputtering in a vacuum atmosphere (for example, refer to Patent Document 1). For example, when forming a titanium layer or an aluminum layer, a vacuum chamber in which a titanium or aluminum target and a substrate are arranged to face each other is evacuated to a specific pressure, and then a rare gas (eg, argon) is introduced into the vacuum chamber to The target is injected with a DC power having a negative potential to form a plasma, and the target is sputtered by ions of an ionized rare gas in the plasma. For example, the first titanium layer is 50 nm, the aluminum layer is 500 nm, and the second titanium layer is 50 nm) to form a titanium layer or an aluminum layer. At this time, various sputtering conditions such as the power applied to the target, the gas introduction amount of the rare gas, and the total pressure in the vacuum chamber during film formation are set in consideration of productivity and film thickness distribution (for example, applied power of 20 to 40 kW, Full pressure 0.2~1.0Pa).
此處,為了確認層積構造體的耐屈曲性,使用特定形狀的試驗基材,於試驗基材表面以特定的濺鍍條件依序層積第1鈦層、鋁層、第2鈦層之後,對由試驗基材剝離的層積構造體實施拉伸試驗時,查明了僅施加提供5%的伸長量所必要的拉伸荷重,層積構造體伸長2倍以上。此外,觀察拉伸試驗後的層積構造體的表面(亦即鈦層表面)狀態時,查明了在鈦層發生著多數個在厚度方向上延伸的龜裂。在此,本案發明人等,反覆進行銳意研究,得到了比較小的結晶粒排列於膜厚方向而具有以結晶粒界在其膜厚方向延伸的方式連接之結晶構造,同時由於成膜時帶入鈦層內的氮分子或氧分子等不純物而被形成導致結晶粒界硬且脆之氮化鈦或氧化鈦等鈦化合物的話,層積構造體無法得到強的耐屈曲性之知識見解。 [先前技術文獻] [專利文獻] Here, in order to confirm the buckling resistance of the laminated structure, a test substrate of a specific shape was used, and a first titanium layer, an aluminum layer, and a second titanium layer were sequentially laminated on the surface of the test substrate under specific sputtering conditions. , when a tensile test was performed on the laminated structure peeled from the test base material, it was found that the laminated structure stretched by 2 times or more by applying only the tensile load necessary to provide an elongation of 5%. In addition, when the state of the surface of the laminated structure after the tensile test (that is, the surface of the titanium layer) was observed, it was found that a large number of cracks extending in the thickness direction were generated in the titanium layer. Here, the inventors of the present invention have repeatedly conducted intensive research, and obtained a crystal structure in which relatively small crystal grains are arranged in the film thickness direction and have a crystal structure connected so that the crystal grain boundaries extend in the film thickness direction. If impurities such as nitrogen molecules or oxygen molecules are incorporated into the titanium layer to form titanium compounds such as titanium nitride or titanium oxide that make crystal grain boundaries hard and brittle, it is known that the laminated structure cannot obtain strong buckling resistance. [Prior Art Literature] [Patent Literature]
[專利文獻1]日本特開2015-177105號公報[Patent Document 1] Japanese Patent Laid-Open No. 2015-177105
[發明所欲解決之課題][The problem to be solved by the invention]
本發明係有鑑於前述知識見解而完成者,課題在於提供具有強的耐屈曲性的層積構造體及層積構造體之製造方法。 [供解決課題之手段] The present invention has been made in view of the above-mentioned knowledge and knowledge, and an object of the present invention is to provide a laminated structure having strong buckling resistance and a method for producing the laminated structure. [Means for solving problems]
為了解決前述課題,依序層積第1鈦層、鋁層、第2鈦層之本發明的層積構造體,特徵為第1及第2鈦層之各鈦層,具有在根據X線繞射測定之密勒指數的(002)面及(100)面有繞射峰之結晶構造,在(002)面之繞射峰的半峰全幅值為1.0deg以下,在(100)面的繞射峰的半峰全幅值為0.6deg以下。在此場合,前述鋁層,以具有在根據X線繞射測定之密勒指數的(111)面有繞射峰之結晶構造為佳。In order to solve the aforementioned problems, the laminated structure of the present invention in which a first titanium layer, an aluminum layer, and a second titanium layer are sequentially laminated is characterized in that each titanium layer of the first and second titanium layers has an X-ray winding. The (002) plane and (100) plane of the Miller index measured by radiation have a crystal structure with diffraction peaks. The full width at half maximum of the emission peak is 0.6deg or less. In this case, the aluminum layer preferably has a crystal structure having a diffraction peak on the (111) plane of the Miller index measured by X-ray diffraction.
此外,為了解決前述課題,製造依序層積第1鈦層、鋁層、第2鈦層之層積構造體的本發明之層積構造體之製造方法,包含:藉由濺鍍法,於基材上成膜第1鈦層之第1步驟,於第1鈦層之上成膜鋁層之第2步驟,以及在鋁層之上成膜第2鈦層之第3步驟;第1及第3步驟之各步驟,進而包含:直到分別達到氮氣分壓3.0×10 -4Pa以下、氧氣分壓9.0×10 -5Pa以下、水蒸氣分壓8.0×10 -4Pa以下、氫氣分壓5.0×10 -5Pa以下為止,真空排氣被配置鈦製之靶與基材之真空室內的真空排氣步驟,以維持真空室內的全壓為0.2Pa~0.5Pa之範圍內的方式導入稀有氣體,對鈦製的靶施加特定電力並以3nm/sec~5nm/sec的範圍內之成膜速度成膜第1及第2鈦層的各層之成膜步驟。在此場合,前述第2步驟,最好是進而包含:以被配置鋁製之靶與基材之真空室內的全壓維持在0.2Pa~0.5Pa之範圍內的方式導入稀有氣體,對鋁製的靶施加特定電力並以7nm/sec~10nm/sec的範圍內之成膜速度成膜鋁層之成膜步驟。 In addition, in order to solve the above-mentioned problems, a method for manufacturing a laminated structure of the present invention for manufacturing a laminated structure in which a first titanium layer, an aluminum layer, and a second titanium layer are sequentially laminated comprises: by sputtering, on The first step of forming a first titanium layer on the substrate, the second step of forming an aluminum layer on the first titanium layer, and the third step of forming a second titanium layer on the aluminum layer; the first and Each step of the third step further includes: until the partial pressure of nitrogen is 3.0×10 -4 Pa or less, the partial pressure of oxygen is 9.0×10 -5 Pa or less, the partial pressure of water vapor is 8.0×10 -4 Pa or less, and the partial pressure of hydrogen is reached. Up to 5.0×10 -5 Pa or less, vacuum evacuation is carried out in the vacuum evacuation step in the vacuum chamber where the titanium target and the substrate are arranged, and the rare earth is introduced so that the total pressure in the vacuum chamber is maintained within the range of 0.2Pa to 0.5Pa. A gas is applied to a titanium target, and a specific electric power is applied to form a film of each of the first and second titanium layers at a film-forming rate in the range of 3 nm/sec to 5 nm/sec. In this case, the second step preferably further includes introducing a rare gas so that the total pressure in the vacuum chamber in which the aluminum target and the substrate are arranged is maintained within a range of 0.2Pa to 0.5Pa, and the aluminum A film-forming step of forming an aluminum layer at a film-forming speed in the range of 7 nm/sec to 10 nm/sec by applying a specific electric power to the target.
根據以上,先於在真空氛圍中在真空室內藉由濺鍍法成膜第1鈦層、鋁層及第2鈦層,藉著使真空室內真空排氣直到不純物氣體(例如氮氣、氧氣、水蒸氣氣體、氫氣)的分壓達到特定值以下,可達成抑制在第1及第2鈦層之各層的結晶粒界,被形成氮化鈦或氧化鈦等鈦化合物。接著,第1及第2鈦層之各層成膜時,使其成膜速度在3nm/sec~5nm/sec之範圍內的話,可以使第1及第2鈦層之各層,具有粒徑大的結晶粒在其膜厚方向上不規則重疊且結晶粒界在膜厚方向上不連接的結晶構造。According to the above, prior to forming the first titanium layer, the aluminum layer and the second titanium layer by sputtering in the vacuum chamber in a vacuum atmosphere, the vacuum chamber is evacuated until the impurity gas (such as nitrogen, oxygen, water) When the partial pressure of vapor gas, hydrogen) becomes below a specific value, it is possible to suppress the formation of titanium compounds such as titanium nitride and titanium oxide at the crystal grain boundaries of each of the first and second titanium layers. Next, when each of the first and second titanium layers is formed into a film, if the film-forming speed is in the range of 3 nm/sec to 5 nm/sec, each of the first and second titanium layers can have a large particle size. A crystal structure in which crystal grains are irregularly overlapped in the film thickness direction and crystal grain boundaries are not connected in the film thickness direction.
使如前述作法而成膜之鈦層進行X線繞射時,確認在(002)面之繞射峰與在(100)面之繞射峰,在(100)面之繞射峰對在(002)面之繞射峰的強度比為0.20以上。此時,在(002)面的繞射峰的半峰全幅值為1.0deg以下、在(100)面的繞射峰的半峰全幅值為0.6deg以下,由此,具有前述繞射圖案的話,於第1及第2鈦層之各鈦層的結晶粒界,抑制鈦化合物的形成,成為具有粒徑大的結晶粒在其膜厚方向上不規則重疊且結晶粒界不連接的結晶構造。接著,對前述同樣的層積構造體的拉伸試驗即使施加5%或者10%之伸長量所必要的拉伸荷重,層積構造體的伸長量也被抑制在10%以內,而且,拉伸試驗後的層積構造體的表面觀察,也確認了沒有發生龜裂。結果,本發明之層積構造體,與從前的例子相比具有強的耐屈曲性。When the titanium layer formed as described above is subjected to X-ray diffraction, the diffraction peak on the (002) plane and the diffraction peak on the (100) plane are confirmed, and the diffraction peak on the (100) plane is opposite to the diffraction peak on the (100) plane. The intensity ratio of the diffraction peak of the 002) plane is 0.20 or more. At this time, the full width at half maximum of the diffraction peak on the (002) plane is 1.0 degrees or less, and the full width at half maximum of the diffraction peak on the (100) plane is 0.6 degrees or less. In the case of patterning, the formation of titanium compounds is suppressed in the crystal grain boundaries of each titanium layer of the first and second titanium layers, and the crystal grains with large particle diameters are irregularly overlapped in the film thickness direction and the crystal grain boundaries are not connected. Crystal structure. Next, in the tensile test of the same laminate structure as described above, even if a tensile load required for an elongation of 5% or 10% was applied, the elongation of the laminate structure was suppressed within 10%. The surface observation of the laminated structure after the test also confirmed that no cracks occurred. As a result, the laminated structure of the present invention has higher buckling resistance than the conventional examples.
以下,參照圖式說明本發明之層積構造體及層積構造體之製造方法的實施型態。Hereinafter, embodiments of the laminated structure and the method for producing the laminated structure of the present invention will be described with reference to the drawings.
如圖1所示,本實施型態的層積構造體LS,係將基材Sw做成例如在玻璃基板Sg的表面黏貼聚醯亞胺膜Pf(在玻璃基板Sg與聚醯亞胺膜Pf之邊界面可以剝離),且於基材Sw表面具備在真空氛圍中藉由濺鍍法一貫地依序成膜(層積)之第1鈦層L1、鋁層L2、與第2鈦層L3。As shown in FIG. 1 , in the laminated structure LS of the present embodiment, the base material Sw is formed by, for example, pasting a polyimide film Pf on the surface of a glass substrate Sg (on the glass substrate Sg and the polyimide film Pf). The boundary surface can be peeled off), and the surface of the substrate Sw is provided with a first titanium layer L1, an aluminum layer L2, and a second titanium layer L3, which are consistently formed (laminated) sequentially by sputtering in a vacuum atmosphere. .
如圖2所示,可以利用於前述層積構造體LS之濺鍍裝置Sm係所謂叢集工具(cluster tool)式的裝置,具備設有搬送機器手臂R的中央搬送真空室Tc,並於中央搬送真空室Tc的周圍中介柵型閥Gv而分別連結著載入載出真空室Lc、成膜第1鈦層L1的真空室(以下簡稱「成膜真空室」)Pc1、成膜鋁層L2的成膜真空室Pc2、成膜第2鈦層L3的成膜真空室Pc3。在此,於成膜真空室Pc1,Pc2,Pc3內,由於除了使用的靶以外,設有相同的構造零件,所以參照圖3並以成膜真空室Pc1為例說明的話,於成膜真空室Pc1連接通向由渦輪式分子泵或旋轉式泵等構成的真空泵單元Pu之排氣管11,可以將成膜真空室Pc1真空排氣直到特定的真空度(例如1×10
-6Pa)。於真空室Pc1的側壁,連接介設質量流量控制器12的氣管13,可以將被流量控制的稀有氣體(例如氬氣)導入成膜真空室Pc1內。於成膜真空室Pc1的上部,以面向基材Sw的姿勢配置鈦製的靶2(在成膜真空室Pc2為鋁製的靶),並於其上方配置著公知的磁石單元3。
As shown in FIG. 2 , the sputtering apparatus Sm that can be used for the above-mentioned laminated structure LS is a so-called cluster tool type apparatus, and includes a central transfer vacuum chamber Tc provided with a transfer robot R, and transfers the central The surrounding of the vacuum chamber Tc is connected to the load-out vacuum chamber Lc, the vacuum chamber for forming the first titanium layer L1 (hereinafter referred to as the "film-forming vacuum chamber") Pc1, and the film-forming aluminum layer L2 through a gate valve Gv, respectively. The film-forming vacuum chamber Pc2 and the film-forming vacuum chamber Pc3 for forming the second titanium layer L3. Here, the film formation vacuum chambers Pc1, Pc2, and Pc3 are provided with the same structural components except for the target to be used. Therefore, referring to FIG. 3 and taking the film formation vacuum chamber Pc1 as an example, the film formation vacuum chamber Pc1 is connected to the
使用純度99.9%以上的鈦製的靶2,此外,使用純度99.99%以上的鋁製的靶。於靶2,連接來自濺鍍電源Ps的輸出,可以對靶2投入具有負的電位之直流電力。於成膜真空室Pc1的下部,配置對向於靶2的載物台4,可以設置基材Sw。於成膜真空室Pc1,設置著測定其內部的全壓與不純物氣體(例如氮氣、氧氣、水蒸氣氣體、氫氣)的分壓之測定器5。作為這樣的測定器5,可以利用電離真空計或質量分析計等公知的測定器,所以省略進一步的說明。以下具體地說明利用濺鍍裝置Sm之層積構造體LS的製造方法。The
對大氣氛圍的載入載出真空室Lc投入基材Sw,真空排氣載入載出真空室Lc之後,藉由搬送機械臂R將基材Sw搬送至成膜真空室Pc1。又,在往載入載出真空室Lc投入基材Sw之前,搬送真空室Tc及各成膜真空室Pc1, Pc2,Pc3被真空排氣直到預先特定壓力(1×10
-3Pa)為止,且成為待機狀態。當基材Sw被設置於成膜真空室Pc1的載物台4上時,續行真空排氣,直到達到利用質量分析計5測定的氮氣分壓3.0×10
-4Pa以下、氧氣分壓9.0×10
-5Pa以下、水蒸氣分壓8.0×10
-4Pa以下、氫氣分壓5.0×10
-5Pa以下為止,真空排氣成膜真空室Pc1內(第1步驟的真空排氣步驟)。
The base material Sw is loaded into the load-carrying/unloading vacuum chamber Lc of the atmospheric atmosphere, and the load-carrying/unloading vacuum chamber Lc is evacuated and evacuated. In addition, before the substrate Sw is loaded into the loading and unloading vacuum chamber Lc, the transport vacuum chamber Tc and the respective film-forming vacuum chambers Pc1, Pc2, and Pc3 are evacuated to a predetermined pressure (1×10 -3 Pa), and becomes the standby state. When the substrate Sw is set on the
其次,當各氣體分壓分別成為特定值以下時,於被真空排氣的成膜真空室Pc1內,以其全壓維持在0.2Pa~0.5Pa之範圍內的方式導入氬氣,由濺鍍電源Ps對靶2投入具有負的電位之直流電力20kW~30kW。然後,於成膜真空室Pc1內形成電漿。在電漿中藉由電離的氬氣的離子濺射靶2。藉此,使由靶2飛散的濺射粒子附著、堆積於基材Sw的成膜面(聚醯亞胺膜Pf),並於基材Sw上以3nm/sec~5nm/sec的成膜速度成膜第1鈦層L1(在第1步驟的成膜步驟)。此時,適當設定濺鍍時間,將第1鈦層L1形成例如10nm~50nm的膜厚。Next, when the partial pressures of the respective gases become equal to or less than a specific value, argon gas is introduced into the evacuated film-forming vacuum chamber Pc1 so that the total pressure thereof is maintained in the range of 0.2Pa to 0.5Pa, and sputtering is performed by sputtering. The power supply Ps supplies 20 kW to 30 kW of DC power having a negative potential to the
第1步驟結束後,將基材Sw搬送至成膜真空室Pc2,與第1步驟同樣地進行真空排氣步驟。當各氣體分壓分別成為特定值以下時,於被真空排氣的成膜真空室Pc2內,以其全壓維持在0.2Pa~0.5Pa之範圍內的方式導入氬氣,由濺鍍電源Ps對鋁製的靶2投入具有負的電位之直流電力30kW~40kW。然後,於成膜真空室Pc2內形成電漿,使由靶2飛散的濺射粒子附著、堆積於第1鈦層L1的表面,並於第1鈦層L1上以7nm/sec~10nm/sec的成膜速度成膜鋁層L2(在第2步驟的成膜步驟)。此時,適當控制濺鍍時間,將鋁層L2形成例如200nm~800nm的膜厚。After the completion of the first step, the substrate Sw is transferred to the film-forming vacuum chamber Pc2, and a vacuum evacuation step is performed in the same manner as the first step. When the partial pressure of each gas becomes below a specific value, argon gas is introduced into the film-forming vacuum chamber Pc2 evacuated to keep the total pressure in the range of 0.2Pa to 0.5Pa, and the sputtering power supply Ps is used to introduce argon gas. A DC power of 30 kW to 40 kW having a negative potential is supplied to the
第2步驟結束後,將基材Sw搬送至成膜真空室Pc3,與第1步驟同樣地進行真空排氣步驟。當各氣體分壓分別成為特定值以下時,在與第1步驟相同濺鍍條件下,於鋁層L2上以3nm/sec~5nm/sec的成膜速度成膜第2鈦層L3(在第3步驟的成膜步驟)。此時,適當控制濺鍍時間,將第2鈦層L3形成與第1鈦層L1同樣的膜厚(例如10~50nm)。After the second step is completed, the substrate Sw is transferred to the film-forming vacuum chamber Pc3, and the vacuum evacuation step is performed in the same manner as in the first step. When the partial pressures of the respective gases are equal to or less than a specific value, the second titanium layer L3 (in the first step) is formed on the aluminum layer L2 at a film deposition rate of 3 nm/sec to 5 nm/sec under the same sputtering conditions as in the first step. 3-step film-forming step). At this time, the sputtering time is appropriately controlled, and the second titanium layer L3 is formed to have the same film thickness (for example, 10 to 50 nm) as the first titanium layer L1.
如以上說明的方式製造層積構造體LS的話,可達成抑制不純物被帶入各鈦層L1,L3內部,並抑制於結晶粒界Cf形成氮化鈦或氧化鈦等鈦化合物(參照圖1中以單點虛線包圍的部分)。此外,藉著以3nm/sec~5nm/sec之範圍內的成膜速度成膜各鈦層L1,L3,使結晶粒Cg的粒徑與從前的例子相比要大,而且這些結晶粒Cg在其膜厚方向上不規則重疊,結果,可以具有結晶粒界Cf在膜厚方向上不連接的結晶構造(參照圖1)。又,測定這樣的鈦層L1,L3之X線繞射時,確認在(002)面之繞射峰與在(100)面之繞射峰,在(100)面之繞射峰對在(002)面之繞射峰的強度比為0.20以上。此時,在(002)面的繞射峰的半峰全幅值為1.0deg以下,在(100)面的繞射峰的半峰全幅值為0.6deg以下。When the laminated structure LS is produced as described above, it is possible to suppress the introduction of impurities into the respective titanium layers L1 and L3 and to suppress the formation of titanium compounds such as titanium nitride or titanium oxide in the grain boundaries Cf (see FIG. 1 ). part surrounded by a single-dotted line). In addition, by forming the respective titanium layers L1 and L3 at a film forming rate in the range of 3 nm/sec to 5 nm/sec, the grain size of the crystal grains Cg is made larger than that in the previous example, and these crystal grains Cg are in the These are irregularly overlapped in the film thickness direction, and as a result, it is possible to have a crystal structure in which the crystal grain boundaries Cf are not connected in the film thickness direction (see FIG. 1 ). In addition, when the X-ray diffraction of such titanium layers L1 and L3 was measured, it was confirmed that the diffraction peak on the (002) plane and the diffraction peak on the (100) plane, and the diffraction peak on the (100) plane was opposite to ( The intensity ratio of the diffraction peak of the 002) plane is 0.20 or more. At this time, the full width at half maximum of the diffraction peak on the (002) plane is 1.0 degrees or less, and the full width at half maximum of the diffraction peak on the (100) plane is 0.6 degrees or less.
其次,為了確認前述效果,使用前述濺鍍裝置Sm,並進行下列實驗。Next, in order to confirm the aforementioned effects, the following experiments were performed using the aforementioned sputtering apparatus Sm.
在發明實驗中,基材Sw是在玻璃基板Sg上面黏貼聚醯亞胺膜Pf,在基材Sw被設置於成膜真空室Pc1的載物台4上後,進行真空排氣直到達到利用質量分析計5測定的氮氣分壓1.0×10
-4Pa、氧氣分壓8.0×10
-5Pa、水蒸氣分壓5.0×10
-4Pa、氫氣分壓5.0×10
-5Pa為止(第1步驟的真空排氣步驟)。此時,真空室Pc1內的全壓係7.3×10
-4Pa。真空排氣步驟之後,以真空室Pc1內的全壓維持在0.3Pa的方式將氬氣以流量120sccm導入真空室Pc1內,與此同時對靶2投入20~30kW直流電力並濺鍍鈦製靶2,以3nm/sec的成膜速度於基材Sw表面成膜50nm膜厚的第1鈦層L1(第1步驟的成膜步驟)。將成膜的第1鈦層L1的X線繞射之測定結果以實線顯示於圖4。也參照表1,分別確認了於繞射角(2θ)38~39°附近在(002)面的繞射峰、於繞射角35~36°附近在(100)面的繞射峰,在(100)面的繞射峰對在(002)面的繞射峰之強度比為0.25,在(002)面的繞射峰的半峰全幅值為0.5deg、在(100)面的繞射峰的半峰全幅值為0.6deg。第1步驟之後,將基材Sw搬送至成膜真空室Pc2,與第1步驟同樣地進行了真空排氣步驟之後,以成膜真空室Pc2的全壓維持在0.3Pa的方式將氬氣以流量120sccm導入成膜真空室Pc2內,與此同時對鋁製的靶2投入35~40kW直流電力並濺鍍靶2,以7nm/sec的成膜速度於第1鈦層L1上成膜500nm膜厚的鋁層L2。測定成膜的鋁層L2的X線繞射之後,確認於繞射角(2θ)38~39°附近在(111)面的繞射峰。第2步驟之後,將基材Sw搬送至成膜真空室Pc3,與第1步驟同樣地進行真空排氣步驟,然後,在與第1步驟相同成膜條件下,以3nm/sec的成膜速度於鋁層L2上成膜50nm膜厚的第2鈦層L3,藉此,獲得層積構造體LS。測定成膜的第2鈦層L3的X線繞射之後,獲得與第1鈦層L1同樣的繞射圖案(參照圖4)。接著,為了確認如此作法獲得的層積構造體LS的耐屈曲性,於玻璃基板Sg上形成具有公知的形狀(寬幅5mm、長度20mm、厚度0.02mm)之試驗基材(聚醯亞胺膜Pf),於試驗基材表面以前述的濺鍍條件依序層積第1鈦層L1、鋁層L2、第2鈦層L3之後,對於在玻璃基板Sg與聚醯亞胺膜Pf的邊界面剝離獲得的層積構造體LS,使用拉伸試驗機(ORIENTEC製造的「STA-1150」)實施拉伸試驗(拉伸速度0.5mm/min)之後,確認了即使施加5%、10%之伸長量所必要的拉伸荷重,層積構造體的伸長量也被抑制在10%以內(5%、8%)。此外,使用電阻測定器(ADVANTEST製造的「AD7461A」)分別測定施加5%、10%之伸長量的拉伸荷重時的電阻R,求出相對於沒有施加拉伸荷重時的電阻R0之電阻上升率(=(R-R0)/R0)之後,確認可以抑制在10%以內(5%、8%)。此外,使用市售的Microscope觀察拉伸試驗後的層積構造體LS的表面狀態時,確認了沒有發生龜裂。由這些結果可知,在本發明實驗獲得之層積構造體LS,與從前的例子相比具有強的耐屈曲性。
In the invention experiment, the base material Sw is to stick the polyimide film Pf on the glass substrate Sg, and after the base material Sw is set on the
其次,為了與前述發明實驗進行比較,進行下列的比較實驗。在比較實驗1,除了將第1及第3各步驟的成膜步驟之成膜真空室Pc1內的全壓維持於0.6Pa並設定成膜速度2nm/sec之點以外,以與前述發明實驗同樣的方法獲得層積構造體LS。在與前述發明實驗同樣的條件下實施拉伸試驗時,確認了層積構造體LS的伸長量為2倍以上。此外,與前述發明實驗同樣地求出電阻上升率時,為30%、400%。此外,與前述發明實驗同樣地觀察拉伸試驗後之層積構造體LS的表面狀態時,確認了發生龜裂並白色化。由這些結果可知,在本比較實驗1獲得之層積構造體LS,具有弱的耐屈曲性。又,測定在本比較實驗1被成膜的第1鈦層L1之X線繞射時,如圖4以虛線所示,並未看到在(100)面之繞射峰,僅確認在(002)面之繞射峰,其在(002)面之繞射峰的半峰全幅值為0.9deg。具有這樣的繞射圖案之場合,如圖5(a)所示,推測比較小的結晶粒Cg排列於膜厚方向而具有以結晶粒界Cf在其膜厚方向延伸的方式連接之結晶構造。Next, in order to compare with the aforementioned inventive experiments, the following comparative experiments were conducted. In Comparative Experiment 1, the same procedure as in the above-mentioned invention experiment was performed except that the total pressure in the film-forming vacuum chamber Pc1 in the film-forming steps of the first and third steps was maintained at 0.6 Pa and the film-forming speed was set to 2 nm/sec. method to obtain the layered structure LS. When the tensile test was carried out under the same conditions as in the above-mentioned invention experiment, it was confirmed that the amount of elongation of the laminated structure LS was 2 times or more. Moreover, when the resistance increase rate was calculated|required similarly to the said invention experiment, it was 30% and 400%. In addition, when the surface state of the laminated structure LS after the tensile test was observed in the same manner as in the above-described invention experiment, it was confirmed that cracks were generated and whitened. From these results, it was found that the laminated structure LS obtained in this comparative experiment 1 had weak buckling resistance. In addition, when measuring the X-ray diffraction of the first titanium layer L1 formed in this comparative experiment 1, as shown by the dotted line in FIG. The diffraction peak of the 002) plane, the full amplitude at half maximum of the diffraction peak of the (002) plane is 0.9deg. With such a diffraction pattern, as shown in FIG. 5( a ), it is presumed that relatively small crystal grains Cg are arranged in the film thickness direction and have a crystal structure connected so that the crystal grain boundaries Cf extend in the film thickness direction.
此外,在比較實驗2,除了於第1及第3各步驟不進行真空排氣步驟之點(僅進行成膜步驟之點)以外,以與前述發明實驗同樣的方法獲得層積構造體LS。亦即,當真空室Pc1內的全壓達到特定真空度(2.8×10
-3Pa)時,不管不純物氣體的分壓如何,都將稀有氣體導入真空室Pc1內。在測定此時的不純物氣體的分壓時,氮氣分壓5.0×
10
-4Pa、氧氣分壓2.0×10
-4Pa、水蒸氣分壓2.0×10
-3Pa、氫氣分壓5.0×10
-5Pa,除氫氣外,均低於基準值。在與前述發明實驗同樣的條件下實施拉伸試驗時,確認了層積構造體LS的伸長量為2倍以上。此外,與前述發明實驗同樣地求出電阻上升率時,是比比較實驗1還更差的120%、650%。此外,與前述發明實驗同樣地觀察拉伸試驗後之層積構造體LS的表面狀態時,確認了發生龜裂並白色化。由這些結果可知,在本比較實驗2獲得之層積構造體LS,具有弱的耐屈曲性。又,測定成膜的第1鈦層L1之X線繞射時,雖然不僅觀察到在(002)面之繞射峰還觀察到在(100)面之繞射峰,在(100)面之繞射峰對在(002)面之繞射峰的強度比卻是比0.20更小的0.11。此外,在(100)面的繞射峰之半峰全幅值是比0.6deg還大的0.7deg。具有這樣的繞射圖案的場合,如圖5(b)所示,推測於結晶粒界Cf形成氮化鈦或氧化鈦等鈦化合物Im。
Further, in
此外,在比較實驗3,除了將第1及第3各步驟之成膜時的成膜真空室Pc1,Pc3內的全壓維持於0.6Pa並設定成膜速度2nm/sec,且於第1及第3各步驟不進行真空排氣步驟之點(僅進行成膜步驟之點)以外,以與前述發明實驗同樣的方法獲得層積構造體LS。在與前述發明實驗同樣的條件下實施拉伸試驗時,確認了層積構造體LS的伸長量為2倍以上。此外,與前述發明實驗同樣地求出電阻上升率時,是比比較實驗2還更差的300%、900%。此外,與前述發明實驗同樣地觀察拉伸試驗後之層積構造體LS的表面狀態時,確認了發生龜裂並白色化。由這些結果可知,在本比較實驗3獲得之層積構造體LS,具有比前述比較實驗1,2還弱的耐屈曲性。又,測定在本比較實驗3被成膜的第1鈦層L1之X線繞射時,並未看到在(100)面之繞射峰,僅確認在(002)面之繞射峰,其在(002)面之繞射峰的半峰全幅值為0.8deg。具有這樣的繞射圖案之場合,如圖5(c)所示,推測比較小的結晶粒Cg排列於膜厚方向而具有以結晶粒界Cf在其膜厚方向延伸的方式連接之結晶構造,而且,於其結晶粒界Cf形成鈦化合物Im。In addition, in
以上說明了本發明之實施型態,但在不逸脫本發明的技術思想的範圍可以進行種種變形。在前述實施型態,作為層積構造體LS以層積第1鈦層L1、鋁層L2、第2鈦層L3為例加以說明,但對於在第2鈦層L3之上進而層積氮化鈦層者也可適用本發明。The embodiment of the present invention has been described above, but various modifications can be made without departing from the technical idea of the present invention. In the above-mentioned embodiment, as the laminated structure LS, the first titanium layer L1, the aluminum layer L2, and the second titanium layer L3 are laminated as an example. Titanium layers are also applicable to the present invention.
此外,在前述實施型態,以在成膜真空室Pc1,Pc2,Pc3之間以原地(in-situ)搬送基材Sw,並在真空氛圍中一貫地成膜第1鈦層L1、鋁層L2、第2鈦層L3之場合為例加以說明,但並不以此為限,本發明也可以適用於以不同的濺鍍裝置實施第1及第2鈦層L1,L3與鋁層L2之場合。此外,亦可在同一成膜真空室成膜第1鈦層L1與第2鈦層L3。In addition, in the aforementioned embodiment, the substrate Sw is transferred in-situ between the film-forming vacuum chambers Pc1, Pc2, and Pc3, and the first titanium layer L1, aluminum The case of the layer L2 and the second titanium layer L3 is described as an example, but it is not limited to this. The present invention can also be applied to the first and second titanium layers L1 and L3 and the aluminum layer L2 using different sputtering apparatuses. occasion. In addition, the first titanium layer L1 and the second titanium layer L3 may be formed in the same film formation vacuum chamber.
LS:層積構造體 L1:第1鈦層 L2:鋁層 L3:第2鈦層 Sw:基材 Pc1,Pc2,Pc3:成膜真空室(真空室) 2:靶 LS: Layered Structure L1: 1st titanium layer L2: Aluminum layer L3: 2nd Titanium Layer Sw: substrate Pc1, Pc2, Pc3: Film-forming vacuum chamber (vacuum chamber) 2: target
[圖1]係模式地說明本發明之實施型態之層積構造體之圖。 [圖2]係模式地說明實施本發明之實施型態之層積構造體的製造方法之濺鍍裝置之圖。 [圖3]係模式地說明圖2所示的成膜真空室Pc1之圖。 [圖4]係顯示確認本發明的效果的實驗結果之圖。 [圖5(a)~(c)]係模式地說明在比較實驗1~比較實驗3成膜的鈦層的結晶構造之圖。 Fig. 1 is a diagram schematically illustrating a laminated structure of an embodiment of the present invention. It is a figure explaining the sputtering apparatus which carried out the manufacturing method of the laminated structure which concerns on embodiment of this invention typically. [ Fig. 3] Fig. 3 is a diagram schematically illustrating the deposition vacuum chamber Pc1 shown in Fig. 2 . [ Fig. 4] Fig. 4 is a diagram showing the results of experiments confirming the effects of the present invention. 5( a ) to ( c ) are diagrams schematically illustrating the crystal structures of the titanium layers formed in Comparative Experiments 1 to 3. FIG.
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