TWI615494B - Closed high energy magnetron sputtering device for coating optical hard film and manufacturing method thereof - Google Patents

Closed high energy magnetron sputtering device for coating optical hard film and manufacturing method thereof Download PDF

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TWI615494B
TWI615494B TW105121174A TW105121174A TWI615494B TW I615494 B TWI615494 B TW I615494B TW 105121174 A TW105121174 A TW 105121174A TW 105121174 A TW105121174 A TW 105121174A TW I615494 B TWI615494 B TW I615494B
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magnetron sputtering
hard film
coating
closed
optical
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TW105121174A
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TW201802277A (en
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Bo-Hui Liao
Jian-Nan Xiao
Ming-Hua Xiao
Sheng-Hui Chen
ri-kai Chen
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鍍製光學硬膜之封閉式高能磁控濺鍍裝置及其製造方法 Closed high energy magnetron sputtering device for coating optical hard film and manufacturing method thereof

本發明係有關於一種鍍製光學硬膜之封閉式高能磁控濺鍍裝置及其製造方法，尤指涉及一種光學產業，特別係指鍍製無光學吸收之透明硬膜者。 The invention relates to a closed high energy magnetron sputtering device for coating an optical hard film and a manufacturing method thereof, in particular to an optical industry, in particular to a transparent hard film without optical absorption.

目前薄膜技術已經廣泛應用於半導體、機械、民生、光電、能源、環保、生醫及奈米科技等產業，為了提供元件所需之特性如抗刮損、抗磨耗、耐腐蝕、抗氧化、提昇表面硬度、增添新色彩等優越性能，同時降低成本與提升產率，奈米尺度之硬質薄膜在現今之科技業越顯得重要。以往在奈米硬質薄膜之研究及應用中(如美國專利第2009173622、8,540,786號與中華民國專利第201315830號)，多以過渡金屬之氮化物及碳化物為首選，以超高硬度、提昇表面硬度、耐腐蝕及增進抗磨耗與抗氧化作為取向，然而考量到不同應用需求，如蓬勃發展之光學產業，光學薄膜製程技術一直是光學產業中不可忽略重要基礎技術，而且品質要求也越來越高，例如液晶螢幕、高密度光碟、數位相機光學系統、投影技術、光纖通訊、微影技術及發光二極體等等皆大量需要光學薄膜製程技術，其中氟化物具有較寬之能帶，光可直接通過而不被吸收，因此係非常重要之光學材料。 At present, thin film technology has been widely used in semiconductor, machinery, people's livelihood, optoelectronics, energy, environmental protection, biomedical and nanotechnology industries, in order to provide the required characteristics of components such as scratch resistance, abrasion resistance, corrosion resistance, oxidation resistance, and enhancement. The superior properties of surface hardness and new color, while reducing costs and increasing productivity, make nanometer-scale hard films more important in today's technology industry. In the past, in the research and application of nano-hard films (such as US Patent Nos. 2009173622, 8,540,786 and Republic of China Patent No. 201315830), nitrides and carbides of transition metals are preferred, with ultra-high hardness and surface hardness. Corrosion resistance and anti-wear and anti-oxidation as the orientation, however, considering the different application requirements, such as the booming optical industry, optical film process technology has always been an important basic technology in the optical industry, and the quality requirements are also higher. For example, liquid crystal screens, high-density optical discs, digital camera optical systems, projection technology, optical fiber communication, lithography, and light-emitting diodes all require optical film processing technology, in which fluoride has a wide band of energy, light can be Directly through without being absorbed, it is a very important optical material.

傳統上氟化物之鍍法可分為熱蒸鍍與濺鍍，且這兩種鍍膜方法之起始材料通常係昂貴之氟化物，熱蒸鍍所鍍出之膜雖有較小之光學吸收，但由於蒸鍍堆積密度低，因此對於環境影響明顯較差且機械性質普遍 不好；若製程改以濺鍍，雖成膜能量較高，可以增加堆積密度，但對於光學吸收卻大幅度增加。有些研究表示在製程中添加氟氣可有效的改善膜質之吸收，但由於深具危險因此不予推崇，除此之外若以金屬為靶材進行反應濺鍍時，通入反應性氣體會毒化靶材造成電漿不穩、鍍率變慢，或反應不完全造成薄膜吸收等缺點。因此，實有必要發展一種可用於光學產業之無光學吸收之透明硬膜。故，一般習用者係無法符合使用者於實際使用時之所需。 Traditionally, the plating method of fluoride can be divided into thermal evaporation and sputtering, and the starting materials of the two coating methods are usually expensive fluorides, and the films coated by thermal evaporation have small optical absorption. However, due to the low density of vapor deposition, the environmental impact is obviously poor and the mechanical properties are common. Not good; if the process is changed to sputtering, although the film forming energy is higher, the bulk density can be increased, but the optical absorption is greatly increased. Some studies have shown that the addition of fluorine gas in the process can effectively improve the absorption of the film, but it is not respected because of its danger. In addition, if reactive sputtering is carried out with metal as the target, the reactive gas will be poisoned. The target causes the plasma to be unstable, the plating rate to be slow, or the reaction to be incompletely caused by the absorption of the film. Therefore, it is necessary to develop a transparent hard film that can be used in the optical industry without optical absorption. Therefore, the general practitioners cannot meet the needs of the user in actual use.

本發明之主要目的係在於，克服習知技藝所遭遇之上述問題並提供一種整合可增加鍍膜速率及薄膜反應能力，也可維持電漿之穩定性；以及可降低基材之溫度外，也可提高薄膜緻密度與附著力等二項進步點之封閉式高能磁控濺鍍裝置及其製造方法。 The main object of the present invention is to overcome the above problems encountered in the prior art and to provide an integration which can increase the coating rate and film reaction ability, and also maintain the stability of the plasma; and can reduce the temperature of the substrate, A closed high-energy magnetron sputtering device and a manufacturing method thereof that improve the density and adhesion of a film and the like.

本發明之次要目的係在於，提供一種可改進反應濺鍍化合物薄膜時反應不完全所造成之吸收之具有高機械及光學品質之封閉式高能磁控濺鍍裝置及其製造方法。 A secondary object of the present invention is to provide a closed-type high-energy magnetron sputtering apparatus and a method of manufacturing the same, which have high mechanical and optical qualities, which can improve the absorption caused by incomplete reaction in the reaction of sputtering a compound film.

本發明之另一目的係在於，提供一種鍍製之光學硬膜可引進光學薄膜理論設計多層膜濾光片使觸控螢幕擁有高硬度及高可見光穿透率之封閉式高能磁控濺鍍裝置及其製造方法。 Another object of the present invention is to provide a closed optical high-energy magnetron sputtering device with a high hardness and high visible light transmittance of a touch screen. And its manufacturing method.

為達以上之目的，本發明係一種鍍製光學硬膜之封閉式高能磁控濺鍍裝置及其製造方法，該封閉式高能磁控濺鍍裝置係包括：一真空腔體，其內設置有一基材固定座(substrate holder)，該基材固定座上設置有一基材；一封閉式電漿系統，係包含至少兩組以上設置於該真空腔體內之濺鍍槍，該些濺鍍槍分別裝設有高純度之金屬靶材(target)，該些金屬靶材分別對應該基材，其中，每一金屬靶材表面設有數個以 不平行磁極排列之磁性元件以形成非平衡磁控濺鍍槍，而該金屬靶材係以廉價之高純度金屬作為起始材料，且為鈦(Ti)、鋁(Al)、鉭(Ta)、鋯(Zr)、鈮(Nb)、鉿(Hf)、鉻(Cr)、鋅(Zn)、錫(Sn)、矽(Si)金屬或其組合；以及一高功率脈衝電漿源系統，其與該真空腔體連接，係包含一氣體供應器及一脈衝控制器，由該氣體供應器通入氧氣或氮氣或氮氧不同比例之氣體至該真空腔體，於室溫或低於600℃溫度下，經由該脈衝控制器調整鍍膜參數，提供高功率密度脈衝電源於該金屬靶材，對沉積中之薄膜進行離子轟擊，俾以製鍍高透光性、高硬度且厚度

Figure TWI615494BD00001
10μm之透明硬膜，其中該製鍍出之硬膜消光係數小於1×10-3且硬度大於莫氏硬度9(13Gpa)。 For the purpose of the above, the present invention is a closed high energy magnetron sputtering apparatus for coating an optical hard film, and a manufacturing method thereof, the closed high energy magnetron sputtering apparatus comprising: a vacuum chamber, which is provided with a vacuum chamber a substrate holder having a substrate disposed on the substrate holder; a closed plasma system comprising at least two sets of sputtering guns disposed in the vacuum chamber, the sputtering guns respectively A high-purity metal target is disposed, and the metal targets respectively correspond to the substrate, wherein each metal target surface is provided with a plurality of magnetic elements arranged in non-parallel magnetic poles to form an unbalanced magnetron splash A gun is sprayed, and the metal target is made of an inexpensive high-purity metal, and is titanium (Ti), aluminum (Al), tantalum (Ta), zirconium (Zr), niobium (Nb), niobium (Hf). a chromium (Cr), zinc (Zn), tin (Sn), bismuth (Si) metal or a combination thereof; and a high power pulsed plasma source system coupled to the vacuum chamber, comprising a gas supply And a pulse controller, the gas supply device is supplied with oxygen or nitrogen or nitrogen and oxygen in different proportions to the true The chamber adjusts the coating parameters through the pulse controller at room temperature or below 600 ° C, provides a high power density pulse power source to the metal target, and ion bombards the deposited film, and the plating is highly transparent. Light, high hardness and thickness
Figure TWI615494BD00001
A 10 μm transparent hard film in which the hard film extinction coefficient is less than 1 × 10 -3 and the hardness is greater than Mohs hardness of 9 (13 GPa).

於本發明上述實施例中，該磁性元件之磁力線係向外延伸至該基材之封閉曲線。 In the above embodiment of the invention, the magnetic lines of force of the magnetic element extend outwardly to the closed curve of the substrate.

於本發明上述實施例中，該高功率脈衝電漿源系統係用一直流電源(DC power)、一射頻(Radio Frequency,RF)與一高功率脈衝磁控濺鍍源(High Power Impulse Magnetron Sputtering,HIPIMS)，或一中頻(Medium Frequency,MF)與一高功率脈衝磁控濺鍍源搭配組合，以提供高功率密度脈衝電源至該金屬靶材。 In the above embodiment of the present invention, the high power pulse plasma source system uses a DC power, a Radio Frequency (RF), and a High Power Impulse Magnetron Sputtering. , HIPIMS), or a medium frequency (MF) combined with a high power pulsed magnetron sputtering source to provide a high power density pulsed power supply to the metal target.

於本發明上述實施例中，該脈衝控制器調整之鍍膜參數，係包含調控脈衝電源之中斷時間(off time)佔工作週率(duty cycle)範圍為低於10%及脈衝頻率範圍為低於10kHz。 In the above embodiment of the present invention, the pulse controller adjusts the coating parameter, wherein the off time of the regulated pulse power source accounts for less than 10% of the duty cycle range and the pulse frequency range is lower than the pulse frequency range. 10kHz.

於本發明上述實施例中，該基材背面係設置有一加熱源，該加熱源係設置於該真空腔體內，從該基材背面提供加熱並控制其在所需溫度範圍。 In the above embodiment of the present invention, a heat source is disposed on the back surface of the substrate, and the heat source is disposed in the vacuum chamber to provide heating from the back surface of the substrate and to control it in a desired temperature range.

於本發明上述實施例中，該加熱源係為鹵素燈管或電阻式加熱器。 In the above embodiment of the invention, the heating source is a halogen lamp or a resistance heater.

於本發明上述實施例中，該透明硬膜係為氮化矽(Si3N4)、氮氧化矽(Si3-2xO2xN4(1-x)(0

Figure TWI615494BD00002
X
Figure TWI615494BD00003
1))、氮化鋁(AlN)、氮氧化鋁(Al3-xO3xN3(1-x)(0
Figure TWI615494BD00004
X
Figure TWI615494BD00005
1))、氮化矽鋁(AlSiN)、氮氧化矽鋁(AlSiON)、氧化矽(SiO2)、氧化鈦(TiO2)、氧化鋯(ZrO2)、氧化鋁(Al2O3)、或氧化鉭(Ta2O5)。 In the above embodiment of the invention, the transparent hard film is tantalum nitride (Si 3 N 4 ), yttrium oxynitride (Si 3-2 x O 2 x N 4 (1-x) (0
Figure TWI615494BD00002
X
Figure TWI615494BD00003
1)), aluminum nitride (AlN), aluminum oxynitride (Al 3-x O 3x N 3(1-x) (0
Figure TWI615494BD00004
X
Figure TWI615494BD00005
1)), lanthanum aluminum nitride (AlSiN), lanthanum aluminum oxynitride (AlSiON), yttrium oxide (SiO 2 ), titanium oxide (TiO 2 ), zirconium oxide (ZrO 2 ), aluminum oxide (Al 2 O 3 ), Or yttrium oxide (Ta 2 O 5 ).

於本發明上述實施例中，該透明硬膜可進一步應用光學薄膜理論製鍍為抗反射膜、帶通濾光片、截止濾光片、窄帶濾光片、或高反射鏡。於本發明上述實施例中，該封閉式電漿系統係在該些金屬靶材周圍設置氣體阻隔板，以將濺鍍區域與反應區域作隔離。 In the above embodiment of the present invention, the transparent hard film may be further plated into an anti-reflection film, a band pass filter, a cut filter, a narrow band filter, or a high reflection mirror by optical film theory. In the above embodiment of the present invention, the closed plasma system is provided with a gas barrier plate around the metal targets to isolate the sputtering region from the reaction region.

1‧‧‧真空腔體 1‧‧‧vacuum chamber

11‧‧‧基材固定座 11‧‧‧Substrate mount

12‧‧‧加熱源 12‧‧‧heat source

2‧‧‧封閉式電漿系統 2‧‧‧Closed plasma system

21‧‧‧濺鍍槍 21‧‧‧Spray gun

22‧‧‧金屬靶材 22‧‧‧Metal target

23‧‧‧磁性元件 23‧‧‧ Magnetic components

24‧‧‧氣體阻隔板 24‧‧‧ gas barrier

3‧‧‧高功率脈衝電漿源系統 3‧‧‧High Power Pulse Plasma Source System

31‧‧‧氣體供應器 31‧‧‧ gas supply

32‧‧‧脈衝控制器 32‧‧‧pulse controller

33‧‧‧直流電源 33‧‧‧DC power supply

34‧‧‧射頻 34‧‧‧RF

35‧‧‧高功率脈衝磁控濺鍍源 35‧‧‧High power pulsed magnetron sputtering source

4‧‧‧基材 4‧‧‧Substrate

5‧‧‧質量監控器 5‧‧‧Quality monitor

第1圖，係本發明之非平衡磁力線示意圖。 Figure 1 is a schematic view of the unbalanced magnetic lines of force of the present invention.

第2圖，係本發明之濺鍍區域與反應區域隔離示意圖。 Fig. 2 is a schematic view showing the isolation of the sputtering region and the reaction region of the present invention.

第3圖，係本發明之封閉式高能磁控濺鍍裝置示意圖。 Figure 3 is a schematic view of the enclosed high energy magnetron sputtering apparatus of the present invention.

第4圖，係本發明之高功率脈衝電漿源系統之脈衝電源配置示意圖。 Fig. 4 is a schematic diagram showing the configuration of a pulse power supply of the high power pulse plasma source system of the present invention.

第5圖，係本發明之穿透率測試圖。 Figure 5 is a graph of the transmittance test of the present invention.

第6圖，係本發明之硬度測試圖。 Figure 6 is a hardness test chart of the present invention.

第7圖，係本發明之多層抗反射膜穿透率測試圖。 Fig. 7 is a graph showing the transmittance of the multilayer antireflection film of the present invention.

請參閱『第1圖~第7圖』所示，係分別為本發明之非平衡磁力線示意圖、本發明之濺鍍區域與反應區域隔離示意圖、本發明之封閉式高能磁控濺鍍裝置示意圖、本發明之高功率脈衝電漿源系統之脈衝電源配置示意圖、本發明之穿透率測試圖、本發明之硬度測試圖、及本發明之多層抗反射膜穿透率測試圖。如圖所示：本發明係一種鍍製光學 硬膜之封閉式高能磁控濺鍍裝置及其製造方法，該封閉式高能磁控濺鍍裝置係用來鍍製光學硬膜，其包括一真空腔體1、一封閉式電漿系統2、以及一高功率脈衝電漿源系統3所構成。 Please refer to FIG. 1 to FIG. 7 , which are schematic diagrams of the unbalanced magnetic lines of force of the present invention, the isolation of the sputtering region and the reaction region of the present invention, and the schematic diagram of the closed high energy magnetron sputtering device of the present invention. A schematic diagram of a pulse power supply configuration of the high power pulsed plasma source system of the present invention, a transmittance test chart of the present invention, a hardness test chart of the present invention, and a multilayer antireflection film transmittance test chart of the present invention. As shown: the invention is a plating optics A hard-film closed high-energy magnetron sputtering device for manufacturing an optical hard film comprising a vacuum chamber 1 and a closed plasma system 2 And a high power pulse plasma source system 3 is constructed.

上述所提之真空腔體1內設置有一基材固定座(substrate holder)11，該基材固定座11上設置有一基材4，該基材4背面更設置有一加熱源12，該加熱源12係設置於該真空腔體1內，從該基材4背面提供加熱並控制其在所需溫度範圍，其中，該加熱源12係為鹵素燈管或電阻式加熱器。 A substrate holder 11 is disposed in the vacuum chamber 1 , and a substrate 4 is disposed on the substrate holder 11 , and a heating source 12 is further disposed on the back surface of the substrate 4 . It is disposed in the vacuum chamber 1 to provide heating from the back surface of the substrate 4 and to control it in a desired temperature range, wherein the heating source 12 is a halogen tube or a resistance heater.

該封閉式電漿系統2包含至少兩組以上設置於該真空腔體1內之濺鍍槍21，該些濺鍍槍21分別裝設有高純度之金屬靶材(target)22，該些金屬靶材22分別對應該基材4，其中，每一金屬靶材22表面設有數個以不平行磁極排列之磁性元件23以形成非平衡磁控濺鍍槍。 The closed plasma system 2 includes at least two sets of sputter guns 21 disposed in the vacuum chamber 1 , and the sputter guns 21 are respectively provided with high-purity metal targets 22 , the metals The targets 22 respectively correspond to the substrate 4, wherein each of the surfaces of the metal targets 22 is provided with a plurality of magnetic elements 23 arranged in non-parallel magnetic poles to form an unbalanced magnetron sputtering gun.

該高功率脈衝電漿源系統3係與該真空腔體1連接，係包含一氣體供應器31及一脈衝控制器32，並使用一直流電源(DC power)33、一射頻(Radio Frequency,RF)34與一高功率脈衝磁控濺鍍源(High Power Impulse Magnetron Sputtering,HIPIMS)35(如第3圖所示)，或一直流電源33、一中頻(Medium Frequency,MF)與一高功率脈衝磁控濺鍍源35搭配組合作為濺鍍電源，以提供高功率密度脈衝至該金屬靶材22。如是，藉由上述揭露之流程構成一全新之封閉式高能磁控濺鍍裝置。 The high-power pulse plasma source system 3 is connected to the vacuum chamber 1 and includes a gas supplier 31 and a pulse controller 32, and uses a DC power source 33 and a radio frequency (Radio Frequency, RF). 34 and a High Power Impulse Magnetron Sputtering (HIPIMS) 35 (as shown in Figure 3), or a DC power supply 33, a Medium Frequency (MF) and a high power The pulsed magnetron sputtering source 35 is combined as a sputtering power supply to provide high power density pulses to the metal target 22. If so, a new closed high-energy magnetron sputtering device is constructed by the above disclosed process.

上述裝置更包括一質量監控器5連接於該真空腔體1內，靠近被濺鍍之基材4。該質量監控器5如一石英晶體微量天平(Quartz Crystal Microbalance,QCM)可被用於測量基材上濺鍍薄膜之品質。 The apparatus further includes a mass monitor 5 coupled to the vacuum chamber 1 adjacent to the substrate 4 being sputtered. The quality monitor 5, such as a Quartz Crystal Microbalance (QCM), can be used to measure the quality of a sputtered film on a substrate.

上述封閉式電漿系統2中每一濺鍍槍21之磁性元件23(例如磁鐵)皆為非平衡系統，其磁力線可向外延伸，經適當濺鍍槍組合，其磁力線會是向外延伸至該基材之一封閉曲線。如第1圖所示，其可使本裝置產生a、b、c及d四個電漿區，因此基材、濺鍍出之靶材粒子及反應氣體都會在電漿籠罩中，可藉此增加鍍膜速率及薄膜與反應氣體之化合能力，也可維持電漿之穩定性。此外，本裝置亦可如第2圖所示，該封閉式電漿系統2可在該些金屬靶材周圍設置氣體阻隔板24，以將濺鍍區域與反應區域作隔離，使此系統擁有高濺鍍率及高電漿穩定性。 The magnetic elements 23 (e.g., magnets) of each of the sputtering guns 21 in the closed plasma system 2 are unbalanced systems, and the magnetic lines of force can extend outwardly, and the magnetic lines of force are extended outward by a suitable combination of the sputtering guns. One of the substrates closes the curve. As shown in Fig. 1, the device can generate four plasma regions a, b, c and d, so that the substrate, the sputtered target particles and the reaction gas are all in the plasma envelope. Increasing the coating rate and the ability of the film to combine with the reactive gas can also maintain the stability of the plasma. In addition, the device can also be as shown in FIG. 2, the closed plasma system 2 can be provided with a gas barrier baffle 24 around the metal targets to isolate the sputtering region from the reaction region, so that the system has a high Sputter rate and high plasma stability.

上述高功率脈衝電漿源3如第3、4圖所示，此於原本之直流濺鍍系統之直流電源33上加裝脈衝控制器32，在數百微秒內提供高功率密度脈衝電源(kW/cm2)於該金屬靶材22，該基材4上產生之離子電流密度可高出直流磁控濺鍍(direct current magnetron sputtering,dcMS)兩個數量級，藉由該脈衝控制器32調整鍍膜參數，包含調控脈衝電源之中斷時間(off time)，於低工作週率(duty cycle)運作(<10%)及低脈衝頻率(<10kHz)使平均功率密度遠低於峰值功率密度，近似於一般dcMS(~W/cm2)，而電漿密度則提昇至1018/m3以上，相較dcMS之電漿密度(1014~1016/m3)約高出100~10000倍左右，其金屬靶材22之游離率更高達70%以上。藉由此高功率密度脈衝電源對沉積中之薄膜進行離子轟擊，除了可降低基材4之溫度外，也可提高薄膜緻密度與附著力，本裝置非常適合應用於高品質之光學膜及硬膜。 The high-power pulse plasma source 3 is as shown in Figures 3 and 4, and the pulse controller 32 is added to the DC power supply 33 of the original DC sputtering system to provide a high power density pulse power supply in hundreds of microseconds ( kW/cm 2 ) on the metal target 22, the ionic current density generated on the substrate 4 can be two orders of magnitude higher than the direct current magnetron sputtering (dcMS), which is adjusted by the pulse controller 32. Coating parameters, including the off time of the regulated pulse power supply, operating at low duty cycle (<10%) and low pulse frequency (<10kHz) make the average power density much lower than the peak power density, approximate In general dcMS (~W/cm 2 ), the plasma density is increased to above 10 18 /m 3 , which is about 100~10000 times higher than the plasma density of dcMS (10 14 ~ 10 16 /m 3 ). The detachment rate of the metal target 22 is as high as 70% or more. By ion bombardment of the deposited film by the high power density pulse power supply, in addition to lowering the temperature of the substrate 4, the film density and adhesion can be improved, and the device is very suitable for application to high quality optical film and hard. membrane.

本發明整合此封閉式電漿系統2、及高功率脈衝電漿源系統3二種技術，並使用較廉價之高純度金屬作為起始材料，如鈦(Ti)、鋁(Al)、 鉭(Ta)、鋯(Zr)、鈮(Nb)、鉿(Hf)、鉻(Cr)、鋅(Zn)、錫(Sn)、矽(Si)金屬或其組合等，由該氣體供應器31通入氧氣或氮氣或氮氧不同比例之氣體至該真空腔體1，於室溫或低於600℃溫度下，經由該脈衝控制器32調整鍍膜參數，提供高功率密度脈衝電源於該金屬靶材22，對沉積中之薄膜進行離子轟擊，俾以製鍍高透光性、高硬度且厚度

Figure TWI615494BD00006
10μm之透明硬膜，如氮化矽(Si3N4)、氮氧化矽(Si3-2xO2xN4(1-x)(0
Figure TWI615494BD00007
X
Figure TWI615494BD00008
1))、氮化鋁(AlN)、氮氧化鋁(Al3-xO3xN3(1-x)(0
Figure TWI615494BD00009
X
Figure TWI615494BD00010
1))、氮化矽鋁(AlSiN)、氮氧化矽鋁(AlSiON)、氧化矽(SiO2)、氧化鈦(TiO2)、氧化鋯(ZrO2)、氧化鋁(Al2O3)、或氧化鉭(Ta2O5)等，其中該製鍍出之硬膜消光係數小於1×10-3且硬度大於莫氏硬度9(13Gpa)。最後，該可應用光學薄膜理論，製鍍多層膜高透光硬膜，以應用於各種光學元件，如抗反射膜、帶通濾光片、截止濾光片、窄帶濾光片、或高反射鏡等。 The invention integrates the two technologies of the closed plasma system 2 and the high-power pulse plasma source system 3, and uses a relatively inexpensive high-purity metal as a starting material, such as titanium (Ti), aluminum (Al), bismuth ( Ta), zirconium (Zr), niobium (Nb), hafnium (Hf), chromium (Cr), zinc (Zn), tin (Sn), bismuth (Si) metal or a combination thereof, etc., are passed through the gas supply 31 A gas of different proportions of oxygen or nitrogen or nitrogen and oxygen is introduced into the vacuum chamber 1, and the coating parameters are adjusted via the pulse controller 32 at room temperature or below 600 ° C to provide a high power density pulse power source to the metal target. 22, ion bombardment of the film in the deposition, 俾 plating to achieve high light transmission, high hardness and thickness
Figure TWI615494BD00006
10μm transparent hard film , such as tantalum nitride (Si 3 N 4 ), niobium oxynitride (Si 3-2x O 2x N 4(1-x) (0
Figure TWI615494BD00007
X
Figure TWI615494BD00008
1)), aluminum nitride (AlN), aluminum oxynitride (Al 3-x O 3x N 3(1-x) (0
Figure TWI615494BD00009
X
Figure TWI615494BD00010
1)), lanthanum aluminum nitride (AlSiN), lanthanum aluminum oxynitride (AlSiON), yttrium oxide (SiO 2 ), titanium oxide (TiO 2 ), zirconium oxide (ZrO 2 ), aluminum oxide (Al 2 O 3 ), Or yttrium oxide (Ta 2 O 5 ) or the like, wherein the hard film extinction coefficient of the system is less than 1×10 -3 and the hardness is greater than Mohs hardness of 9 (13 GPa). Finally, the optical film theory can be applied to produce a multilayer high-transparent hard film for use in various optical components such as anti-reflection films, band pass filters, cut-off filters, narrow-band filters, or high reflections. Mirror and so on.

本發明藉由整合封閉式非平衡磁控濺鍍系統及高功率脈衝濺鍍技術，除了可降低反應溫度外，也可提高薄膜緻密度與附著力，使此裝置可應用於製鍍高透光性且高硬度之透明硬膜。如第5~7圖及表一所示，經實驗證明此透明硬膜之折射率為所有鍍膜系統製鍍中最高者，且硬度亦為所有鍍膜系統製鍍中最高者，本發明中也藉由摻雜其他元素來提高穿透率，最後引進光學薄膜之理論，製鍍多層膜高透光硬膜，以應用於各種光學元件。 The invention integrates the closed unbalanced magnetron sputtering system and the high-power pulse sputtering technology, in addition to lowering the reaction temperature, the film density and adhesion can also be improved, so that the device can be applied to high transmittance of plating. Sexual and high hardness transparent hard film. As shown in Figures 5-7 and Table 1, it has been experimentally proved that the refractive index of the transparent hard film is the highest among all the plating systems, and the hardness is also the highest among all the plating systems. By doping other elements to improve the transmittance, and finally introducing the theory of optical films, a multi-layer film high-transmission hard film is applied to various optical components.

Figure TWI615494BD00011
Figure TWI615494BD00011

藉此，本發明具有下列兩項進步點： Thereby, the present invention has the following two advancements:

1.本裝置可增加鍍膜速率及薄膜反應能力，也可維持電漿之穩定性。 1. This device can increase the coating rate and film reaction ability, and also maintain the stability of the plasma.

2.本裝置可降低基材之溫度外，也可提高薄膜緻密度與附著力。 2. The device can reduce the temperature of the substrate and increase the density and adhesion of the film.

綜上所述，本發明係一種鍍製光學硬膜之封閉式高能磁控濺鍍裝置及其製造方法，可有效改善習用之種種缺點，透過整合上述二項進步點，使本裝置可改進反應濺鍍化合物薄膜時反應不完全所造成之吸收，本裝置也可增加成膜能量以提高薄膜緻密度，進而提出一具有高機械及光學品質之新型濺鍍裝置及其製造方法，並應用此新型濺鍍技術鍍製透明硬膜材料，最後引進光學薄膜理論設計多層膜濾光片使觸控螢幕 擁有高硬度及高可見光穿透率，進而使本發明之產生能更進步、更實用、更符合使用者之所須，確已符合發明專利申請之要件，爰依法提出專利申請。 In summary, the present invention is a closed high-energy magnetron sputtering device for coating an optical hard film and a manufacturing method thereof, which can effectively improve various disadvantages of the conventional use, and the device can improve the reaction by integrating the above two advance points. The device can also increase the film forming energy to increase the density of the film when the compound film is sputtered. The novel sputtering device with high mechanical and optical quality and its manufacturing method are proposed, and the new type is applied. Sputtering technology to plate transparent hard film materials, and finally introducing optical film theory to design multilayer film filters to make touch screens It has high hardness and high visible light transmittance, which makes the invention more progressive, more practical and more suitable for users. It has indeed met the requirements of the invention patent application and has filed a patent application according to law.

惟以上所述者，僅為本發明之較佳實施例而已，當不能以此限定本發明實施之範圍；故，凡依本發明申請專利範圍及發明說明書內容所作之簡單的等效變化與修飾，皆應仍屬本發明專利涵蓋之範圍內。 However, the above is only the preferred embodiment of the present invention, and the scope of the present invention is not limited thereto; therefore, the simple equivalent changes and modifications made in accordance with the scope of the present invention and the contents of the invention are modified. All should remain within the scope of the invention patent.

1‧‧‧真空腔體 1‧‧‧vacuum chamber

11‧‧‧基材固定座 11‧‧‧Substrate mount

12‧‧‧加熱源 12‧‧‧heat source

2‧‧‧封閉式電漿系統 2‧‧‧Closed plasma system

21‧‧‧濺鍍槍 21‧‧‧Spray gun

22‧‧‧金屬靶材 22‧‧‧Metal target

23‧‧‧磁性元件 23‧‧‧ Magnetic components

3‧‧‧高功率脈衝電漿源系統 3‧‧‧High Power Pulse Plasma Source System

31‧‧‧氣體供應器 31‧‧‧ gas supply

32‧‧‧脈衝控制器 32‧‧‧pulse controller

33‧‧‧直流電源 33‧‧‧DC power supply

34‧‧‧射頻 34‧‧‧RF

35‧‧‧高功率脈衝磁控濺鍍源 35‧‧‧High power pulsed magnetron sputtering source

4‧‧‧基材 4‧‧‧Substrate

5‧‧‧質量監控器 5‧‧‧Quality monitor

Claims (8)

一種鍍製光學硬膜之封閉式高能磁控濺鍍裝置，係包括：一真空腔體，其內設置有一基材固定座(substrate holder)，該基材固定座上設置有一基材；一封閉式電漿系統，係包含至少兩組以上設置於該真空腔體內之濺鍍槍，該些濺鍍槍分別裝設有高純度之金屬靶材(target)，該些金屬靶材分別對應該基材，其中，每一金屬靶材表面設有數個以不平行磁極排列之磁性元件以形成非平衡磁控濺鍍槍，該磁性元件之磁力線係向外延伸至該基材之封閉曲線，而該金屬靶材係以廉價之高純度金屬作為起始材料，且為鈦(Ti)、鋁(Al)、鉭(Ta)、鋯(Zr)、鈮(Nb)、鉿(Hf)、鉻(Cr)、鋅(Zn)、錫(Sn)、矽(Si)金屬或其組合；以及一高功率脈衝電漿源系統，其與該真空腔體連接，係包含一氣體供應器及一脈衝控制器，由該氣體供應器通入氧氣或氮氣或氮氧不同比例之氣體至該真空腔體，於室溫或低於600℃溫度下，經由該脈衝控制器調整鍍膜參數，提供高功率密度脈衝電源於該金屬靶材，對沉積中之薄膜進行離子轟擊，俾以製鍍高透光性、高硬度且厚度10μm之透明硬膜，其中該製鍍出之硬膜消光係數小於1×10-3且硬度大於莫氏硬度9(13Gpa)。 A closed high-energy magnetron sputtering device for coating an optical hard film, comprising: a vacuum chamber, wherein a substrate holder is disposed, the substrate holder is provided with a substrate; The plasma system comprises at least two sets of sputtering guns disposed in the vacuum chamber, and the sputtering guns are respectively provided with high-purity metal targets, and the metal targets respectively correspond to the base a material, wherein each metal target surface is provided with a plurality of magnetic elements arranged in non-parallel magnetic poles to form an unbalanced magnetron sputtering gun, the magnetic lines of force of the magnetic element extending outward to a closed curve of the substrate, and the material The metal target is made of inexpensive high-purity metal, and is titanium (Ti), aluminum (Al), tantalum (Ta), zirconium (Zr), niobium (Nb), hafnium (Hf), chromium (Cr). a zinc (Zn), tin (Sn), bismuth (Si) metal or a combination thereof; and a high power pulsed plasma source system coupled to the vacuum chamber, comprising a gas supply and a pulse controller , the gas supply device is supplied with oxygen or nitrogen or nitrogen and oxygen in different proportions of the gas to the vacuum chamber, in the chamber Or lower than 600 ° C, through the pulse controller to adjust the coating parameters, provide a high power density pulse power supply to the metal target, ion bombardment of the deposited film, 制 plating high transmittance, high hardness and thickness 10μm of a transparent hard film, wherein the dura mater manufactured by plating an extinction coefficient of less than 1 × 10 -3 and a hardness greater than the Mohs hardness 9 (13Gpa). 依申請專利範圍第1項所述之鍍製光學硬膜之封閉式高能磁控濺鍍裝置，其中，該高功率脈衝電漿源系統係用一直流電源(DC power)、一射頻(Radio Frequency,RF)與一高功率脈衝磁控濺鍍源(High Power Impulse Magnetron Sputtering,HIPIMS)，或一 直流電源、一中頻(Medium Frequency,MF)與一高功率脈衝磁控濺鍍源搭配組合，以提供高功率密度脈衝電源至該金屬靶材。 The closed high-energy magnetron sputtering device for coating an optical hard film according to the first aspect of the patent application, wherein the high-power pulse plasma source system uses a DC power source and a radio frequency (Radio Frequency). , RF) and a High Power Impulse Magnetron Sputtering (HIPIMS), or A DC power supply, a Medium Frequency (MF), and a high power pulsed magnetron sputtering source are combined to provide a high power density pulsed power supply to the metal target. 依申請專利範圍第1項所述之鍍製光學硬膜之封閉式高能磁控濺鍍裝置，其中，該脈衝控制器調整之鍍膜參數，係包含調控脈衝電源之中斷時間(off time)佔工作週率(duty cycle)範圍為低於10%及脈衝頻率範圍為低於10kHz。 The closed high-energy magnetron sputtering device for coating an optical hard film according to the first aspect of the patent application, wherein the pulse controller adjusts the coating parameter to include an off-time of the regulated pulse power supply. The duty cycle range is below 10% and the pulse frequency range is below 10 kHz. 依申請專利範圍第1項所述之鍍製光學硬膜之封閉式高能磁控濺鍍裝置，其中，該基材背面係設置有一加熱源，該加熱源係設置於該真空腔體內，從該基材背面提供加熱並控制其在所需溫度範圍。 The closed high-energy magnetron sputtering device of the optical hard film according to the first aspect of the invention, wherein the back surface of the substrate is provided with a heating source, and the heating source is disposed in the vacuum chamber. The back side of the substrate provides heating and controls it over the desired temperature range. 依申請專利範圍第4項所述之鍍製光學硬膜之封閉式高能磁控濺鍍裝置，其中，該加熱源係為鹵素燈管或電阻式加熱器。 A closed high-energy magnetron sputtering apparatus for coating an optical hard film according to claim 4, wherein the heating source is a halogen lamp or a resistance heater. 依申請專利範圍第1項所述之鍍製光學硬膜之封閉式高能磁控濺鍍裝置，其中，該透明硬膜係為氮化矽(Si3N4)、氮氧化矽(Si3-2xO2xN4(1-x)(0X1))、氮化鋁(AlN)、氮氧化鋁(Al3-xO3xN3(1-x)(0X1))、氮化矽鋁(AlSiN)、氮氧化矽鋁(AlSiON)、氧化矽(SiO2)、氧化鈦(TiO2)、氧化鋯(ZrO2)、氧化鋁(Al2O3)、或氧化鉭(Ta2O5)。 A closed high-energy magnetron sputtering device for coating an optical hard film according to claim 1, wherein the transparent hard film is tantalum nitride (Si 3 N 4 ) or bismuth oxynitride (Si 3- 2x O 2x N 4(1-x) (0 X 1)), aluminum nitride (AlN), aluminum oxynitride (Al 3x O 3x N 3 ( 1-x) (0 X 1)), lanthanum aluminum nitride (AlSiN), lanthanum aluminum oxynitride (AlSiON), yttrium oxide (SiO 2 ), titanium oxide (TiO 2 ), zirconium oxide (ZrO 2 ), aluminum oxide (Al 2 O 3 ), Or yttrium oxide (Ta 2 O 5 ). 依申請專利範圍第1項所述之鍍製光學硬膜之封閉式高能磁控濺鍍裝置，其中，該透明硬膜可進一步應用光學薄膜理論製鍍為抗反射膜、帶通濾光片、截止濾光片、窄帶濾光片、或高反射鏡。 The closed high-energy magnetron sputtering device for coating an optical hard film according to the first aspect of the patent application, wherein the transparent hard film can be further coated with an optical film to form an anti-reflection film, a band pass filter, Cut-off filter, narrow band filter, or high mirror. 依申請專利範圍第1項所述之鍍製光學硬膜之封閉式高能磁控濺鍍裝置，其中，該封閉式電漿系統係在該些金屬靶材周圍設置氣體阻隔板，以將濺鍍區域與反應區域作隔離。 A closed high-energy magnetron sputtering device for coating an optical hard film according to claim 1, wherein the closed plasma system is provided with a gas barrier plate around the metal targets for sputtering The area is isolated from the reaction area.
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TWI692538B (en) * 2018-11-27 2020-05-01 財團法人金屬工業研究發展中心 Thin-film manufacturing apparatus with vhf reactive plasma and thin-film deposition method

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US20080135400A1 (en) * 2006-12-12 2008-06-12 Oc Oerlikon Balzers Ag Arc suppression and pulsing in high power impulse magnetron sputtering (hipims)
TW200944606A (en) * 2008-04-03 2009-11-01 Oc Oerlikon Balzers Ag Apparatus for sputtering and a method of fabricating a metallization structure
US20150004432A1 (en) * 2011-10-28 2015-01-01 Korea Institute Of Machinery & Materials Titanium-nickel alloy thin film, and preparation method of titanium-nickel alloy thin film using multiple sputtering method
TW201514329A (en) * 2013-10-01 2015-04-16 Nat Applied Res Laboratories Magnetron sputtering gun device

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
US20080135400A1 (en) * 2006-12-12 2008-06-12 Oc Oerlikon Balzers Ag Arc suppression and pulsing in high power impulse magnetron sputtering (hipims)
TW200944606A (en) * 2008-04-03 2009-11-01 Oc Oerlikon Balzers Ag Apparatus for sputtering and a method of fabricating a metallization structure
US20150004432A1 (en) * 2011-10-28 2015-01-01 Korea Institute Of Machinery & Materials Titanium-nickel alloy thin film, and preparation method of titanium-nickel alloy thin film using multiple sputtering method
TW201514329A (en) * 2013-10-01 2015-04-16 Nat Applied Res Laboratories Magnetron sputtering gun device

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