TW201938829A - Method for manufacturing gallium nitride thin film - Google Patents
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Abstract
Description
本發明係關於氮化鎵薄膜之製造方法，尤其是關於結晶配向性為良好的氮化鎵薄膜之製造方法。The present invention relates to a method for manufacturing a gallium nitride thin film, and more particularly to a method for manufacturing a gallium nitride thin film with good crystal alignment.
現在，氮化鎵薄膜，係被使用於LED或無線通訊用半導體等，為了提昇使用有氮化鎵薄膜之電子元件的特性，而研究開發可得到結晶性佳的薄膜之方法。Currently, gallium nitride thin films are used in LEDs, semiconductors for wireless communications, and the like. In order to improve the characteristics of electronic components using gallium nitride thin films, research and development methods have been developed to obtain thin films with good crystallinity.
於下述專利文獻1中，係記載有以反應性濺鍍方法使氮化鎵薄膜成長的技術，於下述專利文獻2中，係記載有使用有自由基的氮化鎵薄膜之製造方法。又，於下述專利文獻3中，係記載有使用有離子束之反應性濺鍍方法，雖可推測結晶性已有所提昇，但要求有使結晶性進一步提昇的技術。
第7圖，係展示將金屬鎵靶材進行濺鍍來形成氮化鎵薄膜時之氮氣分壓與所形成的薄膜之含氮量的關係之圖表，於區域A之氮氣分壓中，自由基反應係為支配性，所形成的薄膜係為鎵薄膜，於區域B之氮氣分壓中，反應性濺鍍反應係為支配性，所形成的薄膜係為氮化鎵薄膜，但是，配向性係為差。
[先前技術文獻]
[專利文獻]The following Patent Document 1 describes a technique for growing a gallium nitride thin film by a reactive sputtering method, and the following Patent Document 2 describes a manufacturing method of a gallium nitride thin film using a radical. Moreover, in the following patent document 3, the reactive sputtering method using an ion beam is described. Although it is estimated that crystallinity has been improved, a technique for further improving crystallinity is required.
Figure 7 is a graph showing the relationship between the nitrogen partial pressure and the nitrogen content of the formed thin film when a gallium metal target is sputtered to form a gallium nitride thin film. The reaction system is dominant. The formed film is a gallium film. In the nitrogen partial pressure of region B, the reactive sputtering reaction system is dominant and the formed film is a gallium nitride film. However, the alignment system is Is bad.
[Prior technical literature]
[Patent Literature]
[專利文獻1]WO2007/108266
[專利文獻2]日本特開2013-125851號公報
[專利文獻3]日本特開2017-201050號公報[Patent Document 1] WO2007 / 108266
[Patent Document 2] Japanese Patent Laid-Open No. 2013-125851
[Patent Document 3] Japanese Patent Laid-Open No. 2017-201050
[發明所欲解決之課題][Problems to be Solved by the Invention]
本發明係以得到結晶性佳之氮化鎵薄膜作為課題。
[用以解決課題之手段]The present invention is directed to obtaining a gallium nitride thin film having excellent crystallinity.
[Means to solve the problem]
為了解決上述課題，本發明，係為藉由在第7圖之區域C中，一邊照射氮氣自由基一邊進行反應性濺鍍而形成配向性優異的氮化鎵薄膜之發明，本發明係一種氮化鎵薄膜之製造方法，其係一邊從自由基槍部的放出口對被配置於真空槽內的基板照射氮自由基，一邊將金屬鎵的靶材藉由含有氮氣與濺鍍氣體的混合氣體之電漿來進行濺鍍，並使所產生的濺鍍粒子到達基板，而形成氮化鎵薄膜。
本發明係氮化鎵薄膜之製造方法，其中，前述靶材，係以與前述基板相對面的方式來配置於防附著板容器之中，於前述防附著板容器之中導入前述濺鍍氣體與前述氮氣。
本發明係氮化鎵薄膜之製造方法，其中，於前述放出口處，係配置將氮氣之離子去除的過濾器。
本發明係氮化鎵薄膜之製造方法，其中，身為被導入至前述自由基槍部的氮氣之在前述真空槽內部的分壓值之原料氣體分壓之值，係相對於將身為於前述混合氣體中所含有之氮氣的分壓值之反應氣體分壓之值與前述原料氣體分壓之值合計所得之合計值而言，成為38%以上63%以下之範圍。
本發明係氮化鎵薄膜之製造方法，其中，當使前述基板昇溫至300℃以上500℃以下時，身為被導入至前述自由基槍部的氮氣之在前述真空槽內部的分壓值之原料氣體分壓之值，係相對於將身為於前述混合氣體中所含有之氮氣的分壓值之反應氣體分壓之值與前述原料氣體分壓之值合計所得之合計值而言，成為38%以上50%以下之範圍。
[發明效果]In order to solve the above-mentioned problems, the present invention is an invention for forming a gallium nitride thin film with excellent alignment by reactive sputtering in a region C of FIG. 7 while irradiating nitrogen radicals, and the present invention is a nitrogen A method for manufacturing a gallium thin film is to irradiate a substrate disposed in a vacuum tank with nitrogen radicals from a discharge port of a radical gun section, while passing a target of metal gallium through a mixed gas containing nitrogen and a sputtering gas. Plasma is used for sputtering, and the generated sputtering particles reach the substrate to form a gallium nitride film.
In the method for manufacturing a gallium nitride thin film according to the present invention, the target is disposed in an anti-adhesion plate container so as to face the substrate, and the sputtering gas and the anti-adhesion plate container are introduced into the anti-adhesion plate container. The aforementioned nitrogen.
The present invention relates to a method for manufacturing a gallium nitride film, wherein a filter for removing nitrogen ions is arranged at the discharge port.
The present invention is a method for manufacturing a gallium nitride thin film, wherein the value of the partial pressure of the raw material gas, which is the partial pressure of the nitrogen gas introduced into the radical gun portion in the vacuum chamber, is relative to that of The total value obtained by adding the partial pressure value of the reaction gas and the partial pressure value of the raw material gas to the partial pressure value of nitrogen contained in the mixed gas is in a range of 38% to 63%.
In the method for manufacturing a gallium nitride thin film according to the present invention, when the substrate is heated to a temperature of 300 ° C. or higher and 500 ° C. or lower, the partial pressure value of the nitrogen gas introduced into the radical gun portion in the vacuum chamber is The value of the partial pressure of the raw material gas is relative to the total value obtained by adding the value of the partial pressure of the reaction gas and the value of the partial pressure of the raw material gas, which is the partial pressure of the nitrogen contained in the mixed gas. 38% to 50%.
[Inventive effect]
在使氮化鎵之結晶成長時，在靶材側與基板側之雙方處氮化係被促進，因此，可得到結晶性佳之氮化鎵薄膜。When the crystal of gallium nitride is grown, the nitride system is promoted on both the target side and the substrate side, and thus a gallium nitride thin film having excellent crystallinity can be obtained.
參照第1圖，符號2，係為使用於本發明之成膜裝置，並具有真空槽10。
於真空槽10的內部，係具有：基板配置部20、反應性濺鍍部30、以及自由基槍部40。Referring to FIG. 1, reference numeral 2 is a film forming apparatus used in the present invention, and has a vacuum tank 10.
Inside the vacuum chamber 10, the substrate includes a substrate disposing portion 20, a reactive sputtering portion 30, and a radical gun portion 40.
基板配置部20，係具有：供基板22配置的基板保持具21、和將被配置於基板保持具21的基板22進行加熱的加熱器23。
基板保持具21係被設置於真空槽10的頂部，加熱器23，係以位於被配置於基板保持具21的基板22的背面與頂部之間的方式來被固定於頂部。The substrate placement section 20 includes a substrate holder 21 on which the substrate 22 is placed, and a heater 23 that heats the substrate 22 placed on the substrate holder 21.
The substrate holder 21 is provided on the top of the vacuum tank 10, and the heater 23 is fixed on the top so as to be located between the back surface and the top of the substrate 22 disposed on the substrate holder 21.
反應性濺鍍部30與自由基槍部40係被配置於基板保持具21的下方，被配置於基板保持具21的基板22之表面，係以面向反應性濺鍍部30與自由基槍部40的方式來朝向下方。The reactive sputtering part 30 and the radical gun part 40 are arranged below the substrate holder 21 and are arranged on the surface of the substrate 22 of the substrate holder 21 so as to face the reactive sputtering part 30 and the radical gun part. 40 ways to face down.
基板保持具21，係亦可不設置於頂部而設置於真空槽10的壁面或底面，而將反應性濺鍍部30與自由基槍部40設置於與基板保持具21相對向的位置。The substrate holder 21 may be provided on the wall surface or the bottom surface of the vacuum tank 10 instead of the top portion, and the reactive sputtering portion 30 and the radical gun portion 40 may be provided at positions facing the substrate holder 21.
反應性濺鍍部30係具有防附著板容器31，於防附著板容器31的內部，係配置有濺鍍電極32。濺鍍電極32，係為容器形形狀，於身為濺鍍電極32之容器之中，係配置有由金屬鎵所成之靶材33。The reactive sputtering portion 30 includes an anti-adhesion plate container 31, and a sputtering electrode 32 is arranged inside the anti-adhesion plate container 31. The sputtering electrode 32 has a container shape, and a target 33 made of metal gallium is arranged in a container that is the sputtering electrode 32.
防附著板容器31係具有放出口37，濺鍍電極32的開口34與防附著板容器31的放出口37係相連通。靶材33，係以經由該等開口34與放出口37，來與被配置於基板保持具21之基板22相對面的方式而被配置。The anti-adhesion plate container 31 has a discharge opening 37, and the opening 34 of the sputter electrode 32 is in communication with the anti-adhesion plate container 31 discharge. The target 33 is disposed so as to face the substrate 22 disposed on the substrate holder 21 through the opening 34 and the discharge port 37.
於真空槽10的外部處，係配置有濺鍍電源35與加熱電源28。
濺鍍電極32係被連接於濺鍍電源35，真空槽10係被連接於接地電位，若使濺鍍電源35動作，則會對濺鍍電極32施加濺鍍電壓，若使加熱電源28動作，則加熱器23會被通電而發熱。A sputtering power source 35 and a heating power source 28 are arranged outside the vacuum tank 10.
The sputtering electrode 32 is connected to the sputtering power source 35, and the vacuum tank 10 is connected to the ground potential. If the sputtering power source 35 is operated, a sputtering voltage is applied to the sputtering electrode 32, and if the heating power source 28 is operated, The heater 23 is energized and generates heat.
於真空槽10之外部處，係被配置有氣體供給裝置15。氣體供給裝置15，係具有：供給濺鍍氣體之濺鍍氣體源26與供給反應氣體之反應氣體源27、和被連接於濺鍍氣體源26與反應氣體源27的混合器36。A gas supply device 15 is arranged outside the vacuum tank 10. The gas supply device 15 includes a sputtering gas source 26 for supplying a sputtering gas, a reaction gas source 27 for supplying a reaction gas, and a mixer 36 connected to the sputtering gas source 26 and the reaction gas source 27.
混合器36係被連接於防附著板容器31，從濺鍍氣體源26與反應氣體源27，濺鍍氣體與反應氣體係以所期望的流量分別被供給至混合器36，被供給的濺鍍氣體與反應氣體係在混合器36作混合，成為混合氣體而被供給至防附著板容器31的內部。The mixer 36 is connected to the anti-adhesion plate container 31. The sputtering gas source 26 and the reaction gas source 27, the sputtering gas and the reaction gas system are respectively supplied to the mixer 36 at a desired flow rate, and the supplied sputtering is performed. The gas and the reaction gas system are mixed in the mixer 36 to be mixed gas and supplied to the inside of the anti-adhesion plate container 31.
於濺鍍氣體中係使用氬等之稀有氣體，反應氣體係為包含氮原子的氣體，可採用N2 氣體(氮氣)、NH3 氣體、N2 H4 氣體、NO2 氣體、NO氣體、N2 O氣體等。在此係使用氮氣。A rare gas such as argon is used in the sputtering gas. The reaction gas system is a gas containing nitrogen atoms. N 2 gas (nitrogen), NH 3 gas, N 2 H 4 gas, NO 2 gas, NO gas, N 2 O gas and so on. Here, nitrogen was used.
於真空槽10係連接有真空排氣裝置19，若使真空排氣裝置19動作，則真空槽10之內部會被真空排氣，而形成真空環境。
在使真空槽10之內部形成真空環境之後，若一邊從氣體供給裝置15之混合器36對於防附著板容器31的內部導入混合氣體，一邊使濺鍍電源35啟動來對濺鍍電極32施加交流之濺鍍電壓，則包含氬氣之電漿與氮氣之電漿的混合氣體之電漿會被形成於靶材33的表面上，藉由氬氣電漿而使靶材33的表面被濺鍍。A vacuum exhaust device 19 is connected to the vacuum tank 10. If the vacuum exhaust device 19 is operated, the inside of the vacuum tank 10 will be evacuated by vacuum to form a vacuum environment.
After a vacuum environment is formed inside the vacuum tank 10, if a mixed gas is introduced into the anti-adhesion plate container 31 from the mixer 36 of the gas supply device 15, the sputtering power source 35 is activated to apply AC to the sputtering electrode 32. The sputtering voltage, a plasma of a mixed gas containing an argon plasma and a nitrogen plasma is formed on the surface of the target 33, and the surface of the target 33 is sputtered by the argon plasma. .
此時，靶材33的表面之金屬鎵，係藉由氮氣電漿而被氮化，而使靶材33的表面之氮化鎵被濺鍍。At this time, the metal gallium on the surface of the target 33 is nitrided by a nitrogen plasma, and the gallium nitride on the surface of the target 33 is sputtered.
身為從靶材33的表面所飛散的氮化鎵的粒子之濺鍍粒子38，係通過開口34與放出口37，被放出至真空槽10的內部，並到達被配置於基板保持具21的基板22。交流之濺鍍電壓係為13.56MHz之高頻電壓。The sputtered particles 38, which are gallium nitride particles scattered from the surface of the target 33, are discharged into the vacuum chamber 10 through the opening 34 and the discharge port 37, and reach the substrate disposed on the substrate holder 21. Substrate 22. The AC sputtering voltage is a high-frequency voltage of 13.56 MHz.
自由基槍部40，係具有反應筒44、和被設置於反應筒44的活性化裝置43。
於真空槽10處，係設置有裝置用容器42，反應筒44，係被配置於裝置用容器42的內部。The radical gun unit 40 includes a reaction tube 44 and an activation device 43 provided in the reaction tube 44.
At the vacuum chamber 10, a device container 42 and a reaction tube 44 are provided inside the device container 42.
於真空槽10的外部處，係配置有原料氣體供給源45與反應用電源46。於原料氣體供給源45係配置有原料氣體，並將原料氣體供給至反應筒44的內部。在此，原料氣體係為氮氣。A source gas supply source 45 and a reaction power source 46 are arranged outside the vacuum tank 10. A source gas is arranged in the source gas supply source 45, and the source gas is supplied to the inside of the reaction tube 44. Here, the source gas system is nitrogen.
此時，若從反應用電源46將高頻之離子化電壓供給至活性化裝置43，則原料氣體係在反應筒44的內部被活性化，而產生原料氣體之離子(氮離子)與原料氣體之自由基(氮自由基48)。活性化裝置43，係為被捲繞於反應筒44的周圍的線圈。At this time, if a high-frequency ionization voltage is supplied to the activation device 43 from the reaction power source 46, the raw material gas system is activated inside the reaction cylinder 44 to generate raw material gas ions (nitrogen ions) and raw material gas. Free radicals (nitrogen radicals 48). The activation device 43 is a coil wound around the reaction tube 44.
圖中符號24係為閘門，藉由旋轉軸25而被旋轉，並藉由閘門24的開閉而使基板22露出，或是被覆蓋。在此，閘門24係被打開，而基板22係露出。Symbol 24 in the figure is a gate, which is rotated by the rotation shaft 25, and the substrate 22 is exposed or covered by the opening and closing of the gate 24. Here, the shutter 24 is opened, and the substrate 22 is exposed.
反應筒44係具有放出口49。於放出口49處，係配置有不讓離子通過之周知的過濾器裝置47，身為在反應筒44之內部所產生之原料氣體的自由基之氮自由基48雖會通過過濾器裝置47，但原料氣體的離子並無法通過過濾器裝置47，而構成為原料氣體的離子不會從放出口49漏出至反應筒44的外部。The reaction tube 44 has a discharge port 49. At the discharge port 49, a well-known filter device 47 is provided to prevent ions from passing. Although the nitrogen radical 48, which is a radical of the raw material gas generated inside the reaction tube 44, passes through the filter device 47, However, the ions of the source gas cannot pass through the filter device 47, and the ions of the source gas are not leaked from the discharge port 49 to the outside of the reaction tube 44.
從自由基槍部40係不放出原料氣體的離子，而是放出身為原料氣體的自由基之氮自由基48，並到達被配置於基板保持具21之基板22的表面。The radical gun portion 40 does not emit ions of the source gas, but emits nitrogen radicals 48 which are radicals that are the source gas, and reaches the surface of the substrate 22 disposed on the substrate holder 21.
加熱器23，係藉由加熱電源28而被通電，基板22，係藉由已發熱的加熱器23而被加熱並昇溫至600℃以上的溫度。但，基板22的溫度若為300℃以上，則可為未達900℃。
到達基板22的表面的濺鍍粒子38之中，氮不足的濺鍍粒子38中之鎵會與氮自由基48進行反應，而形成氮的比例變大的氮化鎵結晶，而於基板22的表面使氮化鎵薄膜成長。The heater 23 is energized by the heating power source 28, and the substrate 22 is heated by the heated heater 23 and heated to a temperature of 600 ° C or higher. However, if the temperature of the substrate 22 is 300 ° C or higher, it may be less than 900 ° C.
Among the sputtered particles 38 reaching the surface of the substrate 22, gallium in the nitrogen-deficient sputtered particles 38 will react with the nitrogen radicals 48 to form a gallium nitride crystal with a larger proportion of nitrogen. The surface makes the GaN film grow.
第2圖之符號6，係為被形成為特定膜厚的氮化鎵薄膜，基板22，係於藍寶石基板4上配置以HVPE法(氫化物氣相成長法：Hydride Vapor Phase Epitaxy)成長後的n型氮化鎵薄膜5，使藉由本發明之成膜裝置2而成長的氮化鎵薄膜6接觸配置於該n型氮化鎵薄膜5的表面。Symbol 6 in FIG. 2 is a gallium nitride thin film having a specific thickness. The substrate 22 is formed on the sapphire substrate 4 and is grown by HVPE method (Hydride Vapor Phase Epitaxy). The n-type gallium nitride thin film 5 is such that a gallium nitride thin film 6 grown by the film forming apparatus 2 of the present invention is placed in contact with the surface of the n-type gallium nitride thin film 5.
於反應氣體中，係含有決定所形成之氮化鎵薄膜6之p型或n型的雜質之化合物，例如，在添加有鎂化合物氣體的情況，係若是於在基板22的表面成長的氮化鎵薄膜中摻雜鎂，則形成p型的氮化鎵薄膜。The reaction gas is a compound containing impurities that determine the p-type or n-type of the gallium nitride film 6 to be formed. For example, when a magnesium compound gas is added, the reaction gas is a nitride that grows on the surface of the substrate 22. Magnesium is doped in the gallium film to form a p-type gallium nitride film.
於以HVPE法所形成的n型氮化鎵薄膜5被露出的基板22之表面，改變混合氣體中之反應氣體的含有率來形成氮化鎵薄膜6。On the surface of the substrate 22 on which the n-type gallium nitride film 5 formed by the HVPE method is exposed, the content ratio of the reaction gas in the mixed gas is changed to form the gallium nitride film 6.
於下述表1展示形成薄膜的條件。
由氬所成之濺鍍氣體的壓力(濺鍍氣體分壓)係維持在一定值之0.130Pa，身為被導入至自由基槍部40之原料氣體之氮氣之真空槽10中的壓力(原料氣體分壓)亦被維持在一定值之0.030Pa，在該狀態下，使身為被與濺鍍氣體混合之反應氣體之氮氣之真空槽10中的壓力(反應氣體分壓)變化。The conditions for forming a thin film are shown in Table 1 below.
The pressure (sputter gas partial pressure) of the sputtering gas formed by argon is maintained at a constant value of 0.130 Pa. The pressure (raw material) in the vacuum tank 10 of nitrogen, which is a raw material gas introduced into the radical gun section 40 The gas partial pressure) is also maintained at a certain value of 0.030 Pa. In this state, the pressure (reaction gas partial pressure) in the vacuum tank 10 of nitrogen gas, which is a reaction gas mixed with the sputtering gas, is changed.
表1中之「氮比率1」，係為原料氣體分壓RG(一定值之0.03Pa)相對於原料氣體分壓RG(Pa)與反應氣體分壓RE(Pa)之合計值的比率，「氮比率2」，係為原料氣體分壓RG(Pa)與反應氣體分壓RE(Pa)之合計值相對於原料氣體分壓RG(Pa)與反應氣體分壓RE(Pa)與濺鍍氣體分壓SP(Pa)之合計值的比率。
原料氣體分壓RG(Pa)與反應氣體分壓RE(Pa)，係為將被配置於真空槽10內之基板22的環境之壓力設為全壓時之在真空槽10之內部的分壓值。The "nitrogen ratio 1" in Table 1 is a ratio of the partial pressure RG of the raw gas (0.03 Pa of a certain value) to the total value of the partial pressure RG (Pa) of the raw gas and the partial pressure RE (Pa) of the reactive gas. Nitrogen ratio 2 "is the total value of the partial pressure RG (Pa) of the raw gas and the partial pressure RE (Pa) of the reaction gas relative to the partial pressure RG (Pa) of the raw gas and the partial pressure of the reaction gas RE (Pa) and the sputtering gas. Ratio of the sum of the partial pressures SP (Pa).
The partial pressure of the source gas RG (Pa) and the partial pressure of the reaction gas RE (Pa) are the partial pressures in the vacuum tank 10 when the pressure of the environment of the substrate 22 disposed in the vacuum tank 10 is set to the full pressure. value.
於下述表1～表4中，氮比率1與氮比率2係以下述式表示。
氮比率1＝RG/(RG+RE)
氮比率2＝(RG+RE)/(RG+RE+SP)In the following Tables 1 to 4, the nitrogen ratio 1 and the nitrogen ratio 2 are represented by the following formulas.
Nitrogen ratio 1 = RG / (RG + RE)
Nitrogen ratio 2 = (RG + RE) / (RG + RE + SP)
於表1中，作為成膜條件，係被記載為作了變化之反應氣體分壓RE(Pa)之值、和對應於反應氣體分壓RE(Pa)之值的氮比率1與氮比率2。In Table 1, the film formation conditions are described as the values of the reactive gas partial pressure RE (Pa) and the nitrogen ratio 1 and nitrogen ratio 2 corresponding to the values of the reactive gas partial pressure RE (Pa). .
在此等成膜條件下，首先，觀察所形成之薄膜的表面狀態，並判斷出薄膜為金屬鎵之薄膜或是氮化鎵薄膜6。將判斷結果展示於下述表1。Under these film formation conditions, first, the surface state of the formed thin film is observed, and it is determined whether the thin film is a metal gallium thin film or a gallium nitride thin film 6. The judgment results are shown in Table 1 below.
又，將所得之氮化鎵薄膜6進行X線射線繞射解析(在此係X射線搖擺曲線法)，並依據ω與X射線繞射強度的關係，求出代表(10-10)配向性之峰值之半高寬(秒：arcsec)。將其結果展示於下述表1與第3圖之圖表。In addition, the obtained gallium nitride film 6 was subjected to X-ray diffraction analysis (here, the X-ray rocking curve method), and a representative (10-10) orientation was obtained based on the relationship between ω and X-ray diffraction intensity. The full width at half maximum of the peak (seconds: arcsec). The results are shown in the graphs in Tables 1 and 3 below.
又，測定所得之氮化鎵薄膜6的膜厚，並依據測定結果與成膜時間，算出氮化鎵薄膜6之成長速度(nm/分)。將其結果展示於下述表1與第4圖之圖表。The film thickness of the obtained gallium nitride thin film 6 was measured, and the growth rate (nm / min) of the gallium nitride thin film 6 was calculated based on the measurement results and the film formation time. The results are shown in the graphs in Tables 1 and 4 below.
依據表1，得知：在進行自由基照射來形成氮化鎵薄膜的情況時，氮比率1係以40%以上63%以下之範圍內為佳。According to Table 1, when the gallium nitride thin film is formed by radical irradiation, it is found that the nitrogen ratio 1 is preferably within a range of 40% to 63%.
表1中，記載有「-」的欄位，係為無法確認氮化鎵之成膜條件的結果，但是，在反應氣體分壓0.035Pa之條件下雖以目視可觀察到金屬，但可觀察到X射線之峰值，因此，可推測於表面之金屬層的下層處，係形成有氮化鎵薄膜。The column "-" in Table 1 is a result of not being able to confirm the film formation conditions of gallium nitride. However, the metal can be visually observed under the conditions of the partial pressure of the reaction gas of 0.035 Pa, but it can be observed. At the peak of X-ray, it can be presumed that a gallium nitride thin film is formed at the lower layer of the metal layer on the surface.
接著，將從自由基槍部40被導入至真空槽10中之氮氣的分壓值(於表1中係原料氣體分壓)、和作為反應性濺鍍之反應氣體而被導入至真空槽10中之氮氣的分壓值、以及基板22的溫度，作為濺鍍條件，測定出(10-10)面之XRC半值寬(XRC：X射線搖擺曲線法)、和(0002)面之XRC半值寬、以及成長速度。濺鍍氣體的分壓值係各條件均為0.13Pa。
將測定結果展示於表2～4。於濺鍍氣體中係使用有氬氣。
表2、3中之「◎」，係代表半值寬為狹窄的測定結果，「○」與「△」與「×」，係半值寬之值依此順序變大。在以被記載為「×」之條件所形成的薄膜係為無法使用之不良品，但，以被記載為「◎」之條件所形成的薄膜、和以被記載為「○」之條件所形成的薄膜、以及以被記載為「△」之條件所形成的薄膜係為可使用的品質。
表4中之「◎」，係代表成膜速度為大的測定結果，「○」與「△」與「×」，係成膜速度之值依此順序變小。被記載為「×」之條件的成膜速度為小，由於在薄膜形成上需要長時間，因此不適合實際使用，但，被記載為「◎」之條件、和被記載為「○」之條件、以及被記載為「△」之條件的成膜速度係為可實際使用的條件。
另外，表2～4中，「-」係為無法形成薄膜的條件。「Metal」係被記載於無法形成氮化鎵薄膜而形成了金屬鎵薄膜的條件。
依據以上之表2～4的測定結果，於300℃以上、未達900℃之溫度範圍中，氮比率1，係RG＝0.03Pa、RE＝0.05時之值0.375(＝0.03(0.03+0.05)：表中係為38%)成為可得到良品之最低值。
在300℃以上500℃以下之溫度範圍內得到良品時之氮比率1之最大值係為0.5。
接著，第5圖，係為使用有藉由本發明所形成之氮化鎵薄膜6的發光元件(LED)50，若將電流流通於陽極電極61與陰極電極62之間，則發光層53會發光。Next, the partial pressure value of nitrogen gas (the partial pressure of the source gas in Table 1) introduced from the radical gun portion 40 into the vacuum tank 10 and the reactive gas as a reactive sputtering gas are introduced into the vacuum tank 10 The partial pressure of nitrogen in the medium and the temperature of the substrate 22 were used as the sputtering conditions to determine the XRC half-value width of the (10-10) plane (XRC: X-ray rocking curve method) and the XRC half of the (0002) plane. The value is wide, and the speed of growth. The partial pressure value of the sputtering gas is 0.13 Pa under each condition.
The measurement results are shown in Tables 2 to 4. Argon was used as the sputtering gas.
"◎" in Tables 2 and 3 represents the measurement results when the half-value width is narrow, and "○", "△", and "×" indicate that the half-value width becomes larger in this order. The thin film formed under the conditions described as "×" is a defective product that cannot be used, but the thin film formed under the conditions described as "◎" and the conditions described as "○" The quality of the thin film and the thin film formed under the conditions described as "△" are acceptable qualities.
"◎" in Table 4 represents a measurement result with a large film-forming speed, and "○", "△", and "×" indicate that the value of the film-forming speed becomes smaller in this order. The film formation speed of the conditions described as "×" is small, and it takes a long time to form a thin film, so it is not suitable for practical use. However, the conditions described as "◎" and the conditions described as "○" In addition, the film formation rate of the conditions described as "△" is a condition which can be actually used.
In addition, in Tables 2-4, "-" is a condition which cannot form a thin film. "Metal" is described in a condition where a gallium nitride thin film cannot be formed and a metal gallium thin film is formed.
According to the measurement results in Tables 2 to 4 above, in a temperature range of 300 ° C or higher and less than 900 ° C, the nitrogen ratio is 0.375 (= 0.03 (0.03 + 0.05) when RG = 0.03Pa and RE = 0.05). (38% in the table) becomes the lowest value for obtaining good products.
The maximum value of the nitrogen ratio 1 when a good product is obtained in a temperature range of 300 ° C to 500 ° C is 0.5.
Next, FIG. 5 is a light emitting element (LED) 50 using the gallium nitride thin film 6 formed by the present invention. If a current is passed between the anode electrode 61 and the cathode electrode 62, the light emitting layer 53 emits light. .
此發光元件50，係以在藍寶石基板51上藉由磊晶成長所形成的氮化鎵薄膜52～55、6、57～59所構成，詳細而言，發光元件50，係具有接觸到藍寶石基板51的表面來成長之膜厚2μm的n-GaN薄膜52、和於n-GaN薄膜52上成長之膜厚70nm的發光層(MQW)53，陰極電極62，係與n-GaN薄膜52接觸來形成。The light-emitting element 50 is composed of a gallium nitride film 52 to 55, 6, 57 to 59 formed by epitaxial growth on a sapphire substrate 51. In detail, the light-emitting element 50 has a contact with a sapphire substrate The n-GaN film 52 with a film thickness of 2 μm grown on the surface of 51, the light-emitting layer (MQW) 53 with a film thickness of 70 nm grown on the n-GaN film 52, and the cathode electrode 62 are in contact with the n-GaN film 52. form.
於發光層53上，係使膜厚20nm的p型底層薄膜54與發光層53接觸來成長，於p型底層薄膜54的表面，係使膜厚100nm的p型層薄膜55成長，於p型層薄膜55的表面上，係使以本發明所形成，並含有高濃度的鎂之膜厚4nm的p＋ 型之氮化鎵薄膜6成長。On the light-emitting layer 53, a p-type underlayer film 54 having a thickness of 20 nm is grown in contact with the light-emitting layer 53. On the surface of the p-type under-layer film 54, a p-type layer thin film 55 with a thickness of 100 nm is grown on the p-type On the surface of the layer film 55, a p + -type gallium nitride film 6 formed in the present invention and containing a high concentration of magnesium and having a film thickness of 4 nm is grown.
發光層53，係為多層量子阱(MQW)構造的氮化鎵薄膜。p型底層薄膜54之雜質係為鋁。The light emitting layer 53 is a gallium nitride thin film with a multilayer quantum well (MQW) structure. The impurity of the p-type underlayer film 54 is aluminum.
於p＋ 型之氮化鎵薄膜6的表面上，係使含有高濃度的矽之膜厚2nm的n＋ 型之氮化鎵薄膜57成長，於該氮化鎵薄膜57的表面，係使膜厚400nm的n型之氮化鎵薄膜58成長。On the surface of the p + -type gallium nitride film 6, an n + -type gallium nitride film 57 having a film thickness of 2 nm containing a high concentration of silicon is grown. On the surface of the gallium nitride film 57, a film is formed. An n-type gallium nitride film 58 having a thickness of 400 nm grows.
於n型之氮化鎵薄膜58的表面上，係使以高濃度含有n型雜質之膜厚20nm的接點薄膜59成長，陽極電極61，係與接點薄膜59接觸來作形成。On the surface of the n-type gallium nitride film 58, a contact film 59 having a film thickness of 20 nm containing n-type impurities at a high concentration is grown, and an anode electrode 61 is formed in contact with the contact film 59.
陽極電極61與陰極電極62，係使鈦薄膜與鋁薄膜與鈦薄膜與金薄膜依此順序層積而成的金屬薄膜，且使接觸電阻小，若將電流流通於陽極電極61與陰極電極62之間，則發光層53會以高效率發光。The anode electrode 61 and the cathode electrode 62 are metal films formed by stacking titanium thin films, aluminum thin films, titanium thin films, and gold thin films in this order, and the contact resistance is small. If current is passed through the anode electrodes 61 and the cathode electrodes 62, In between, the light emitting layer 53 emits light with high efficiency.
於上述例中，係藉由本發明來形成位於膜厚100nm的p型層薄膜55上之膜厚4nm的p＋ 型之氮化鎵薄膜6，但是，可藉由本發明來形成位於發光層53上之各氮化鎵薄膜，尤其，係可考慮本發明之對於膜厚2nm的n＋ 型之氮化鎵薄膜57、和膜厚400nm的n型之氮化鎵薄膜58、以及以高濃度含有n型雜質之膜厚20nm的接點薄膜59之適用。In the above example, the p + -type gallium nitride film 6 having a thickness of 4 nm is formed on the p-type layer thin film 55 having a thickness of 100 nm by the present invention. However, the light-emitting layer 53 may be formed by the present invention. Each of the gallium nitride thin films may include n + type gallium nitride film 57 having a film thickness of 2 nm, n type gallium nitride film 58 having a film thickness of 400 nm, and n in a high concentration. A contact film 59 having a thickness of 20 nm for the type impurity is suitable.
於上述例中，係於反應性氣體之中含有雜質之化合物氣體來形成n型或p型之氮化鎵薄膜，但是，可使用含有雜質之靶材來形成n型或p型之氮化鎵薄膜。In the above example, the compound gas containing impurities in the reactive gas is used to form an n-type or p-type gallium nitride thin film, but a target material containing impurities may be used to form an n-type or p-type gallium nitride. film.
第6圖之符號2’，係為可使用於該情況之製造方法的成膜裝置，該成膜裝置2’，係具有反應性濺鍍部30a和輔助濺鍍部30b。Reference numeral 2 'in FIG. 6 is a film forming apparatus that can be used in the manufacturing method in this case, and the film forming apparatus 2' has a reactive sputtering part 30a and an auxiliary sputtering part 30b.
第6圖之成膜裝置2’的反應性濺鍍部30a，係為與上述第1圖之成膜裝置2的反應性濺鍍部30相同之構造，並對於與上述第1圖之成膜裝置2的反應性濺鍍部30相同的構件，於上述第1圖之成膜裝置2的反應性濺鍍部30的構件之符號附加字a並省略說明。又，於成膜裝置2’之其他的構件中，對於與第1圖之成膜裝置2相同的構件，係標示相同的符號並省略說明。The reactive sputtering part 30a of the film forming apparatus 2 'of FIG. 6 has the same structure as the reactive sputtering part 30 of the film forming apparatus 2 of FIG. The components of the reactive sputtering part 30 of the apparatus 2 are the same as those of the reactive sputtering part 30 of the film forming apparatus 2 of the above-mentioned FIG. In addition, among the other members of the film forming apparatus 2 ', the same members as those of the film forming apparatus 2 of Fig. 1 are denoted by the same reference numerals, and description thereof will be omitted.
輔助濺鍍部30b，係具有輔助防附著板容器31b，於輔助防附著板容器31b的內部，係配置有輔助濺鍍電極32b。於輔助濺鍍電極32b，係配置有決定半導體之p型或n型之由雜質所成之雜質用靶材33b。The auxiliary sputtering portion 30b includes an auxiliary anti-adhesion plate container 31b, and an auxiliary sputtering electrode 32b is disposed inside the auxiliary anti-adhesion plate container 31b. The auxiliary sputtering electrode 32b is provided with an impurity target 33b made of impurities that determines the semiconductor's p-type or n-type.
輔助防附著板容器31b係具有輔助放出口37b，雜質用靶材33b，係以經由輔助放出口37b而與被配置於基板保持具21的基板22相對面的方式來配置。The auxiliary anti-adhesion plate container 31b has an auxiliary discharge port 37b, and an impurity target 33b is disposed so as to face the substrate 22 disposed on the substrate holder 21 through the auxiliary discharge port 37b.
於真空槽10的外部處，係配置有輔助濺鍍電源35b。
輔助濺鍍電極32b係被連接於輔助濺鍍電源35b，真空槽10係被連接於接地電位，若輔助濺鍍電源35b動作，則會對輔助濺鍍電極32b施加濺鍍電壓。An auxiliary sputtering power source 35b is disposed outside the vacuum tank 10.
The auxiliary sputtering electrode 32b is connected to the auxiliary sputtering power supply 35b, and the vacuum tank 10 is connected to the ground potential. When the auxiliary sputtering power supply 35b operates, a sputtering voltage is applied to the auxiliary sputtering electrode 32b.
於真空槽10之外部處，係配置有輔助氣體供給裝置15b。於輔助氣體供給裝置15b，係配置有供給身為氬等之稀有氣體之輔助濺鍍氣體的輔助濺鍍氣體源26b。An auxiliary gas supply device 15b is arranged outside the vacuum tank 10. The auxiliary gas supply device 15b is provided with an auxiliary sputtering gas source 26b for supplying an auxiliary sputtering gas including a rare gas such as argon.
此成膜裝置2’之反應性濺鍍部30a的靶材33a係藉由與第1圖之成膜裝置2相同的動作而被反應性濺鍍，當從自由基槍部40氮自由基48被放出而於基板22的表面使氮化鎵薄膜成長時，若將輔助濺鍍部30b的雜質用靶材33b以輔助濺鍍氣體進行濺鍍，並使所產生的輔助濺鍍粒子38b到達基板22表面，則於被形成於基板22的表面之氮化鎵薄膜中含有輔助濺鍍粒子38b之雜質，而可形成p型、或n型之氮化鎵薄膜。The target 33a of the reactive sputtering part 30a of this film forming apparatus 2 'is reactively sputtered by the same operation as the film forming apparatus 2 of FIG. When the gallium nitride thin film is grown on the surface of the substrate 22 after being released, the target 33b for impurities in the auxiliary sputtering portion 30b is sputtered with an auxiliary sputtering gas, and the generated auxiliary sputtering particles 38b reach the substrate. On the surface 22, the gallium nitride film formed on the surface of the substrate 22 contains impurities assisting the sputtering particles 38b, and a p-type or n-type gallium nitride film can be formed.
6‧‧‧氮化鎵薄膜6‧‧‧GaN film
22‧‧‧基板 22‧‧‧ substrate
31‧‧‧防附著板容器 31‧‧‧Anti-stick plate container
33‧‧‧靶材 33‧‧‧Target
38‧‧‧濺鍍粒子 38‧‧‧Sputtered particles
40‧‧‧自由基槍部 40‧‧‧Free radical gun department
48‧‧‧氮自由基 48‧‧‧ nitrogen free radicals
49‧‧‧放出口 49‧‧‧ release
50‧‧‧發光元件 50‧‧‧Light-emitting element
53‧‧‧發光層 53‧‧‧Light-emitting layer
[第1圖]係使用於本發明之成膜裝置[FIG. 1] It is a film forming apparatus used in the present invention
[第2圖]係用以對於基板與氮化鎵薄膜的位置關係作說明之圖 [Fig. 2] A diagram for explaining the positional relationship between the substrate and the gallium nitride film
[第3圖]係展示氮氣壓與半高寬的關係之圖表 [Figure 3] is a graph showing the relationship between nitrogen pressure and full width at half maximum
[第4圖]係展示氮氣壓與成長速度的關係之圖表 [Figure 4] A graph showing the relationship between nitrogen pressure and growth rate
[第5圖]係使用有藉由本發明所製造之氮化鎵薄膜的LED之一例 [Fig. 5] An example of an LED using a gallium nitride film manufactured by the present invention
[第6圖]係使用於本發明之成膜裝置之另一例 [Figure 6] Another example of the film forming apparatus used in the present invention
[第7圖]係展示氮分壓與所形成的薄膜中之含氮量的關係之圖表 [Figure 7] A graph showing the relationship between the nitrogen partial pressure and the nitrogen content in the formed film
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