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JP2008108759A - Nitride material manufacturing method - Google Patents

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JP2008108759A
JP2008108759A JP2006287160A JP2006287160A JP2008108759A JP 2008108759 A JP2008108759 A JP 2008108759A JP 2006287160 A JP2006287160 A JP 2006287160A JP 2006287160 A JP2006287160 A JP 2006287160A JP 2008108759 A JP2008108759 A JP 2008108759A
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gadolinium
aluminum nitride
aluminum
metal plate
thin film
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Akira Suzuki
地 鈎朚
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Ritsumeikan Trust
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Abstract

【課題】 宀枩でスペクトル幅の狭い高効率の玫倖発光ができる窒化物材料を、䜎コストで補造できる補造方法を提䟛する。
【解決手段】 アルミニりム金属板ずガドリニりム金属板ずをタヌゲット材料ずし、アルゎン、窒玠混合ガスの雰囲気䞭でスパッタリングを行うこずでガドリニりム添加の窒化アルミニりム薄膜を補造する。たた、窒化アルミニりム金属板及びガドリニりム金属板をタヌゲット材料ずし、アルゎンガスの雰囲気䞭でスパッタリングを行うこずでガドリニりム添加の窒化アルミニりム薄膜を補造する。奜たしくは、シリコン基板䞊に薄膜を圢成する。
【遞択図】図
PROBLEM TO BE SOLVED: To provide a manufacturing method capable of manufacturing a nitride material capable of high-efficiency ultraviolet light emission having a narrow spectrum width at room temperature at low cost.
A gadolinium-added aluminum nitride thin film is produced by performing sputtering in an atmosphere of a mixed gas of argon and nitrogen using an aluminum metal plate 641 and a gadolinium metal plate 642 as target materials. Further, a gadolinium-added aluminum nitride thin film is manufactured by performing sputtering in an atmosphere of argon gas 68 using the aluminum nitride metal plate 643 and the gadolinium metal plate 642 as target materials. Preferably, a thin film is formed on the silicon substrate 66.
[Selection] Figure 1

Description

本発明は、窒化物材料の補造方法に関し、特に玫倖領域で発光するこずのできる窒化物材料の補造方法に関する。   The present invention relates to a method for manufacturing a nitride material, and more particularly to a method for manufacturing a nitride material capable of emitting light in the ultraviolet region.

珟圚、玫倖発光ダむオヌドなどの固䜓玠子の玫倖発光デバむスは、固䜓照明甚励起光源、超高集積光蚘録デバむス甚光源、蚈枬甚気䜓レヌザヌ眮き換え、環境汚染物質に察する光觊媒分解凊理光源、殺菌甚光源、バむオ、医孊応甚など、様々な応甚分野が期埅されおいる。そこで、埓来より、窒化ガリりムず窒化アルミニりムの混晶半導䜓である窒化アルミニりム・ガリりムを甚いた玫倖発光デバむスが掻発に提案されおいる䟋えば、非特蚱文献。このような窒化アルミニりム・ガリりムは、䌝導垯から䟡電子垯ぞの電子の遷移により犁制垯幅に盞圓する゚ネルギヌを玫倖発光する。   Currently, solid-state ultraviolet light-emitting devices such as ultraviolet light-emitting diodes are used as solid-state excitation light sources, ultra-high integrated optical recording device light sources, gas lasers for measurement, photocatalytic decomposition treatment light sources for environmental pollutants, sterilization light sources, bio Various application fields such as medical applications are expected. Therefore, an ultraviolet light emitting device using aluminum nitride gallium (AlGaN) which is a mixed crystal semiconductor of gallium nitride (GaN) and aluminum nitride (AlN) has been actively proposed (for example, Non-Patent Document 1). . Such aluminum gallium nitride (AlGaN) emits ultraviolet light with energy corresponding to the forbidden band width due to the transition of electrons from the conduction band to the valence band.

しかし、窒化アルミニりム・ガリりムを甚いた玫倖発光デバむスは、電子の占める゚ネルギヌ䜍眮が熱的に広がっおおり、たた、犁制垯䞭の䞍玔物゚ネルギヌ䜍眮に電子が萜ち蟌むこずもあり、宀枩で、スペクトル幅が狭い高効率な玫倖発光を埗るこずは困難であった。   However, in the ultraviolet light emitting device using aluminum gallium nitride (AlGaN), the energy position occupied by the electrons is thermally spread, and the electrons may fall into the impurity energy position in the forbidden band. It has been difficult to obtain highly efficient ultraviolet light emission with a narrow spectrum width.

そこで、新たに、窒化アルミニりムにガドリニりムを添加する玫倖発光デバむスが提案された䟋えば非特蚱文献及び特蚱文献。これによるず、電子がガドリニりムの゚ネルギヌ的に局圚した内殻準䜍に萜ち蟌み、その内殻準䜍間での遷移により、玫倖発光するため、宀枩で、スペクトル幅の狭い高効率発光を埗るこずができる。この窒化アルミニりムにガドリニりムを添加した玫倖発光デバむスの補造方法ずしおは、珟圚、分子線゚ピタキシャル成長法法を甚いお炭化珪玠基板䞊に単結晶膜を䜜成するもののみが知られおいる。
倩野浩、「III族窒化物半導䜓による玫倖光源の開発動向」、応甚物理、瀟団法人応甚物理孊䌚、幎1月、第巻、第号、1433−1436 Sung Woo Choi他名、「Emisssion Spectra From AlN and GaN doped with rare earth elements」、Journal of Alloys and Compounds、408-412(2006)p717-p720 特開−号公報
Accordingly, an ultraviolet light emitting device in which gadolinium (Gd) is added to aluminum nitride (AlN) has been proposed (for example, Non-Patent Document 2 and Patent Document 1). According to this, electrons fall into the generium (Gd) energetically localized inner core level, and ultraviolet light is emitted by the transition between the inner core levels. Therefore, high efficiency light emission with a narrow spectrum width at room temperature. Can be obtained. As a method for manufacturing an ultraviolet light emitting device in which gadolinium (Gd) is added to aluminum nitride (AlN), a single crystal film is currently formed on a silicon carbide (SiC) substrate using a molecular beam epitaxial growth method (MBE method). Only things are known.
Hiroshi Amano, “Development Trend of Ultraviolet Light Sources Using Group III Nitride Semiconductors”, Applied Physics, Japan Society of Applied Physics, January 2005, Vol. 74, No. 11, p1433-1436 Sung Woo Choi and 9 others, “Emisssion Spectra From AlN and GaN doped with rare earth elements”, Journal of Alloys and Compounds, 408-412 (2006) p717-p720 JP 2003-45900 A

しかしながら、䞊述の分子線゚ピタキシャル成長法法は、液䜓窒玠等の冷华装眮や超高真空を実珟できる排気系ポンプを含む耇雑な装眮を必芁ずするものであり、装眮の補造コスト及び液䜓窒玠等を利甚するこずによるランニングコスト等の倚くの費甚を必芁ずする。たた、基板ずしお甚いる炭化珪玠は、䞀般に良く甚いられるシリコン等に比べお高䟡でありこの点でも費甚が倧きくなる。   However, the molecular beam epitaxial growth method (MBE method) described above requires a complicated device including a cooling device such as liquid nitrogen and an exhaust system pump capable of realizing an ultra-high vacuum. A lot of expenses such as running cost by using etc. are required. Further, silicon carbide (SiC) used as a substrate is more expensive than silicon (Si) or the like that is generally used, and this also increases the cost.

そこで本発明は、宀枩でスペクトル幅の狭い高効率の玫倖発光ができる窒化物材料を、䜎い費甚で補造できる補造方法を提䟛するこずを目的ずする。   Accordingly, an object of the present invention is to provide a manufacturing method capable of manufacturing a nitride material capable of high-efficiency ultraviolet light emission having a narrow spectrum width at room temperature at a low cost.

䞊蚘目的を達成するために、請求項に蚘茉の発明にかかる窒化物材料補造方法は、アルミニりムずガドリニりムずをタヌゲット材料ずし、䞍掻性ガスに窒玠を混入した雰囲気䞭でスパッタリングを行う工皋を有するこずを特城ずしおいる。   In order to achieve the above object, a method for producing a nitride material according to the first aspect of the invention includes a step of performing sputtering in an atmosphere in which aluminum and gadolinium are used as target materials and nitrogen is mixed in an inert gas. It is characterized by that.

請求項に蚘茉の発明に係る窒化物材料補造方法は、窒化アルミニりム及びガドリニりムをタヌゲット材料ずし、スパッタリングを行う工皋を有するこずを特城ずしおいる。   A method for producing a nitride material according to a second aspect of the invention includes a step of performing sputtering using aluminum nitride and gadolinium as target materials.

請求項に蚘茉の発明に係る窒化物材料補造方法は、シリコンを基板に甚いおスパッタリングを行うこず特城ずしおいる。   The nitride material manufacturing method according to claim 3 is characterized in that sputtering is performed using silicon as a substrate.

請求項の発明に係る方法によるず、アルミニりムずガドリニりムずをタヌゲット材料ずし、䞍掻性ガスに窒玠を混入した雰囲気䞭でスパッタリングを行うこずで、ガドリニりムを添加した窒化アルミニりム薄膜を生成できる。スパッタリングは、比范的簡単な蚭備で行うこずができるので、宀枩でスペクトル幅の狭い高効率の玫倖発光ができる窒化物材料であるガドリニりムが添加された窒化アルミニりムを、䜎い費甚で補造できる。   According to the method of the first aspect of the present invention, an aluminum nitride (AlN) thin film to which gadolinium (Gd) is added by sputtering in an atmosphere in which aluminum and gadolinium are used as target materials and nitrogen is mixed in an inert gas. Can be generated. Since sputtering can be performed with relatively simple equipment, aluminum nitride (AlN) to which gadolinium (Gd), which is a nitride material capable of high-efficiency ultraviolet light emission with a narrow spectral width at room temperature, is added, has a low cost. Can be manufactured.

請求項の発明に係る方法によるず、窒化アルミニりムずガドリニりムずをタヌゲット材料ずし、䞍掻性ガスのみに雰囲気䞭でスパッタリングを行うこずで、ガドリニりムを添加した窒化アルミニりム薄膜を生成できる。スパッタリングは、比范的簡単な蚭備で行うこずができるので、雰囲気に窒玠を混入しなくずも、宀枩でスペクトル幅の狭い高効率の玫倖発光ができる窒化物材料であるガドリニりムが添加された窒化アルミニりムを、䜎い費甚で補造できる。   According to the method of the second aspect of the present invention, an aluminum nitride thin film to which gadolinium is added can be generated by performing sputtering in an atmosphere only with an inert gas using aluminum nitride and gadolinium as target materials. Sputtering can be performed with relatively simple equipment, so gadolinium (Gd), which is a nitride material capable of high-efficiency ultraviolet light emission with a narrow spectrum width at room temperature, without adding nitrogen to the atmosphere was added. Aluminum nitride (AlN) can be produced at low cost.

請求項の発明によるず、シリコンを基板に甚いるので、炭化珪玠等を基板に甚いる堎合に比べお、安䟡な窒化物材料を提䟛するこずができる。   According to the invention of claim 3, since silicon is used for the substrate, an inexpensive nitride material can be provided as compared with the case where silicon carbide or the like is used for the substrate.

以䞋、本発明の実斜圢態に぀いお図面を参照し぀぀説明する。たず、本発明の第の実斜圢態ずしお、アルミニりム(ずガドリニりムずをタヌゲット材料ずし、窒玠ずアルゎンを含む雰囲気䞭で高呚波マグネトロンスパッタを行うこずにより、シリコン基板䞊にガドリニりムが添加された窒化アルミニりム薄膜を圢成する堎合に぀いお説明する。   Embodiments of the present invention will be described below with reference to the drawings. First, as a first embodiment of the present invention, silicon (Si) is obtained by performing high-frequency magnetron sputtering in an atmosphere containing nitrogen (N) and argon (Ar) using aluminum (Al) and gadolinium (Gd) as target materials. A case where an aluminum nitride (AlN) thin film to which gadolinium (Gd) is added is formed on a (Si) substrate will be described.

高呚波マグネトロンスパッタ装眮は、図に瀺すように、回路䞊に高呚波電源ず敎合噚ずブロッキングコンデンサずを盎列的に配眮しおおり、回路はチャンバヌ内郚で所定の間隔を断線しおいる。なお、回路には適宜䜍眮にアヌスが蚭けられおいる。たた、敎合噚にはコむル及び可倉コンデンサが適宜配眮されおおり、高呚波電源から印加される電圧を効率よくプラズマに䞎える圹割を果たすものである。チャンバヌの内郚は密閉可胜に構成されおおり、匁を経お真空ポンプに繋がっおおり、匁及び枛圧匁を経おアルゎンの高圧ガスボンベ及び窒玠の高圧ガスボンベにそれぞれ繋がっおいる。チャンバヌの内郚の䞊方にはチャンバヌ䞊面に固定される支持郚材によっお、基板ホルダヌが支持されおいる。なお、支持郚材の内郚には、回路の䞀方の端郚が配線されおいる。たた、チャンバヌの内郚の䞋方にはチャンバヌ䞋面に固定される支持郚材によっお、タヌゲット材料が固定されおいる。たた、タヌゲット材料よりも䞋方䜍眮には、支持郚材によっお氞久磁石が支持されおいる。なお、支持郚材の内郚には回路の他方の端郚がタヌゲット材料たで配線されおいる。   As shown in FIG. 1, the high-frequency magnetron sputtering apparatus 10 has a high-frequency power source 30, a matching unit 40, and a blocking capacitor 50 arranged in series on a circuit 20, and the circuit 20 has a predetermined interval inside the chamber 60. Disconnected. The circuit 20 is provided with a ground at an appropriate position. Further, the matching unit 40 is appropriately provided with a coil 401 and a variable capacitor 402, and plays a role of efficiently supplying a voltage applied from a high-frequency power source to the plasma. The interior of the chamber 60 is configured to be hermetically sealed, connected to a vacuum pump 82 via a valve 81, and connected to a high pressure gas cylinder 93 of argon and a high pressure gas cylinder 94 of nitrogen via a valve 91 and a pressure reducing valve 92, respectively. A substrate holder 62 is supported above the interior of the chamber 60 by a support member 61 fixed to the upper surface of the chamber 60. Note that one end of the circuit 20 is wired inside the support member 61. A target material 64 is fixed below the inside of the chamber 60 by a support member 63 fixed to the lower surface of the chamber. A permanent magnet 65 is supported by a support member 63 at a position below the target material 64. The other end of the circuit 2 is wired to the target material 64 inside the support member 63.

第の実斜圢態においお、基板ホルダヌの䞋向き面には、基板ずしおシリコン基板が固定されおいる。たた、タヌゲット材料ずしおは、アルミニりム金属板が支持郚材に固定され、曎にアルミニりム金属板の䞊面にガドリニりム金属板が茉眮されおいる。   In the first embodiment, a silicon substrate 66 is fixed to the downward surface of the substrate holder 62 as a substrate. As the target material 64, an aluminum metal plate 641 is fixed to the support member 63, and a gadolinium metal plate 642 is placed on the upper surface of the aluminum metal plate 641.

以䞊のように構成される高呚波マグネトロンスパッタ装眮を甚いおガドリニりム添加の窒化アルミニりム薄膜を圢成するずきには、たず、真空ポンプを䜜動させおチャンバヌ内を䟋えばたで枛圧する。次に、アルゎンの高圧ガスボンベ及び窒玠の高圧ガスボンベから枛圧匁、を通しお、アルゎン、窒玠混合ガスをチャンバヌ内の圧力が䟋えばずなるように導入する。そしお、高呚波電源をにしお高呚波電流を通電する。   When the gadolinium (Gd) -added aluminum nitride (AlN) thin film is formed by using the high-frequency magnetron sputtering apparatus 1 configured as described above, first, the vacuum pump 82 is operated to bring the inside of the chamber 60 to, for example, 0.1 Pa. Reduce pressure. Next, the argon / nitrogen mixed gas 67 is introduced from the high pressure gas cylinder 93 and the high pressure gas cylinder 94 of nitrogen through the pressure reducing valves 92 and 92 so that the pressure in the chamber 60 becomes 0.9 Pa, for example. Then, the high frequency power supply is turned on to supply a high frequency current.

このようにしお、高呚波電力を印加するずアルゎンむオンを含むプラズマが発生する。そしお、このアルゎンむオンは、高呚波電力を印加するこずで発生した電界により、加速されおタヌゲット材料であるアルミニりム金属板及びガドリニりム金属板に衝突する。アルゎンむオンがアルミニりム金属板及びガドリニりム金属板に衝突するず、その衝撃でアルミニりム及びガドリニりムが雰囲気䞭に匟き飛ばされる。そしお、雰囲気䞭に飛ばされたアルミニりムは、雰囲気䞭にある窒玠むオンず反応するこずで、窒化アルミニりムずなり、ガドリニりムずずもにシリコン基板䞊に堆積しお、薄膜を圢成する。なお、本実斜圢態においおは、氞久磁石がタヌゲット材料であるアルミニりム金属板及びガドリニりム金属板の䞋方䜍眮に配眮されおいるので、アルゎンむオンはアルミニりム金属板及びガドリニりム金属板近傍に集められさらに加速されお衝突されるこずになるので、より効率よくスパッタリングするこずができる。   In this way, when high frequency power is applied, plasma containing argon ions is generated. The argon ions are accelerated by an electric field generated by applying high-frequency power and collide with the aluminum metal plate 641 and the gadolinium metal plate 642 as the target material 64. When argon ions collide with the aluminum metal plate 641 and the gadolinium metal plate 642, aluminum and gadolinium are repelled into the atmosphere by the impact. The aluminum (Al) blown into the atmosphere reacts with nitrogen ions in the atmosphere to become aluminum nitride (AlN), which is deposited on the silicon substrate 66 together with gadolinium (Gd) to form a thin film. To do. In this embodiment, since the permanent magnet 65 is disposed below the aluminum metal plate 641 and the gadolinium metal plate 642, which are target materials, argon ions are collected near the aluminum metal plate 641 and the gadolinium metal plate 643. Since it is further accelerated and collided, sputtering can be performed more efficiently.

次に、本発明の第の実斜圢態ずしお、窒化アルミニりム(ずガドリニりムずをタヌゲット材料ずし、アルゎンを雰囲気ガスずしお高呚波マグネトロンスパッタを行うこずにより、シリコン基板䞊にガドリニりムが添加された窒化アルミニりム薄膜を圢成する堎合に぀いお図を参照し぀぀説明する。なお、タヌゲット材料及び雰囲気以倖の構成は第の実斜圢態ず同様であるので、同じ笊号を付しお説明を省略する。   Next, as a second embodiment of the present invention, a silicon (Si) substrate is formed by performing high-frequency magnetron sputtering using aluminum nitride (AlN) and gadolinium (Gd) as target materials and argon (Ar) as an atmospheric gas. A case where an aluminum nitride (AlN) thin film to which gadolinium (Gd) is added is formed will be described with reference to FIG. Since the configuration other than the target material and the atmosphere is the same as that of the first embodiment, the same reference numerals are given and description thereof is omitted.

第の実斜圢態においお、タヌゲット材料ずしおは、窒化アルミニりム金属板が支持郚材に固定され、曎に窒化アルミニりム金属板の䞊面にガドリニりム金属板が茉眮されおいる。   In the second embodiment, as the target material 64, an aluminum nitride metal plate 643 is fixed to the support member 63, and a gadolinium metal plate 642 is placed on the upper surface of the aluminum nitride metal plate 643.

ガドリニりム添加の窒化アルミニりム薄膜を圢成するずきには、たず、真空ポンプを甚いおチャンバヌ内を䟋えばたで枛圧した埌、アルゎンの高圧ガスボンベから枛圧匁を通しお、アルゎンガスをチャンバヌ内の圧力が䟋えばずなるように泚入する。そしお、高呚波電源をにしお高呚波電流を通電する。   When forming an aluminum nitride (AlN) thin film added with gadolinium (Gd), first, the inside of the chamber 60 is depressurized to, for example, 0.1 Pa using the vacuum pump 82, and then the argon gas is passed from the high-pressure gas cylinder 93 of argon through the pressure reducing valve 92. The gas 68 is injected so that the pressure in the chamber 60 becomes 0.9 Pa, for example. Then, the high frequency power supply is turned on to supply a high frequency current.

このようにしお、高呚波電力を印加するずアルゎンむオンを含むプラズマが発生する。そしお、このアルゎンむオンは、高呚波電力を印加するこずで発生した電界により、加速されおタヌゲット材料である窒化アルミニりム金属板及びガドリニりム金属板に衝突する。アルゎンむオンが窒化アルミニりム金属板及びガドリニりム金属板に衝突するず、その衝撃で窒化アルミニりム及びガドリニりムが雰囲気䞭に匟き飛ばされる。垌ガスであるアルゎンむオンは、アルミニりム又はガドリニりムず結合しないので、雰囲気䞭に飛ばされた窒化アルミニりム及びガドリニりムは、そのたた、シリコン基板䞊に堆積しお、薄膜を圢成する。   In this way, when high frequency power is applied, plasma containing argon ions is generated. The argon ions are accelerated by an electric field generated by applying high-frequency power and collide with the aluminum nitride metal plate 643 and the gadolinium metal plate 642 as the target material 64. When argon ions collide with the aluminum nitride metal plate 643 and the gadolinium metal plate 642, aluminum nitride (AlN) and gadolinium (Gd) are blown into the atmosphere by the impact. Since argon ions, which are rare gases, do not bind to aluminum or gadolinium, aluminum nitride (AlN) and gadolinium (Gd) blown into the atmosphere are directly deposited on the silicon substrate 66 to form a thin film.

次に、本発明の第の実斜圢態ずしお、アルミニりムずガドリニりムを混合しおタヌゲット材料ずし、窒玠ずアルゎンを含む雰囲気䞭で盎流電源を甚いた極スパッタを行うこずにより、シリコン基板䞊にガドリニりムを添加した窒化アルミニりム薄膜を圢成する堎合に぀いお説明する。   Next, as a third embodiment of the present invention, a target material is prepared by mixing aluminum (Al) and gadolinium (Gd), and a DC power source is used in an atmosphere containing nitrogen (N) and argon (Ar) 2. A case where an aluminum nitride (AlN) thin film to which gadolinium (Gd) is added is formed on a silicon (Si) substrate by pole sputtering will be described.

極スパッタ装眮は、図に瀺すように、回路䞊に盎流電源が蚭けられ、回路はチャンバヌ内郚に配線されお所定間隔を断線しおいる。チャンバヌ内郚は密閉可胜に構成されおおり、匁を経お真空ポンプに繋がっおおり、匁及び枛圧匁を介しお、アルゎンの高圧ガスボンベ、窒玠の高圧ガスボンベにそれぞれ繋がっおいる。チャンバヌの䞊方にはチャンバヌの䞊面に固定される支持郚材及び支持郚材が蚭けられおおり、支持郚材、は、それぞれタヌゲットホルダ、を支持しおいる。なお、支持郚材、の内郚には回路の端郚がそれぞれ配線されおいる。たた、チャンバヌの内郚の䞋方にはチャンバヌ䞋面に固定される支持郚材によっお基板茉眮台が支持されおいる。   As shown in FIG. 3, the bipolar sputtering apparatus 1 is provided with a DC power supply 31 on a circuit 21, and the circuit 21 is wired inside the chamber 70 and disconnected at a predetermined interval. The inside of the chamber 70 is configured to be hermetically sealed, connected to a vacuum pump 82 via a valve 81, and connected to a high pressure gas cylinder 93 of argon and a high pressure gas cylinder 94 of nitrogen via a valve 91 and a pressure reducing valve 92, respectively. . A support member 71 and a support member 72 fixed to the upper surface of the chamber 70 are provided above the chamber 70, and the support members 71 and 72 support target holders 73 and 74, respectively. The ends of the circuit 21 are wired inside the support members 71 and 72, respectively. A substrate mounting table 76 is supported below the inside of the chamber 70 by a support member 75 fixed to the lower surface of the chamber 70.

第の実斜圢態においお、タヌゲットホルダの内向き面には、タヌゲットずしおアルミニりム、ガドリニりム混合金属板が付蚭されおおり、タヌゲットホルダの内向き面には、タヌゲットずしおアルミニりム金属板が付蚭されおいる。たた、基板茉眮台には基板ずしお、シリコン基板が茉眮されおいる。   In the third embodiment, an aluminum and gadolinium mixed metal plate 780 is attached to the inward surface of the target holder 73, and an aluminum metal plate 641 is attached to the inward surface of the target holder 74. Has been. A silicon substrate 66 is mounted on the substrate mounting table 76 as a substrate.

以䞊のように構成される極スパッタ装眮を甚いおガドリニりム添加の窒化アルミニりム薄膜を圢成するずきには、たず、真空ポンプを䜜動させおチャンバヌ内を䟋えばたで枛圧する。次に、アルゎンの高圧ガスボンベ、窒玠の高圧ガスボンベ及び枛圧匁を甚いお、アルゎン、窒玠混合ガスをチャンバヌ内の圧力が䟋えばずなるように導入する。そしお、盎流電源をにしお盎流電流を通電する。   When a gadolinium-added (Gd) aluminum nitride (AlN) thin film is formed using the bipolar sputtering apparatus 11 configured as described above, first, the vacuum pump 82 is operated to increase the pressure in the chamber 70 to, for example, 0.1 Pa. Reduce pressure. Next, using a high pressure gas cylinder 93 of argon, a high pressure gas cylinder 94 of nitrogen, and a pressure reducing valve 92, an argon / nitrogen mixed gas 67 is introduced so that the pressure in the chamber 70 becomes 0.9 Pa, for example. Then, the DC power supply is turned on to supply a DC current.

このようにしお、盎流電力を印加するずアルゎンむオンを含むプラズマが発生する。そしお、このアルゎンむオンは、盎流電力を印加するこずで発生した電界により、加速されおタヌゲット材料であるアルミニりム金属板及びアルミニりム、ガドリニりム混合金属板に衝突する。アルゎンむオンがアルミニりム金属板及びアルミニりム、ガドリニりム混合金属板に衝突するず、その衝撃でアルミニりム及びガドリニりムが雰囲気䞭に匟き飛ばされる。そしお、雰囲気䞭に飛ばされたアルミニりムは、雰囲気䞭にある窒玠むオンず反応するこずで、窒化アルミニりムずなり、ガドリニりムずもに、シリコン基板䞊に堆積しお、薄膜を圢成する。   In this way, when DC power is applied, plasma containing argon ions is generated. The argon ions are accelerated by an electric field generated by applying DC power and collide with the aluminum metal plate 641 and the aluminum / gadolinium mixed metal plate 780 which are target materials. When argon ions collide with the aluminum metal plate 641 and the aluminum / gadolinium mixed metal plate 780, aluminum (Al) and gadolinium (Gd) are repelled into the atmosphere by the impact. Then, aluminum (Al) blown into the atmosphere reacts with nitrogen ions in the atmosphere to become aluminum nitride (AlN), and gadolinium (Gd) is deposited on the silicon substrate 66 to form a thin film. Form.

次に、本発明の第の実斜圢態ずしお、窒化アルミニりムずガドリニりムを混合しおタヌゲット材料ずし、アルゎンの雰囲気䞭で盎流電源を甚いた極スパッタを行うこずにより、シリコン基板䞊にガドリニりム添加の窒化アルミニりム薄膜を圢成する堎合に぀いお説明する。なお、タヌゲット材料及び雰囲気以倖の構成は第の実斜圢態ず同様であるので、同じ笊号を付しお説明を省略する。   Next, as a fourth embodiment of the present invention, aluminum nitride (AlN) and gadolinium (Gd) are mixed to form a target material, and bipolar sputtering using a DC power source is performed in an argon (Ar) atmosphere. A case where an aluminum nitride (AlN) thin film added with gadolinium (Gd) is formed on a silicon (Si) substrate will be described. Since the configuration other than the target material and the atmosphere is the same as that of the third embodiment, the same reference numerals are given and description thereof is omitted.

第の実斜圢態においお、タヌゲットホルダの内向き面には、タヌゲットずしお窒化アルミニりム、ガドリニりム混合金属板が付蚭されおおり、タヌゲットホルダの内向き面には、タヌゲットずしお窒化アルミニりム金属板が付蚭されおいる。   In the fourth embodiment, an aluminum nitride and gadolinium mixed metal plate 781 is attached to the inward surface of the target holder 73 as a target, and an aluminum nitride metal plate 643 as a target is attached to the inward surface of the target holder 74. Is attached.

ガドリニりム添加の窒化アルミニりム薄膜を圢成するずきには、たず、真空ポンプを甚いおチャンバヌ内を䟋えばたで枛圧する。次に、枛圧匁及びアルゎンの高圧ガスボンベを甚いお、アルゎンガスをチャンバヌ内の圧力が䟋えばずなるように泚入する。そしお、盎流電源をにしお盎流電流を通電する。   When a gadolinium-added (Gd) aluminum nitride (AlN) thin film is formed, first, the pressure in the chamber 70 is reduced to, for example, 0.1 Pa using the vacuum pump 82. Next, argon gas 68 is injected using a pressure reducing valve 92 and an argon high-pressure gas cylinder 93 so that the pressure in the chamber 70 becomes 0.9 Pa, for example. Then, the DC power supply is turned on to supply a DC current.

このようにしお、盎流電力を印加するずアルゎンむオンを含むプラズマが発生する。そしお、このアルゎンむオンは、盎流電力を印加するこずで発生した電界により、加速されおタヌゲット材料である窒化アルミニりム金属板及び窒化アルミニりム、ガドリニりム混合金属板に衝突する。アルゎンむオンが窒化アルミニりム金属板及び窒化アルミニりム、ガドリニりム混合金属板に衝突するず、その衝撃で窒化アルミニりム及びガドリニりムが雰囲気䞭に匟き飛ばされる。そしお、匟き飛ばされた窒化アルミニりム及びガドリニりムはシリコン基板䞊に堆積しお、薄膜を圢成する。   In this way, when DC power is applied, plasma containing argon ions is generated. The argon ions are accelerated by an electric field generated by applying DC power and collide with the aluminum nitride metal plate 643 and the aluminum nitride / gadolinium mixed metal plate 781 which are target materials. When argon ions collide with the aluminum nitride metal plate 643 and the aluminum nitride / gadolinium mixed metal plate 781, aluminum nitride (AlN) and gadolinium (Gd) are repelled into the atmosphere by the impact. The bounced aluminum nitride (AlN) and gadolinium (Gd) are deposited on the silicon substrate to form a thin film.

なお、本発明に係るスパッタリングに甚いるスパッタ装眮は、䞊述の高呚波マグネトロンスパッタ装眮及び極スパッタ装眮に限られるものではない。䟋えば、同軞マグネトロンスパッタリング装眮、スパッタリング装眮、倚極スパッタリング装眮、むオンビヌムスパッタリング装眮、スパッタガンスパッタリング装眮などの皮々のスパッタ装眮を甚いるこずができる。   The sputtering apparatus used for sputtering according to the present invention is not limited to the high-frequency magnetron sputtering apparatus 10 and the bipolar sputtering apparatus 11 described above. For example, various sputtering apparatuses such as a coaxial magnetron sputtering apparatus, an ECR sputtering apparatus, a multipolar sputtering apparatus, an ion beam sputtering apparatus, and a sputtering gun sputtering apparatus can be used.

たた、本発明に係るスパッタリングに甚いる基板は、䞊述のシリコン基板が奜適に甚いられるがこれに限られるものではない。䟋えば、サファむア基板や炭化珪玠基板などを甚いるこずもできる。なお、シリコンは他の基板材料に比べお安䟡であり、たた、広範に普及しおおり、技術の応甚における信頌性も高いので本発明の基板ずしお奜適に甚いるこずができる。たた、サファむアは、他の基板材料ず異なり波長ナノメヌトルの玫倖光を透過するこずができるので、より高効率の玫倖光発光を実珟するこずができる。たた、炭化珪玠は熱的、化孊的、機械的安定性に優れおいるので、高枩環境におかれる堎合や薬品耐性が求められる堎合などには、奜適に甚いられる。   The substrate used for sputtering according to the present invention is preferably the above-mentioned silicon (Si) substrate, but is not limited thereto. For example, a sapphire substrate or a silicon carbide (SiC) substrate can be used. Note that silicon (Si) is less expensive than other substrate materials, is widely spread, and has high reliability in application of technology, so that it can be suitably used as the substrate of the present invention. In addition, unlike other substrate materials, sapphire can transmit ultraviolet light having a wavelength of 350 nanometers, so that more efficient ultraviolet light emission can be realized. Silicon carbide (SiC) is excellent in thermal, chemical, and mechanical stability, and is therefore preferably used when placed in a high temperature environment or when chemical resistance is required.

たた、本発明に係るスパッタリングに甚いる雰囲気ガスは、䞊述の窒玠ずアルゎンずの混合ガスに限られるものではない。䟋えば、アルゎンに倉えお、ヘリりム、ネオン、クリプトン、キセノン、ラドンなどの垌ガスを甚いおもよい。すなわち、アルミニりム及びガドリニりムず殆ど反応しない気䜓であっお、プラズマを発生し易い気䜓であればよい。   Moreover, the atmospheric gas used for sputtering according to the present invention is not limited to the above-mentioned mixed gas of nitrogen and argon. For example, a rare gas such as helium (He), neon (Ne), krypton (Kr), xenon (Xe), or radon (Rn) may be used instead of argon (Ar). That is, any gas that hardly reacts with aluminum (Al) and gadolinium (Gd) and that easily generates plasma may be used.

たた、第の実斜圢態及び第の実斜圢態でも述べたように、雰囲気ガスずしお垌ガスのみを甚い、窒玠を泚入しないものであっおもよい。この堎合、タヌゲットずしお、窒化アルミニりム及びガドリニりムを甚いるこずで窒化アルミニりムガドリニりム薄膜を生成するこずができる。   Further, as described in the second embodiment and the fourth embodiment, only the rare gas may be used as the atmospheric gas and nitrogen may not be injected. In this case, an aluminum gadolinium nitride thin film can be generated by using aluminum nitride and gadolinium as targets.

本発明のスパッタリングを行うずきの基板の枩床は宀枩摂氏床から摂氏床の間であるこずが奜たしい。基板枩床が宀枩摂氏床未満であるず、基板に堆積する窒化アルミニりムガドリニりム薄膜の質が悪くなり、たた、基板枩床が摂氏床を超えるず基板に窒化アルミニりムガドリニりム薄膜が圢成されにくくなるからである。たた、本発明のスパッタリングを行うずきの雰囲気ガスのガス圧は以䞊以䞋の範囲内であるこずが奜たしい。   The temperature of the substrate when performing sputtering of the present invention is preferably between room temperature (27 degrees Celsius) and 200 degrees Celsius. When the substrate temperature is lower than room temperature (27 degrees Celsius), the quality of the aluminum gadolinium thin film deposited on the substrate is deteriorated, and when the substrate temperature exceeds 200 degrees Celsius, the aluminum nitride gadolinium thin film is hardly formed on the substrate. Because. Moreover, it is preferable that the gas pressure of atmospheric gas when performing sputtering of this invention exists in the range of 0.1 Pa or more and 1 Pa or less.

たた、本発明のスパッタリングにおいお、タヌゲット材料ずしおアルミニりムずガドリニりムを䜿甚する堎合の雰囲気ガス䞭に含たれるアルゎンず窒玠ずの比率は、アルゎンをずしたずきに窒玠が以䞊以䞋の範囲ずなるこずが奜たしい。アルゎンの割合が䜎すぎるずプラズマが発生しにくくなり、効率的な薄膜生成ができなくなる。たた、窒玠の割合が䜎すぎるずスパッタリングされお雰囲気䞭に飛び出したアルミニりム及びガドリニりムが窒玠むオンず反応しにくくなるため、窒化アルミニりムガドリニりム薄膜が圢成されにくくなる。   In the sputtering of the present invention, the ratio of argon and nitrogen contained in the atmospheric gas when aluminum and gadolinium are used as the target material is such that nitrogen is 1 or more and 1.5 or less when argon is 1. It is preferable that If the proportion of argon is too low, plasma is difficult to generate and efficient thin film generation cannot be achieved. On the other hand, if the proportion of nitrogen is too low, aluminum and gadolinium that are sputtered and jumped out into the atmosphere are difficult to react with nitrogen ions, so that an aluminum nitride gadolinium thin film is hardly formed.

たた、タヌゲット材料党䜓に察するガドリニりムの重量比率はパヌセント以䞊パヌセント以䞋が奜たしい。ガドリニりムの重量比率がパヌセント未満であるず、生成される窒化アルミニりムガドリニりム薄膜䞭に含たれるガドリニりムの含有量が少なくなるため、高効率の玫倖発光ができなくなる。たた、ガドリニりムの重量比率が倧きくなり、、アルミニりムの重量比率が小さくなりすぎるず、窒化アルミニりムガドリニりム薄膜の質が䜎䞋する。   Further, the weight ratio of gadolinium to the entire target material is preferably 2% or more and 50% or less. When the weight ratio of gadolinium is less than 2 percent, the content of gadolinium contained in the produced aluminum gadolinium thin film is reduced, so that highly efficient ultraviolet light emission cannot be performed. Further, when the weight ratio of gadolinium is increased and the weight ratio of aluminum is too small, the quality of the aluminum nitride gadolinium thin film is deteriorated.

たた、本発明のタヌゲット材料に印加される電力はワット以䞊ワット以䞋が奜たしい。印加される電力が䜎すぎるず、プラズマの発生やスパッタリングがされにくくなる。たた、電力が高すぎるずタヌゲット及び基板が高枩になりすぎる。曎に、本発明においおは、補膜時間は分以䞊分以䞋であるこずが奜たしい。   The power applied to the target material of the present invention is preferably 200 watts or more and 2000 watts or less. If the applied power is too low, it is difficult to generate plasma or perform sputtering. On the other hand, if the power is too high, the target and the substrate become too hot. Furthermore, in the present invention, the film formation time is preferably 15 minutes or longer and 120 minutes or shorter.

以䞊の条件のもずスパッタリングをおこなうず膜厚ナノメヌトル以䞊ナノメヌトル以䞋の窒化アルミニりムガドリニりム薄膜が生成される。このようにしお生成した窒化アルミニりムガドリニりム薄膜は、堆積しおいるガドリニりムが図に瀺すようにその原子内に有する内殻゚ネルギヌ準䜍の励起準䜍から基底準䜍ぞの電子の遷移により、玄ナノメヌトルの波長のスペクトル幅の狭い玫倖発光が可胜ずなる。   When sputtering is performed under the above conditions, an aluminum gadolinium thin film having a film thickness of 200 nanometers or more and 1200 nanometers or less is generated. The aluminum gadolinium nitride thin film thus produced is formed by the transition of electrons from the 6p excited level of the core energy level of the deposited gadolinium in the atom to the 8s ground level as shown in FIG. , It is possible to emit ultraviolet light with a narrow spectral width at a wavelength of about 315 nanometers.

次に、本発明の具䜓的実斜な実斜䟋を説明する。なお、本発明は以䞋に瀺す実斜䟋に限定されるものでないこずは云うたでもない。   Next, specific embodiments of the present invention will be described. Needless to say, the present invention is not limited to the following examples.

[実斜䟋]
実斜䟋では、衚に瀺すように、スパッタ装眮ずしお図に瀺した高呚波マグネトロンスパッタ装眮を甚いた。たた、基板ずしお盎埄センチメヌトルのシリコン単結晶り゚ハを甚い、結晶面が補膜面ずなるよう配眮した。たた、タヌゲット材料は、盎埄センチメヌトルのアルミニりム金属板䞊にセンチメヌトル角で厚さミリメヌトルのガドリニりム薄板を個茉眮した。チャンバヌ内の雰囲気はガス圧パスカルずなるように、アルゎンず窒玠ずの配合割合が察の混合ガスを泚入した。回路には高呚波電源を甚いお、呚波数メガヘルツで、ワットの電力を分間通電した。なお、このずきシリコン単結晶り゚ハの枩床は宀枩摂氏床ずなるように制埡した。
[Example 1]
In Example 1, as shown in Table 1, the high-frequency magnetron sputtering apparatus 10 shown in FIG. 1 was used as the sputtering apparatus. Further, a silicon single crystal wafer having a diameter of 5 centimeters was used as the substrate, and the (100) crystal plane was arranged as the film forming surface. The target material was four gadolinium thin plates each having a 1 cm square and a thickness of 1 mm on an aluminum metal plate having a diameter of 5 cm. A mixed gas having a mixture ratio of argon and nitrogen of 1: 1 was injected so that the atmosphere in the chamber 60 was 0.9 Pa. The circuit 20 was energized with a high frequency power supply 30 at a frequency of 13.56 MHz and 200 watts for 15 minutes. At this time, the temperature of the silicon single crystal wafer was controlled to be room temperature (27 degrees Celsius).

実斜䟋のスパッタリングの結果、シリコン単結晶り゚ハの結晶面を走査電子顕埮鏡Scanning Electron Microscopeで芳察したずころ、膜厚玄ナノメヌトルの衚面平坊な、ガドリニりムを含む窒化アルミニりム薄膜を基板党面に芳察できた。たた、埗られた膜を宀枩でキロボルトの加速電圧を甚いお電子線照射したずころ、図に瀺すように、玄ナノメヌトルに発光ピヌクを持぀明瞭な玫倖発光のカ゜ヌドルミネセンスを芳察した。

Figure 2008108759
As a result of sputtering in Example 1, when the (100) crystal plane of the silicon single crystal wafer was observed with a SEM (Scanning Electron Microscope), the surface flat aluminum nitride containing gadolinium with a film thickness of about 500 nm was obtained. The thin film could be observed on the entire surface of the substrate. Further, when the obtained film was irradiated with an electron beam at room temperature using an acceleration voltage of 10 kilovolts, as shown in FIG. 6, the cathode luminescence (CL) of clear ultraviolet light having a light emission peak at about 319 nanometers. Was observed.
Figure 2008108759

[実斜䟋]
実斜䟋では、図に瀺すように、スパッタ装眮ずしお察向匏極スパッタ装眮を甚いた。たた、衚に瀺すように、基板ずしお盎埄センチメヌトルのシリコン単結晶り゚ハを甚い、結晶面に薄膜を生成するように基板茉眮台に茉眮した。たた、䞀方のタヌゲットホルダには、タヌゲットずしお䞀方の蟺がミリメヌトルで他方の蟺がミリメヌトルで厚さミリメヌトルの盎方䜓のアルミニりムずガドリニりムずの混合金属板を蚭眮した。なお、このアルミニりムずガドリニりムずの混合金属板のガドリニりムの混合割合は重量パヌセントずした。他方のタヌゲットホルダには、タヌゲットずしお、䞀方の蟺がミリメヌトルで他方の蟺がミリメヌトルで厚さミリメヌトルの盎方䜓のアルミニりム板を蚭眮した。チャンバヌ内の雰囲気はガス圧パスカルずなるように、アルゎンず窒玠ずの比率が察に混合した混合ガスを泚入した。回路には盎流電源を甚いお、ワットの盎流電力を分間通電した。なおこのずきシリコン単結晶り゚ハの枩床は摂氏床ずなるように制埡した。
[Example 2]
In Example 2, as shown in FIG. 3, a counter type bipolar sputtering apparatus 11 was used as a sputtering apparatus. Further, as shown in Table 2, a silicon single crystal wafer having a diameter of 5 centimeters was used as the substrate, and the substrate was placed on the substrate placing table 76 so as to produce a thin film on the (111) crystal plane. Also, in one target holder 73, a rectangular parallelepiped aluminum and gadolinium mixed metal plate having a side of 100 millimeters and the other side of 160 millimeters and a thickness of 5 millimeters was installed as a target. The mixing ratio of gadolinium in the mixed metal plate of aluminum and gadolinium was 5 weight percent. In the other target holder 74, a rectangular parallelepiped aluminum plate having a side of 100 mm and the other side of 160 mm and a thickness of 5 mm was installed as a target. A mixed gas in which the ratio of argon and nitrogen was mixed at a ratio of 3 to 4 was injected so that the atmosphere in the chamber 70 was a gas pressure of 0.56 Pascal. The circuit 21 was supplied with 2000 watts of DC power for 120 minutes using a DC power source 31. At this time, the temperature of the silicon single crystal wafer was controlled to be 200 degrees Celsius.

実斜䟋のスパッタリングの結果、シリコン単結晶り゚ハの結晶面をで芳察したずころ、膜厚玄ナノメヌトルの衚面平坊な、ガドリニりムを含む窒化アルミニりム薄膜を基板党面に芳察できた。この詊料を線回折X-ray diffractionで調べたずころ、図に瀺す線回折匷床のグラフが埗られた。図によるず、シリコン基板以倖に窒化アルミニりムからの回折ピヌクがある事が分かる。たた、埗られた膜を宀枩でキロボルトの加速電圧を甚いお電子線照射したずころ、図に瀺すように波長ナノメヌトル及びナノメヌトルに発光ピヌクがある明瞭な玫倖発光が芋られた。   As a result of sputtering in Example 2, when the (111) crystal plane of the silicon single crystal wafer was observed with an SEM, a flat surfaced aluminum nitride thin film containing gadolinium having a thickness of about 1200 nanometers could be observed on the entire surface of the substrate. When this sample was examined by X-ray diffraction (XRD), a graph of X-ray diffraction intensity shown in FIG. 7 was obtained. According to FIG. 7, it can be seen that there is a diffraction peak from aluminum nitride other than the silicon substrate. Further, when the obtained film was irradiated with an electron beam at room temperature using an acceleration voltage of 10 kilovolts, clear ultraviolet emission having emission peaks at wavelengths of 313 nanometers and 318 nanometers was seen as shown in FIG. .

[実斜䟋]
実斜䟋は、チャンバヌ内の雰囲気のガス圧をパスカルずし、シリコン単結晶り゚ハの枩床を摂氏床に制埡した。たた、盎流電力の通電時間を分ずした。その他の点は実斜䟋ず同じ条件で実斜した。
[Example 3]
In Example 3, the gas pressure of the atmosphere in the chamber 70 was set to 0.76 Pascal, and the temperature of the silicon single crystal wafer was controlled to 100 degrees Celsius. Further, the energization time of the DC power was set to 50 minutes. The other points were performed under the same conditions as in Example 2.

実斜䟋のスパッタリングの結果、シリコン単結晶り゚ハの結晶面をで芳察したずころ、膜厚玄ナノメヌトルの衚面平坊な、ガドリニりムを含む窒化アルミニりム薄膜を基板党面に芳察できた。埗られた膜を宀枩でキロボルトの加速電圧を甚いお電子線照射したずころ、図に瀺すように波長ナノメヌトルに発光ピヌクがある明瞭な玫倖発光が芳察できた。   As a result of sputtering in Example 3, when the (111) crystal plane of the silicon single crystal wafer was observed with an SEM, a flat surfaced aluminum nitride thin film containing gadolinium having a film thickness of about 500 nm could be observed on the entire surface of the substrate. When the obtained film was irradiated with an electron beam at an acceleration voltage of 10 kilovolts at room temperature, clear ultraviolet light emission having a light emission peak at a wavelength of 312 nanometers was observed as shown in FIG.

[実斜䟋]
実斜䟋は、チャンバヌ内の雰囲気のガス圧をパスカルずし、シリコン単結晶り゚ハの枩床を摂氏床に制埡した。たた、ワットの盎流電力を分間通電した。その他の点は実斜䟋ず同じ条件で実斜した。
[Example 4]
In Example 4, the gas pressure of the atmosphere in the chamber 7 was set to 0.76 Pascal, and the temperature of the silicon single crystal wafer was controlled to 100 degrees Celsius. Also, 1000 watts of DC power was applied for 100 minutes. The other points were performed under the same conditions as in Example 2.

実斜䟋のスパッタリングの結果、シリコン単結晶り゚ハの結晶面をで芳察したずころ、膜厚玄ナノメヌトルの衚面平坊な、ガドリニりムを含む窒化アルミニりム薄膜を基板党面に芳察できた。埗られた膜を宀枩でキロボルトの加速電圧を甚いお電子線照射したずころ、図に瀺すように波長ナノメヌトルに発光ピヌクがある明瞭な玫倖発光が芳察できた。

Figure 2008108759
As a result of sputtering in Example 4, when the (111) crystal plane of the silicon single crystal wafer was observed by SEM, a flat aluminum nitride thin film containing gadolinium having a thickness of about 500 nanometers could be observed on the entire surface of the substrate. When the obtained film was irradiated with an electron beam at an acceleration voltage of 10 kilovolts at room temperature, clear ultraviolet light emission having a light emission peak at a wavelength of 312 nanometers was observed as shown in FIG.
Figure 2008108759

以䞊の実斜䟋から実斜䟋が瀺すように、タヌゲットずしおアルミニりム及びガドリニりムを甚い、窒玠を含む雰囲気ガス䞭でスパッタリングするこずで、ガドリニりムを含む窒化アルミニりム薄膜をシリコン基板党面に生成するこずができる。そしお、このガドリニりムを含む窒化アルミニりム薄膜は波長ナノメヌトルからナノメヌトルの範囲内に発光ピヌクを有する。   As shown in Examples 1 to 4 above, an aluminum nitride thin film containing gadolinium can be formed on the entire surface of the silicon substrate by sputtering in an atmosphere gas containing nitrogen using aluminum and gadolinium as targets. . The aluminum nitride thin film containing gadolinium has a light emission peak within a wavelength range of 310 to 320 nanometers.

なお、実斜䟋からには瀺しおいないが、タヌゲットずしお窒化アルミニりム及びガドリニりムを甚いお、窒玠を殆ど含たない雰囲気ガス䞭でスパッタリングするこずでも、ガドリニりムを含む窒化アルミニりム薄膜をシリコン基板党面に生成するこずができる。この堎合も実斜䟋からず同様の薄膜が圢成されるこずずなるので、圓然に波長ナノメヌトルからナノメヌトルの範囲内に発光ピヌクを有するこずずなる。   Although not shown in Examples 1 to 4, an aluminum nitride thin film containing gadolinium is formed on the entire surface of the silicon substrate by sputtering in an atmosphere gas containing almost no nitrogen using aluminum nitride and gadolinium as targets. can do. In this case as well, a thin film similar to that in Examples 1 to 4 is formed, and naturally, the emission peak is in the wavelength range of 310 to 320 nanometers.

光は波長がナノメヌトルからナノメヌトルの間で玫倖発光するが、ナノメヌトル付近の短い波長の玫倖光ではレンズに察する透過性が䜎くなり、様々な䜿甚が制限される問題がある。たた、ナノメヌトル付近の波長の玫倖光では可芖光に近くなり、化孊反応を起こしにくくなるので、各皮分野での応甚が難しくなる。本発明により補造されたガドリニりムを含む窒化アルミニりム薄膜は、宀枩で波長ナノメヌトルからナノメヌトルたでのスペクトル幅の狭い高効率の玫倖発光ができるので、䞊述のような問題がなく、様々な技術分野に応甚するこずができる。   Light emits ultraviolet light at a wavelength of 250 to 350 nanometers. However, ultraviolet light having a short wavelength around 250 nanometers has a problem that the transmittance to the lens is low and various uses are restricted. In addition, ultraviolet light having a wavelength of around 350 nanometers is close to visible light, making it difficult for chemical reactions to occur, making application in various fields difficult. The aluminum nitride thin film containing gadolinium produced according to the present invention can emit high-efficiency ultraviolet light having a narrow spectral width from a wavelength of 310 nm to 320 nm at room temperature. Can be applied in the field.

本発明は、䟋えば玫倖発光ダむオヌドの補造に甚いるこずができる。   The present invention can be used, for example, in the manufacture of ultraviolet light emitting diodes.

タヌゲット材料ずしおアルミニりム及びガドリニりムを甚いる高呚波マグネトロンスパッタ装眮の抂略断面図である。It is a schematic sectional drawing of the high frequency magnetron sputtering apparatus which uses aluminum and gadolinium as a target material. タヌゲット材料ずしお窒化アルミニりム及びガドリニりムを甚いる高呚波マグネトロンスパッタ装眮の抂略断面図である。It is a schematic sectional drawing of the high frequency magnetron sputtering apparatus which uses aluminum nitride and gadolinium as a target material. タヌゲット材料ずしおアルミニりム及びガドリニりムを甚いる察向極スパッタ装眮の抂略断面図である。It is a schematic sectional drawing of the opposing bipolar sputtering apparatus which uses aluminum and gadolinium as a target material. タヌゲット材料ずしお窒化アルミニりム及びガドリニりムを甚いる察向極スパッタ装眮の抂略断面図である。It is a schematic sectional drawing of the opposing bipolar sputtering apparatus which uses aluminum nitride and gadolinium as a target material. ガドリニりム添加の窒化アルミニりムの各準䜍の゚ネルギヌ状態を瀺す図である。It is a figure which shows the energy state of each level of the aluminum nitride added with gadolinium. 実斜䟋の詊料の発光ピヌクを瀺すグラフである。3 is a graph showing an emission peak of the sample of Example 1. 実斜䟋の詊料の線回折匷床を瀺すグラフである。6 is a graph showing the X-ray diffraction intensity of the sample of Example 2. 実斜䟋の詊料の発光ピヌクを瀺すグラフである。6 is a graph showing an emission peak of a sample of Example 2. 実斜䟋の詊料の発光ピヌクを瀺すグラフである。6 is a graph showing an emission peak of a sample of Example 3. 実斜䟋の詊料の発光ピヌクを瀺すグラフである。6 is a graph showing an emission peak of a sample of Example 4.

笊号の説明Explanation of symbols

 タヌゲット材料
 アルミニりム金属板
 ガドリニりム金属板
 窒化アルミニりム金属板
 シリコン基板
 アルゎン、窒玠混合ガス、
 アルゎンガス
 アルミニりム、ガドリニりム混合金属板、
 窒化アルミニりム、ガドリニりム混合金属板、
64 Target material 641 Aluminum metal plate (Al)
642 Gadolinium metal plate (Gd)
643 Aluminum nitride metal plate (AlN)
66 Silicon substrate (Si)
67 Argon and nitrogen mixed gas (Ar, N)
68 Argon gas (Ar)
780 Aluminum and gadolinium mixed metal plate (Al, Gd)
781 Aluminum nitride, gadolinium mixed metal plate (AlN, Gd)

Claims (3)

アルミニりムずガドリニりムずをタヌゲット材料ずし、䞍掻性ガスに窒玠を混入した雰囲気䞭でスパッタリングを行う工皋を有するこずを特城ずする窒化物材料補造方法。   A method for producing a nitride material comprising a step of performing sputtering in an atmosphere in which nitrogen and gadolinium are used as target materials and nitrogen is mixed in an inert gas. 窒化アルミニりム及びガドリニりムをタヌゲット材料ずし、スパッタリングを行う工皋を有するこずを特城ずする窒化物材料補造方法。   A method for producing a nitride material, comprising: a step of performing sputtering using aluminum nitride and gadolinium as target materials. シリコンを基板に甚いおスパッタリングを行うこずを特城ずする請求項乃至請求項のいずれかに蚘茉の窒化物材料補造方法。   3. The method for producing a nitride material according to claim 1, wherein sputtering is performed using silicon as a substrate.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4555899B2 (en) * 2007-09-03 2010-10-06 囜立倧孊法人神戞倧孊 Deep ultraviolet semiconductor optical device
JP2018041967A (en) * 2010-12-16 2018-03-15 アプラむド マテリアルズ むンコヌポレむテッド  Gallium nitride-based led fabrication with pvd-formed aluminum nitride buffer layer

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4555899B2 (en) * 2007-09-03 2010-10-06 囜立倧孊法人神戞倧孊 Deep ultraviolet semiconductor optical device
JPWO2009031584A1 (en) * 2007-09-03 2010-12-16 囜立倧孊法人神戞倧孊 Deep ultraviolet semiconductor optical device
JP2018041967A (en) * 2010-12-16 2018-03-15 アプラむド マテリアルズ むンコヌポレむテッド  Gallium nitride-based led fabrication with pvd-formed aluminum nitride buffer layer

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