JP2014019940A - Method for controlling composition of complex oxide thin film and thin film growth apparatus - Google Patents
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本発明は、２種類以上の金属元素を含む複合酸化物薄膜組成の制御方法に関する。 The present invention relates to a method for controlling a composite oxide thin film composition containing two or more metal elements.
複合酸化物の薄膜を成長・形成する代表的な方法として、（ｉ）スパッタリング法、（ｉｉ）パルス・レーザー堆積（ＰＬＤ）法、（ｉｉｉ）化学気相成長(ＣＶＤ)法、（ｉｖ）分子線エピタキシー（ＭＢＥ）法、などがあり、このうち、（ｉｖ）のＭＢＥ法は一般に、（ｉ）〜（ｉｉｉ）の方法に比べて、結晶性が高く、高い精度で膜厚を制御した薄膜を作製できることが知られている。しかし、ＭＢＥ法では、化学量論組成をもつ複合酸化物を構成するそれぞれの金属を別々の蒸発源を用いて蒸発させて、酸化雰囲気下で、結晶基板上に供給するため、それぞれの金属フラックスの供給レートを制御する必要がある。例えば非特許文献１では、金属フラックスへの電子照射により発生する特性波長の光を定量化する方法（発光分光法）が開示されている。 As typical methods for growing and forming thin films of complex oxides, (i) sputtering, (ii) pulsed laser deposition (PLD), (iii) chemical vapor deposition (CVD), (iv) molecules There is a line epitaxy (MBE) method, and among these, the MBE method (iv) generally has a higher crystallinity than the methods (i) to (iii) and is a thin film whose film thickness is controlled with high accuracy. It is known that can be produced. However, in the MBE method, each metal constituting a composite oxide having a stoichiometric composition is evaporated using a separate evaporation source and supplied onto a crystal substrate in an oxidizing atmosphere. It is necessary to control the supply rate. For example, Non-Patent Document 1 discloses a method (emission spectroscopy) for quantifying light having a characteristic wavelength generated by electron irradiation of a metal flux.
非特許文献２では、金属フラックスに特性波長の光を照射してその吸収量からフラックスを定量化する方法が開示されている。 Non-Patent Document 2 discloses a method of quantifying a flux from the amount of absorption by irradiating a metal flux with light having a characteristic wavelength.
非特許文献３では、供給される金属毎に配置した水晶振動子式膜厚計への蒸着物の付着による振動数の変化を利用する方法が開示されている。 Non-Patent Document 3 discloses a method of using a change in frequency due to adhesion of a deposit to a quartz vibrator type film thickness meter disposed for each supplied metal.
従来の非特許文献１〜３においては、金属フラックスの供給レートを制御して薄膜の組成制御を行うようにしている。しかしながら、複合酸化物を構成する金属材料の化学量論的組成比を保つには、それぞれの金属材料の供給量を調整しながらチューニングしなければならず、煩雑でかつ膨大な時間がかかるという問題があった。 In the conventional non-patent documents 1 to 3, the composition control of the thin film is performed by controlling the supply rate of the metal flux. However, in order to maintain the stoichiometric composition ratio of the metal materials constituting the composite oxide, it is necessary to tune while adjusting the supply amount of each metal material, which is complicated and takes a lot of time. was there.
そこで本発明は、複合酸化物を構成する金属材料の組成をより簡易にかつ迅速に制御することが可能な複合酸化物組成の制御方法およびその制御方法により薄膜を作製することを可能とする薄膜成長装置を提供することを目的とする。 Therefore, the present invention provides a method for controlling a composite oxide composition capable of more easily and rapidly controlling the composition of a metal material constituting the composite oxide, and a thin film capable of producing a thin film by the control method. An object is to provide a growth apparatus.
上記の目的を達成するための複合酸化物薄膜組成の制御方法は、複数種の金属元素を含む複合酸化物薄膜組成の制御方法であって、前記複数種の金属元素を分子線エピタキシー（ＭＢＥ）法により反応させて前記複合酸化物薄膜の成長を行う際に、前記複数種の金属元素のうちの１種類の金属元素は、その金属元素単体の蒸気圧よりも、その金属の単純酸化物の蒸気圧の方が高いものを選択し、かつ、他の金属元素よりも過剰に供給するものである。 A method for controlling a composite oxide thin film composition for achieving the above object is a method for controlling a composite oxide thin film composition containing a plurality of types of metal elements, wherein the plurality of types of metal elements are converted into molecular beam epitaxy (MBE). When the composite oxide thin film is grown by reacting by the method, one kind of metal element of the plurality of kinds of metal elements is more than the vapor pressure of the metal element alone, of the simple oxide of the metal. A material having a higher vapor pressure is selected and supplied in excess of other metal elements.
ここで、前記１種類の金属元素は、Ｓｃ,Ｖ,Ｇｅ,Ｍｏ,Ｒｕ,Ｐｄ,Ｗ,Ｒｅのいずれかとしてよい。 Here, the one type of metal element may be any of Sc, V, Ge, Mo, Ru, Pd, W, and Re.
前記他の金属元素は、Ｓｃ,Ｖ,Ｇｅ,Ｍｏ,Ｒｕ,Ｐｄ,Ｗ,Ｒｅ以外の任意の元素、例えば、Ｌａ,Ｐｒ,Ｎｄ,Ｓｍなどがある。 The other metal element includes any element other than Sc, V, Ge, Mo, Ru, Pd, W, and Re, for example, La, Pr, Nd, and Sm.
上記の目的を達成するための本発明には、上記複合酸化物薄膜組成の制御方法により薄膜を作製することを可能にする薄膜成長装置が含まれる。 The present invention for achieving the above object includes a thin film growth apparatus that makes it possible to produce a thin film by the method for controlling the composite oxide thin film composition.
本発明によれば、複合酸化物を構成する金属材料の組成をより簡易にかつ迅速に制御することができる。 According to the present invention, the composition of the metal material constituting the composite oxide can be controlled more easily and quickly.
以下、本実施例の薄膜成長装置における複合酸化物薄膜組成の制御方法について説明する。この制御方法では、真空中で、ＭＢＥ法を利用して複数の種類の金属元素からなる複合酸化物の組成を制御して薄膜を作製する例について具体的に説明する。 Hereinafter, a method for controlling the composite oxide thin film composition in the thin film growth apparatus of this example will be described. In this control method, an example in which a thin film is manufactured by controlling the composition of a composite oxide composed of a plurality of types of metal elements using an MBE method in a vacuum will be specifically described.
[複合酸化物薄膜組成の制御方法]
この実施例では、２種類の金属元素をＭ(１),Ｍ(２)で表しており、Ｍ(１),Ｍ(２)からなる複合酸化物Ｍ(１) Ｍ(２)Ｏ３の薄膜を結晶基板上に作製する場合を想定する。この場合に、Ｍ(１)とＭ(２)の量を１：１の比率で供給するときには、下記の反応式（１）に従って反応が進行する。
Ｍ(１)＋Ｍ(２)＋(ｘ/２)Ｏ2＝Ｍ(１)Ｍ(２)Ｏ３＋[(ｘ-３)/２]Ｏ２↑ （１）
[Control method of composite oxide thin film composition]
In this embodiment, two kinds of metal elements M (1), are expressed on M (2), M (1 ), M complex oxide consisting of (2) M (1) M (2) of the O 3 Assume that a thin film is formed on a crystal substrate. In this case, when the amounts of M (1) and M (2) are supplied at a ratio of 1: 1, the reaction proceeds according to the following reaction formula (1).
M (1) + M (2) + (x / 2) O 2 = M (1) M (2) O 3 + [(x−3) / 2] O 2 ↑ (1)
一方、Ｍ(１)とＭ(２)の量が１：１の比率で供給されないとき、例えば、M(２)が過剰に供給されるときは、下記の反応式（２）に従って反応が進行する。
Ｍ(1)＋(1+δ)Ｍ(２)＋(ｘ/２)Ｏ2＝Ｍ(１)Ｍ(２)Ｏ３＋δＭ(２)Ｏy＋[(ｘ-３-δｙ)/２]Ｏ２↑ （２）
On the other hand, when the amounts of M (1) and M (2) are not supplied at a ratio of 1: 1, for example, when M (2) is supplied excessively, the reaction proceeds according to the following reaction formula (2). To do.
M (1) + (1 + δ) M (2) + (x / 2) O 2 = M (1) M (2) O 3 + δM (2) Oy + [(x−3−δy) / 2] O 2 ↑ (2)
反応式（２）では、Ｍ(１),Ｍ(２)からなる所望の複合酸化物Ｍ(１) Ｍ(２)Ｏ３が生成されることになるが、反応式（２）に示すように、不純物であるδＭ(２)Ｏyが生成されるため、作製される薄膜の品質が著しく低下する。 In Scheme (2), M (1), M desired composite oxide of (2) M (1) M (2) is O 3 will be produced, as shown in Scheme (2) In addition, since the impurity δM (2) Oy is generated, the quality of the thin film to be manufactured is significantly lowered.
ところが、反応式（２）において、過剰に供給するＭ(２)を例えばＳｃ（スカンジウム）とし、成膜温度と成長速度とを適切に設定した場合には、下記の反応式（３）に従って反応が進行する。
Ｍ(1)＋(1+δ)Ｓｃ＋(ｘ/２)Ｏ2＝Ｍ(１)ＳｃＯ３＋（δ/２）Ｓｃ２Ｏ３↑＋[(ｘ-３-３δ/２)/２]Ｏ２↑ （３）
However, in the reaction formula (2), when M (2) supplied excessively is, for example, Sc (scandium) and the film formation temperature and the growth rate are appropriately set, the reaction is performed according to the following reaction formula (3). Progresses.
M (1) + (1 + δ) Sc + (x / 2) O 2 = M (1) ScO 3 + (δ / 2) Sc 2 O 3 ↑ + [(x−3−3δ / 2) / 2] O 2 ↑ (3)
反応式（３）では、不純物であるＳｃ２Ｏ３が気体となり、基板から再蒸発する。そして、組成が適切に調整された所望の複合酸化物Ｍ(１)ＳｃＯ３（この場合、Ｍ(２)＝Ｓｃ）が生成される。これは、反応式（３）において、供給されたＳｃのうち過剰なＳｃも酸化されて不純物であるＳｃ２Ｏ３となるが、この不純物のＳｃ２Ｏ３の蒸気圧が高いために、成膜用基板からＳｃ２Ｏ３が再蒸発するためである。 In the reaction formula (3), Sc 2 O 3 as an impurity becomes a gas and re-evaporates from the substrate. Then, a desired composite oxide M (1) ScO 3 (in this case, M (2) = Sc) whose composition is appropriately adjusted is generated. This is because, in the reaction formula (3), excessive Sc in the supplied Sc is also oxidized to become Sc 2 O 3 as an impurity, but the vapor pressure of Sc 2 O 3 as the impurity is high, so This is because Sc 2 O 3 re-evaporates from the film substrate.
この観点から、本実施例では、金属元素単体の蒸気圧よりも単純酸化物の蒸気圧が高い元素をＭ(２)として採用する。この具体的な例を表１に示す。 From this viewpoint, in this embodiment, an element having a vapor pressure of a simple oxide higher than that of a single metal element is adopted as M (2) . A specific example of this is shown in Table 1.
表１は、金属元素単体の蒸気圧よりも単純酸化物の蒸気圧が高い元素の例を示す表である。 Table 1 is a table showing examples of elements having a vapor pressure of a simple oxide higher than that of a single metal element.
表１では、元素の一例として、Ｓｃ,Ｖ,Ｇｅ,Ｍｏ,Ｒｕ,Ｐｄ,Ｗ,Ｒｅの場合を例示し、当該元素に対応する各単純酸化物が、それぞれＳｃ２Ｏ３,Ｖ２Ｏ５,ＧｅＯ２,ＭｏＯ３,ＲｕＯ４,ＰｄＯ,ＷＯ３,Ｒｅ２Ｏ７となる場合を想定している。この例では、単純酸化物の蒸気圧は元素単体の蒸気圧よりも高くなるので、元素の蒸気圧が10-4 Torrとなるときの温度Ｄ１は、単純酸化物の蒸気圧が10-4 Torrとなるときの温度Ｄ３よりも高くなる。さらにこの例では、元素の蒸気圧が10-8 Torrとなるときの温度Ｄ２も、温度Ｄ３より高くなる。すなわち、表１では、Ｄ１＞Ｄ２＞Ｄ３を満足する。例えば、Ｓｃの場合、Ｄ１＝1002℃、Ｄ２＝714℃、Ｄ３＝400℃となる。 In Table 1, the case of Sc, V, Ge, Mo, Ru, Pd, W, Re is illustrated as an example of the element, and each simple oxide corresponding to the element is Sc 2 O 3 , V 2 O, respectively. 5 , GeO 2 , MoO 3 , RuO 4 , PdO, WO 3 , Re 2 O 7 are assumed. In this example, the simple vapor pressure of the oxide is higher than the vapor pressure of the single element, the temperature D1 at which the vapor pressure of the element is 10 -4 Torr, the vapor pressure of the simple oxide 10 -4 Torr It becomes higher than the temperature D3 when Furthermore, in this example, the temperature D2 when the vapor pressure of the element is 10 −8 Torr is also higher than the temperature D3. That is, in Table 1, D1>D2> D3 is satisfied. For example, in the case of Sc, D1 = 1002 ° C., D2 = 714 ° C., and D3 = 400 ° C.
なお、表１において、各元素の単純酸化物の蒸気圧は、その元素単体の蒸気圧よりも高くなるが、一般に、元素単体は、その元素からなる単純酸化物の蒸気圧よりも蒸気圧が高いことが知られている。あるいは、単純酸化物の蒸発温度に達する以前に、単純酸化物が分解してしまうことが知られている。 In Table 1, the vapor pressure of the simple oxide of each element is higher than the vapor pressure of the element alone. In general, the vapor pressure of the element simple substance is higher than the vapor pressure of the simple oxide of the element. It is known to be expensive. Alternatively, it is known that the simple oxide decomposes before reaching the evaporation temperature of the simple oxide.
次に、反応式（３）において、Ｍ(１)を、Ｌａ,Ｐｒ,Ｎｄ,Ｓｍのいずれかとしたときに、例えばＬａＡｌＯ３基板の温度を６５０−７００℃として、ＬａＡｌＯ３基板上にＭＢＥ法により薄膜成長を行った場合のＸ線回析パターンについて図１を参照して説明する。 Next, when M (1) is any one of La, Pr, Nd, and Sm in the reaction formula (3), for example, the temperature of the LaAlO 3 substrate is set to 650-700 ° C., and the MBE method is performed on the LaAlO 3 substrate. An X-ray diffraction pattern when a thin film is grown by the method will be described with reference to FIG.
図１は、Ｓｃ過剰条件下で成長した複合酸化物であるＭ(１)ＳｃＯ３薄膜（Ｍ(１)＝Ｌａ,Ｐｒ,Ｎｄ,Ｓｍ)のＸ線回折パターンの例を説明するための図である。なお、図１では、横軸は回析角（度）、縦軸はＸ線回析強度（カウント／秒）を表してある。 FIG. 1 is a diagram for explaining an example of an X-ray diffraction pattern of a M (1) ScO 3 thin film (M (1) = La, Pr, Nd, Sm), which is a complex oxide grown under an excessive Sc condition. It is. In FIG. 1, the horizontal axis represents the diffraction angle (degree), and the vertical axis represents the X-ray diffraction intensity (count / second).
図１に示すように、Ｘ線回析パターンは、４種類のＭ(１)ＳｃＯ３（Ｍ(１)＝Ｌａ,Ｐｒ,Ｎｄ,Ｓｍ)のパターンがある。各パターンでは、ＬａＡｌＯ３基板に由来するピーク（該当するピークの右側に「ＬａＡｌＯ３基板」と示してある。）と、エピタキシャル成長したＭ(１)ＳｃＯ３薄膜に由来するピークとが存在している。換言すれば、それら以外のピーク、すなわち、不純物相のピークは確認することができない。このことは、金属組成のチューニングに高い技術を要するため普及が限定的であったＭＢＥ法において、酸化物自体の蒸気圧が高い金属元素を含む場合には、格段に組成調節が容易となることを示している。 As shown in FIG. 1, the X-ray diffraction patterns include four types of M (1) ScO 3 (M (1) = La, Pr, Nd, Sm) patterns. In each pattern, there are a peak derived from the LaAlO 3 substrate (shown as “LaAlO 3 substrate” on the right side of the corresponding peak) and a peak derived from the epitaxially grown M (1) ScO 3 thin film. . In other words, any other peak, that is, the peak of the impurity phase cannot be confirmed. This means that, in the MBE method, which requires high technology to tune the metal composition, the spread of the metal composition is limited, and when the oxide itself contains a metal element having a high vapor pressure, the composition can be remarkably adjusted. Is shown.
以上説明したように、本実施例によれば、複数種の金属元素Ｍ(１),Ｍ(２)をＭＢＥ法により反応させて複合酸化物薄膜の成長を行う際に、Ｍ(２)として、Ｍ(２)の単純酸化物の蒸気圧がＭ(２)の蒸気圧よりも高いものを選択し、かつ、Ｍ(２)をＭ(１)よりも過剰に供給する。この場合、単純純酸化物は、気体となって基板から蒸発して不純物が取り除かれるため、適切な組成を有する複合酸化物を自動的に生成することができる。したがって、複合酸化物を構成する金属材料の組成をより簡易にかつ迅速に制御することができる。 As described above, according to this example, when a composite oxide thin film is grown by reacting a plurality of kinds of metal elements M (1) and M (2) by the MBE method, M (2) , the vapor pressure of a simple oxide of M (2) selects a higher than the vapor pressure of the M (2), and excess supply than M (1) to M (2). In this case, since the simple pure oxide becomes a gas and is evaporated from the substrate to remove impurities, a complex oxide having an appropriate composition can be automatically generated. Therefore, the composition of the metal material constituting the composite oxide can be controlled more easily and quickly.
なお、上記実施例では、ゲート絶縁体など、誘電体としての応用が期待されるＳｃを含む複合酸化物薄膜の成長を例にとって説明したが、他の元素を含む複合酸化膜の成長に適用してもよい。例えば、良導体であり、かつ酸化物エレクトロニクスにおいて電極としての応用が期待されるＳｒＲｕＯ３（酸化物の蒸気圧が高いＲｕを含むもの。例えば、G. Koster et al., "Dependence of the electronic structure of SrRuO3 and its degree of correlation on cation off-stoichiometry," Phys. Rev. B 76 (2007) 075126-1〜6を参照）の成長や、Ｓｒ２ＰｄＯ４（酸化物の蒸気圧が高いPdを含む。）の成長などに適用することも可能である。 In the above embodiment, the growth of a composite oxide thin film containing Sc, which is expected to be applied as a dielectric, such as a gate insulator, has been described as an example. However, the present invention is applied to the growth of a composite oxide film containing other elements. May be. For example, SrRuO 3 which is a good conductor and is expected to be applied as an electrode in oxide electronics (including Ru having a high vapor pressure of oxide. For example, G. Koster et al., “Dependence of the electronic structure of SrRuO3 and its degree of correlation on cation off-stoichiometry, "Phys. growth or Rev. B 76 (2007) see 075126-1～6), including Pd is high vapor pressure of Sr 2 PdO 4 (oxides. It is also possible to apply to the growth of).
また、上記実施例の金属元素Ｍ(１),Ｍ(２)、ＬａＡｌＯ３基板を用いることは、複合酸化物を得るための一方策に過ぎない。単純酸化物を蒸発させて適切な組成を有する複合酸化物を得るためのいかなる他の公知の構成も利用され得る。 In addition, the use of the metal elements M (1) , M (2) and LaAlO 3 substrate of the above embodiment is only one measure for obtaining the composite oxide. Any other known configuration for evaporating the simple oxide to obtain a composite oxide having the proper composition can be utilized.
Claims (4)
前記複数種の金属元素を分子線エピタキシー（ＭＢＥ）法により反応させて前記複合酸化物薄膜の成長を行う際に、前記複数種の金属元素のうちの１種類の金属元素は、その単純酸化物の蒸気圧の方が元素の蒸気圧よりも高いものを選択し、かつ、他の金属元素よりも過剰に供給する
ことを特徴とする複合酸化物薄膜組成の制御方法。 A method for controlling a composite oxide thin film composition containing a plurality of types of metal elements,
When the composite oxide thin film is grown by reacting the plurality of types of metal elements by a molecular beam epitaxy (MBE) method, one type of the metal elements is a simple oxide. A method for controlling a composite oxide thin film composition, wherein the vapor pressure of the element is selected to be higher than the vapor pressure of the element and is supplied in excess of other metal elements.
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