JPH04170396A - Production of thin film of lithium niobate single crystal - Google Patents
Production of thin film of lithium niobate single crystalInfo
- Publication number
- JPH04170396A JPH04170396A JP29178390A JP29178390A JPH04170396A JP H04170396 A JPH04170396 A JP H04170396A JP 29178390 A JP29178390 A JP 29178390A JP 29178390 A JP29178390 A JP 29178390A JP H04170396 A JPH04170396 A JP H04170396A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- single crystal
- thin film
- linbo3
- sapphire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 35
- 239000010409 thin film Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title 1
- 239000000758 substrate Substances 0.000 claims abstract description 50
- 238000004544 sputter deposition Methods 0.000 claims abstract description 21
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 13
- 239000010980 sapphire Substances 0.000 claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910003327 LiNbO3 Inorganic materials 0.000 abstract description 16
- 238000001552 radio frequency sputter deposition Methods 0.000 abstract description 2
- 229910012463 LiTaO3 Inorganic materials 0.000 abstract 2
- 229910002370 SrTiO3 Inorganic materials 0.000 abstract 2
- 239000008246 gaseous mixture Substances 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 1
- 239000010408 film Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010897 surface acoustic wave method Methods 0.000 description 2
- 102000014824 Crystallins Human genes 0.000 description 1
- 108010064003 Crystallins Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は光関連デバイス及び弾性表面波（ＳＡＷ）デバ
イスとして好適なＬＩＮｂＯ，単結晶薄膜の製造方法に
関するものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for manufacturing a LINbO single crystal thin film suitable for optical-related devices and surface acoustic wave (SAW) devices.
（従来の技術）
ＬｉＮｂＯｚ単結晶は高いキュリー温度を有する強誘電
体であり、その大きな電気機械結合定数、電気光学効果
、非線形光学効果などにおいて非常に優れた性質を有し
ており、現在最も広範に研究されており、かつ光学素子
材料として有望視されている物質のうちの一つである。(Prior art) LiNbOz single crystal is a ferroelectric material with a high Curie temperature, and has excellent properties such as a large electromechanical coupling constant, electro-optic effect, and nonlinear optical effect, and is currently the most widely used. It is one of the substances that has been studied extensively and is considered promising as an optical element material.
近年の半導体技術の進歩による電子部品の集積化及び小
型化に伴い、強誘電体素子も小型化、薄膜化が進みつつ
あり、ＬＩＮｂＯｉ単結晶に関しても薄膜化の需要は強
く、数多くの研究が成されてきている。Along with the integration and miniaturization of electronic components due to recent advances in semiconductor technology, ferroelectric elements are also becoming smaller and thinner. There is also a strong demand for thinner LINbOi single crystals, and a large amount of research has been carried out. It has been done.
従来ＬｉＮｂ０ｚ薄膜の製造方法として液相エピタキシ
ャル法、ＣＶＤ法、真空蒸着法、スパッタリング法等が
報告されているが、これらのうち、スパッタリング法が
最も一般的に用いられている。Conventionally, liquid phase epitaxial method, CVD method, vacuum evaporation method, sputtering method, etc. have been reported as methods for producing LiNb0z thin films, but among these, sputtering method is most commonly used.
従来のスパッタリング法によるＬｉＮｂＯ３薄膜の製造
では、基板温度として４０Ｏ℃以上の高温を用いており
、基板温度の昇温、降温に時間がかかり効率性が悪いと
いう工業化の上で重大な欠点が−あった。In the production of LiNbO3 thin films by the conventional sputtering method, a high temperature of 400°C or more is used as the substrate temperature, which has a serious drawback in terms of industrialization, as it takes time to raise and lower the substrate temperature, resulting in poor efficiency. Ta.
また、高い基板温度での製造は、基板とＷｉＭとの間の
熱膨張係数の違いによる歪の発生により配向性に悪影響
を与える可能性も考えられ、表面状態の悪化にも寄与す
る可能性があった。In addition, manufacturing at high substrate temperatures may adversely affect orientation due to the generation of distortion due to the difference in thermal expansion coefficient between the substrate and WiM, which may also contribute to deterioration of the surface condition. there were.
従来輻告されているスパッタリング法、例えば、Ｊ、Ａ
ｐｐｌ、Ｐｈｙｓ、、４０（１９６９）４２０によるＬ
ｉＮｂ０□＊ｉ＋ｉの合成においては、サファイヤＣ面
上では基板温度約３００℃以下で非晶ａｎ＋、約３８０
℃で多結晶層が得られている。また、Ａｐｐｌｉｅｄ
Ｐｈｙｓｉｃｓ Ｌｅｔｅｒｇ、、２４（１９７４）４
９Ｇで、基板温度５００℃以上で単結晶Ｉｌ！（（００
６）配向）が得られている。ここで、単結晶といわれて
いる膜は、格子定数が１．４１６ｎｍから１．４２４ｎ
臘で、バルクの文献値１．３８６ｎ−と大きく異なって
おり、決して、良好なものと言うことはできない。また
時開１１１５２−１２７５００では、サファイヤＲ面上
では基板温度３００℃から８００℃で、単結晶１［（（
３００）配向）が得られており、その際に、基板温度が
高い程結晶性が良くなるとされている。Conventionally reported sputtering methods, such as J, A
L by ppl, Phys, 40 (1969) 420
In the synthesis of iNb0□*i+i, on the sapphire C surface, amorphous an+, about 380
A polycrystalline layer is obtained at ℃. Also, Applied
Physics Letterg, 24 (1974) 4
Single crystal Il at 9G and substrate temperature of 500℃ or more! ((00
6) Orientation) is obtained. Here, the film that is said to be single crystal has a lattice constant of 1.416 nm to 1.424 nm.
This is significantly different from the bulk literature value of 1.386n-, and cannot be said to be good at all. In addition, for the time opening 11152-127500, the substrate temperature was 300°C to 800°C on the sapphire R surface, and the single crystal 1 [((
300) orientation), and it is said that the higher the substrate temperature, the better the crystallinity.
（発明が解決しようとする課Ｈ）
本発明は、上記の間麗を解決する為になされたものであ
り、従来用いられていた基板温度より低い基板温度（４
００℃未満）で単結晶ＬｉＮｂ０ｓｆｉｆｌ［を効率良
く製造することに関するものである。(Problem H to be solved by the invention) The present invention was made in order to solve the above-mentioned problem, and the present invention is made to solve the problem described above.
This invention relates to the efficient production of single-crystal LiNb0sfifl[at temperatures below 00°C].
（０！題を解決するための手段）
本発明は、サファイヤ基板、ＬｉＮｂＯ３基板、ＬｉＴ
ａＯ３基板、ＭｇＯ基板、シリコン基板または、ＳｒＴ
ｉＯ３基板上にスパッタ法でＬｉＮｂ０ｉ単結晶ＫＭ単
結晶部度として４００℃未満、圧力として０．００５０
ｔｏｒｒ以下でエピタキシャル成長させることを特徴と
するＬｉＮｂ０゜単結晶Ｓａの製造方法である。特に、
基板がサファイヤＣ面であり、成長させるＬｉＮｂＯ３
単結晶薄膜のＣ軸がサファイヤ基板と垂直であることを
特徴とするＬｉＮｂＯ３単結晶薄膜の製造方法、及び、
基板がサファイヤ８面であり、成長させるＬｉＮｂＯ３
単結晶薄膜の（０１２）面がサファイヤ基板と平行であ
ることを特徴とするＬｉＮｂＯ３単結晶薄膜の製造方法
である。(Means for Solving Problem 0!) The present invention is based on a sapphire substrate, a LiNbO3 substrate, a LiT
aO3 substrate, MgO substrate, silicon substrate or SrT
LiNb0i single crystal KM single crystal part temperature is less than 400℃ and pressure is 0.0050 on iO3 substrate by sputtering method.
This is a method for manufacturing LiNb 0° single crystal Sa, which is characterized by epitaxial growth at torr or less. especially,
The substrate is sapphire C-plane, and LiNbO3 is grown.
A method for producing a LiNbO3 single crystal thin film, characterized in that the C axis of the single crystal thin film is perpendicular to a sapphire substrate, and
The substrate is 8-sided sapphire, and LiNbO3 is grown.
This is a method for manufacturing a LiNbO3 single crystal thin film, characterized in that the (012) plane of the single crystal thin film is parallel to a sapphire substrate.
発明者らは、より結晶配向性の良いＬｉＮｂＯ３薄膜を
得るために圧力、ｒｆ−パワー、ガス組成、基板温度、
ターゲットと基板間の距離などのスパッタ条件を詳細に
調べた。その結果、種々のスパッタ条件を最適化し、圧
力を限界まで低くすることによって基板温度が４００℃
未満の領域でサファイヤＣ面上に単結晶ＬｉＮｂＯ３薄
膜（（００６）配向）、サファイヤＲ面上に単結晶Ｌｉ
ＮｂＯ３薄膜（（０１２）配向）が得られることを見い
だした。具体例としては、圧力は放電が生じる範凹内で
低い方が良く、０．００５０ｔ６ｒｒ以下が必要で特に
０．０００１ｔｏｒｒから０．００５０ｔｏｒｒまでが
好ましい。スパッタ出力は低すぎない方が良く、例えば
高周波スパッタリング法では、ｒｆ−パワーとして８０
ｗ以上が必要で特に、 ｔｏｏｗから４００ｗの範囲
が好ましい、酸票ガスの割合は大きい領域が望ましく、
特に３０ｖａ１％以上が好ましい、基板温度は、４００
℃未満であることが必要で、特に２５０℃〜４００℃未
満が好ましい、成膜速度は、０．５から２．５ｎ■／ｓ
ｉｎであった。In order to obtain a LiNbO3 thin film with better crystal orientation, the inventors investigated various changes in pressure, RF power, gas composition, substrate temperature,
The sputtering conditions, such as the distance between the target and the substrate, were investigated in detail. As a result, by optimizing various sputtering conditions and lowering the pressure to the limit, we were able to reduce the substrate temperature to 400°C.
Single-crystal LiNbO3 thin film ((006) orientation) on the sapphire C-plane and single-crystal LiNbO3 thin film ((006) orientation) on the sapphire R-plane in the area below
It has been found that a NbO3 thin film ((012) orientation) can be obtained. As a specific example, it is better for the pressure to be low within the range where discharge occurs, and it is necessary to be 0.0050 t6rr or less, and particularly preferably from 0.0001 torr to 0.0050 torr. It is better that the sputtering power is not too low; for example, in the high frequency sputtering method, the rf-power is 80
W or more is required, in particular, a range from too to 400 W is preferable, and a large proportion of acid gas is desirable.
In particular, the substrate temperature is preferably 30va 1% or more, 400
It is necessary that the temperature is lower than ℃, particularly preferably 250℃ to 400℃, and the film forming rate is 0.5 to 2.5n/s.
It was in.
また、この温度領域で得られるＬｉＮｂＯ３薄躾は、格
子定数もバルクの文献値１．３８６ｎ−と完全に一致し
、かつ、表面状態も鏝面で良好であり、結晶配向性も基
板温度５００℃以上で得られたものよりも優れているこ
とがわかり、よって本発明に到達しえた。In addition, the LiNbO3 thin film obtained in this temperature range has a lattice constant that completely matches the literature value of 1.386n- for the bulk, a good surface condition on the trowel surface, and a crystal orientation at a substrate temperature of 500°C. It was found that this was superior to that obtained above, and thus the present invention was achieved.
２５０℃〜４００℃の基板温度において、単結晶ＬｉＮ
ｂＯ３薄膜が形成された理由は定かではないが、スパッ
タリング法では、ヘテロエピタキシャル成長は、基板温
度とスパッタされて飛んでくる粒子の持つエネルギーと
成膜速度とに大きく影響されると考えられ、低い基板温
度でもスパッタされて飛んでくる粒子の持つエネルギー
がある程度大きく、かつ、成膜速度が適当であればヘテ
ロエピタキシャル成長が起こると考えられる。また、基
板温度が低い方が基板とＬｉＮｂＯ３Ｎ！との間の熱膨
張係数の違いに由来する歪の影響も小さく、よって、よ
り結晶配向性の良い腹が得られたのではないかと考えら
れる。At a substrate temperature of 250°C to 400°C, single crystal LiN
The reason why the bO3 thin film was formed is not clear, but in the sputtering method, heteroepitaxial growth is thought to be greatly influenced by the substrate temperature, the energy of sputtered particles, and the film formation rate. It is thought that heteroepitaxial growth will occur if sputtered particles have a certain amount of energy at a certain temperature and the film formation rate is appropriate. Also, the lower the substrate temperature, the better the substrate and LiNbO3N! It is thought that the effect of strain resulting from the difference in thermal expansion coefficient between the two is also small, and that this is why the antinode with better crystal orientation was obtained.
本発明の実施にあたって、スパッタ装置は、ＲＦ−スパ
ッタ装置でも、ＤＣ−スパッタ装置でも良く、その他マ
グネトロンスパッタ装置、エキシマレイザースパッタ装
置など、いずれのスパッタ装置でも良い。In carrying out the present invention, the sputtering device may be an RF sputtering device, a DC sputtering device, or any other sputtering device such as a magnetron sputtering device or an excimer laser sputtering device.
尚、単結晶ＷＩＮの結晶配向性の評価にはＸ線ロッキン
グカーブの半値幅（σ／ｄｅｇ）をもって行った。その
際、発散スリットは１／６＠のものを用い、受光スリッ
トは［１，３ｍｓのものを用いた。The crystal orientation of single crystal WIN was evaluated using the half width (σ/deg) of the X-ray rocking curve. At that time, a 1/6 @ divergence slit was used, and a 1.3 ms light receiving slit was used.
Ｘ線回折、及び、Ｘ線ロッキングカーブの測定には、リ
ガク製ＲＡＤ−Ａシリーズを用いた。Rigaku RAD-A series was used for X-ray diffraction and X-ray rocking curve measurements.
屈折率の測定にはエリプソメーター（情況光学製ＤＶＬ
−３６Ｌ）を用いた。To measure the refractive index, use an ellipsometer (DVL manufactured by Situ Kogaku Co., Ltd.)
-36L) was used.
以下に本発明についての実施例を示す。尚、この実施例
によってこの発明は限定されるものではない。Examples of the present invention are shown below. Note that the invention is not limited to this example.
（実施例） スパッタ装置は、通常の高周波スパッタ装置を用いた。(Example) A normal high frequency sputtering device was used as the sputtering device.
基板にはサファイヤＣ面を用いた。ターゲットとしてＬ
ｉＮｂＯ３の焼結体（，９９，９％以上）を用い、ター
ゲットと基板間の距離は、５．５ｃｍとした。スパッタ
前に系内を５ｘ １０−’ｔｏｒｒ以下まで減圧後、高
純度アルゴン（９９，９９９９Ｚ以上）と高純度酸素（
９９，９９９５％以上）の混合ガス（または、各ガス単
独）を系内に導入し、プレスパツタを圧力０．０１００
ｔｏｒｒで２０分間行った後に、スパッタを行った。基
板温度は４００℃未満とした。スパッタ条件の詳細は、
表１に示す。A sapphire C-plane was used as the substrate. L as a target
A sintered body of iNbO3 (99.9% or more) was used, and the distance between the target and the substrate was 5.5 cm. After reducing the pressure in the system to 5x 10-'torr or less before sputtering, high-purity argon (99,9999Z or more) and high-purity oxygen (
A mixed gas of 99,9995% or more (or each gas alone) is introduced into the system, and the press sputter is heated to a pressure of 0.0100.
Sputtering was performed after 20 minutes at torr. The substrate temperature was less than 400°C. For details on sputtering conditions, see
It is shown in Table 1.
実験したいずれの基板温度においても基板に対してＬｉ
ＮｂＯ５のＣ軸が垂直に配向した単結晶ＬｉＮｂ０゜薄
膜が得られた。 １＊られた躾の結晶配向性（σ／ｄｅ
ｇ）を表°に示す。また、Ｘ１１回折の結果（第１図）
から格子定数を計算すると１）８６ｎ畠となりバルク単
結
晶の値と完全に一致し、屈折率も２．２８９（ａｔ ６
３２．８ｎｍ）となりバルク単結晶の値と一致した。At all substrate temperatures tested, Li
A single crystal LiNb 0° thin film in which the C axis of NbO5 was vertically oriented was obtained. 1*Crystal orientation (σ/de
g) is shown in Table °. Also, the results of X11 diffraction (Fig. 1)
Calculating the lattice constant from
32.8 nm), which coincided with the value of the bulk single crystal.
（比較例）
基板温度５００℃において得られた膜の結果を比較例と
して表に付記した。本発明によって基板温度４００℃未
満で得られた鰻の方がはるかに優れた結晶配向性を示し
ており、また、格子定数、屈折率も文献値に良く一致し
ているのがわかる。(Comparative Example) The results of a film obtained at a substrate temperature of 500° C. are added to the table as a comparative example. It can be seen that the eel obtained according to the present invention at a substrate temperature of less than 400° C. shows much better crystal orientation, and the lattice constant and refractive index also agree well with the literature values.
（双下奈白）
（発明の効果）
以上のように本発明によると、従来法より低い基板温度
で従来法で得られていたものより優れた結晶配向性の単
結晶ＬｉＮｂＯ３薄膜の製造が可能であり、また、基板
の昇温、降温にかかる時間も大幅に短縮でき、従来法と
比ベニ業化する際に、効率良く単結晶ＬｉＮｂＯ３の製
造が行うことができ、極めて有効である。(Nahaku Soshita) (Effect of the invention) As described above, according to the present invention, it is possible to produce a single-crystal LiNbO3 thin film with better crystal orientation than that obtained by the conventional method at a lower substrate temperature than that obtained by the conventional method. In addition, the time required to raise and lower the temperature of the substrate can be significantly shortened, and when compared with conventional methods, single crystal LiNbO3 can be manufactured efficiently, which is extremely effective.
第１図は、上記実施例で得られたＷＩＨのＸ線回折パタ
ーンを示す図である。
特許出願人 旭化成工業株式会社FIG. 1 is a diagram showing the X-ray diffraction pattern of WIH obtained in the above example. Patent applicant: Asahi Kasei Industries, Ltd.
Claims (1)
基板、ＭｇＯ基板、シリコン基板または、ＳｒＴｉＯ＿
３基板上にスパッタ法でＬｉＮｂＯ＿３単結晶薄膜を基
板温度として４００℃未満、圧力として０．００５０ｔ
ｏｒｒ以下でエピタキシャル成長させることを特徴とす
るＬｉＮｂＯ＿３単結晶薄膜の製造方法。Sapphire substrate, LiNbO_3 substrate, LiTaO_3
Substrate, MgO substrate, silicon substrate or SrTiO_
3 Sputtering a LiNbO_3 single crystal thin film onto a substrate at a substrate temperature of less than 400°C and a pressure of 0.0050t.
A method for producing a LiNbO_3 single crystal thin film, characterized by epitaxial growth at or below orr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29178390A JPH04170396A (en) | 1990-10-31 | 1990-10-31 | Production of thin film of lithium niobate single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29178390A JPH04170396A (en) | 1990-10-31 | 1990-10-31 | Production of thin film of lithium niobate single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04170396A true JPH04170396A (en) | 1992-06-18 |
Family
ID=17773370
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29178390A Pending JPH04170396A (en) | 1990-10-31 | 1990-10-31 | Production of thin film of lithium niobate single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04170396A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022264426A1 (en) * | 2021-06-18 | 2022-12-22 | 日本電信電話株式会社 | Method for forming lithium niobate crystal thin film, and laminate including lithium niobate crystal thin film |
| WO2024075690A1 (en) * | 2022-10-05 | 2024-04-11 | 株式会社シンクロン | Homoepitaxial thin film, and manufacturing method and manufacturing apparatus thereof |
-
1990
- 1990-10-31 JP JP29178390A patent/JPH04170396A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022264426A1 (en) * | 2021-06-18 | 2022-12-22 | 日本電信電話株式会社 | Method for forming lithium niobate crystal thin film, and laminate including lithium niobate crystal thin film |
| WO2024075690A1 (en) * | 2022-10-05 | 2024-04-11 | 株式会社シンクロン | Homoepitaxial thin film, and manufacturing method and manufacturing apparatus thereof |
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