JPH1053491A - Method for forming PrF3 single crystal thin film - Google Patents
Method for forming PrF3 single crystal thin filmInfo
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- JPH1053491A JPH1053491A JP21119596A JP21119596A JPH1053491A JP H1053491 A JPH1053491 A JP H1053491A JP 21119596 A JP21119596 A JP 21119596A JP 21119596 A JP21119596 A JP 21119596A JP H1053491 A JPH1053491 A JP H1053491A
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- prf
- thin film
- substrate
- single crystal
- crystal thin
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Abstract
(57)【要約】
【課題】 従来成膜例のないＰｒＦ3 単結晶薄膜をＭＢ
Ｅ法により膜成長させて、結晶性の良好なＰｒＦ3 単結
晶薄膜を得る。
【解決手段】 ＰｒＦ3 を蒸発セル又は電子ビームによ
り加熱蒸発させて、ＬａＦ3 （０００１）基板又はアル
カリ土類金属フッ化物（１１１）基板３上にＰｒＦ3 単
結晶薄膜を成膜させる。基板温度は２００〜８５０℃、
ＰｒＦ3 の蒸気圧は５．０×１０-8〜１．０×１０-4Ｔ
ｏｒｒの範囲で膜成長させる。
【効果】 基板上に、結晶性の良いＰｒＦ3 単結晶薄膜
を成膜することができ、フッ化物結晶系ヘテロ多層構造
よりなる新規高性能光機能材料開発における大きな進展
が図れる。
PROBLEM TO BE SOLVED: To provide a PrF 3 single crystal thin film having no conventional film formation example by MB
The film is grown by the method E to obtain a PrF 3 single crystal thin film having good crystallinity. SOLUTION: PrF 3 is heated and evaporated by an evaporation cell or an electron beam to form a PrF 3 single crystal thin film on a LaF 3 (0001) substrate or an alkaline earth metal fluoride (111) substrate 3. The substrate temperature is 200 ~ 850 ℃,
The vapor pressure of PrF 3 is 5.0 × 10 −8 to 1.0 × 10 −4 T
The film is grown in the range of orr. [Effect] A PrF 3 single crystal thin film having good crystallinity can be formed on a substrate, and significant progress can be made in the development of a new high-performance optical functional material having a fluoride crystal based hetero multilayer structure.
Description
【０００１】[0001]
【発明の属する技術分野】本発明はＰｒＦ3 （フッ化プ
ラセオジム）単結晶薄膜の成膜方法に係り、特に分子線
エピタキシー法によりＬａＦ3 （０００１）基板又はア
ルカリ土類金属フッ化物（１１１）基板上にＰｒＦ3 単
結晶薄膜を膜成長させることにより高品質なＰｒＦ3 単
結晶薄膜を成膜する方法に関する。The present invention relates to a method for forming a single crystal thin film of PrF 3 (praseodymium fluoride), and more particularly to a LaF 3 (0001) substrate or an alkaline earth metal fluoride (111) substrate by a molecular beam epitaxy method. to a method of forming a high quality PrF 3 single crystal thin film by film growth a PrF 3 single crystal thin film thereon.
【０００２】[0002]
【従来の技術】従来、レーザ結晶材料としては、ＹＡＧ
等の酸化物系レーザ結晶が開発されているが、最近にな
ってフッ化物系レーザ結晶についての開発も進められる
ようになった。2. Description of the Related Art Conventionally, as a laser crystal material, YAG
Oxide-based laser crystals such as those described above have been developed, but recently development of fluoride-based laser crystals has also been advanced.
【０００３】また、フッ化物系単結晶薄膜については各
種光機能性材料としての開発も試みられており、これま
で、ＣａＦ2 単結晶薄膜の成膜については、いくつか報
告がなされている。例えば、Appl.phys.lett.62(21)(24
May 1993) P2616〜2618では、分子線エピタキシー（Ｍ
ＢＥ：Molecular Beam Epitaxy) 法により、ＣａＦ2基
板上にＥｒドープＣａＦ2 単結晶薄膜を成膜することが
記載されている。[0003] Further, development of a fluoride-based single crystal thin film as an optically functional material has been attempted, and several reports have been made on the formation of a CaF 2 single crystal thin film. For example, Appl.phys.lett.62 (21) ( 24
May 1993) In pages 2616 to 2618, molecular beam epitaxy (M
It describes that an Er-doped CaF 2 single crystal thin film is formed on a CaF 2 substrate by a BE (Molecular Beam Epitaxy) method.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、従来に
おいて、ＰｒＦ3 の単結晶薄膜の成膜は行われていな
い。ＰｒＦ3 単結晶薄膜の成膜が可能であるならば、従
来、ＣａＦ2 ベースで検討されていたフッ化物系結晶材
料を希土類元素を構成元素とする材料系に広げることが
でき、アップコンバージョンの高効率化を図る上で大き
な進展が得られるものと考えられる。However, a single crystal thin film of PrF 3 has not been conventionally formed. If a PrF 3 single crystal thin film can be formed, a fluoride-based crystal material, which had been conventionally studied based on CaF 2 , can be expanded to a material system containing a rare earth element as a constituent element. It is thought that significant progress can be made in improving efficiency.
【０００５】本発明は上記従来の実情に鑑みてなされた
ものであり、従来成膜例のないＰｒＦ3 単結晶薄膜をＭ
ＢＥ法により膜成長させることにより、結晶性の良好な
ＰｒＦ3 単結晶薄膜を成膜する方法を提供することを目
的とする。[0005] The present invention has been made in view of the above conventional circumstances, the PrF 3 single crystal thin film having no conventional film formation Example M
An object of the present invention is to provide a method for forming a PrF 3 single crystal thin film having good crystallinity by growing a film by a BE method.
【０００６】[0006]
【課題を解決するための手段】本発明のＰｒＦ3 単結晶
薄膜の成膜方法は、ＰｒＦ3 を蒸発セル又は電子ビーム
により加熱蒸発させて、ＬａＦ3 （０００１）基板又は
アルカリ土類金属フッ化物（１１１）基板上にＰｒＦ3
単結晶薄膜を成膜させる方法であって、該基板温度を２
００〜８５０℃、ＰｒＦ3 の蒸気圧を５．０×１０-8〜
１．０×１０-4Ｔｏｒｒの範囲で膜成長させることを特
徴とする。Means for Solving the Problems] PrF 3 film forming method of a single crystal thin film of the present invention, a PrF 3 by thermal evaporation by evaporation cell or electron beam, LaF 3 (0001) substrate or an alkaline earth metal fluoride PrF 3 on (111) substrate
A method for forming a single-crystal thin film, comprising:
00 to 850 ° C., the vapor pressure of PrF 3 is 5.0 × 10 −8 to
It is characterized in that a film is grown within a range of 1.0 × 10 −4 Torr.
【０００７】基板加熱温度２００〜８５０℃，ＰｒＦ3
蒸気圧５．０×１０-8〜１．０×１０-4Ｔｏｒｒの条件
下でＭＢＥ法によりＬａＦ3 （０００１）基板又はアル
カリ土類金属フッ化物（１１１）基板上に膜成長させる
ことにより、結晶性の良いＰｒＦ3 単結晶薄膜を成膜す
ることができる。Substrate heating temperature 200-850 ° C., PrF 3
By growing a film on a LaF 3 (0001) substrate or an alkaline earth metal fluoride (111) substrate by MBE under a condition of a vapor pressure of 5.0 × 10 −8 to 1.0 × 10 −4 Torr, A PrF 3 single crystal thin film having good crystallinity can be formed.
【０００８】[0008]
【発明の実施の形態】以下、図面を参照して本発明を詳
細に説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail with reference to the drawings.
【０００９】図１は、本発明のＰｒＦ3 単結晶薄膜の成
膜方法の実施に好適な成膜装置を示す模式図である。FIG. 1 is a schematic diagram showing a film forming apparatus suitable for carrying out the method for forming a PrF 3 single crystal thin film of the present invention.
【００１０】図中、１は真空チャンバーであり、内部に
加熱ヒータ２，メインシャッター４，シャッター５を有
する蒸発セル（クヌーセンセル）６及び冷却用の液体窒
素の供給系７を有する。In FIG. 1, reference numeral 1 denotes a vacuum chamber, which has therein a heating heater 2, a main shutter 4, an evaporation cell (Knudsen cell) 6 having a shutter 5, and a liquid nitrogen supply system 7 for cooling.
【００１１】ＰｒＦ3 単結晶薄膜の成膜に当っては、加
熱ヒータ２上にＬａＦ3 （０００１）基板又はアルカリ
土類金属フッ化物（１１１）基板３を載置すると共に、
蒸発セル６内に所定量のＰｒＦ3 の固体ソースを投入す
る。そして、加熱ヒータ２で該基板３を所定の温度に加
熱すると共に、蒸発セル６をヒータ加熱してＰｒＦ3を
蒸発させて真空チャンバー１内を所定のＰｒＦ3 蒸気圧
とする。その後、蒸発セル６のシャッター５及びメイン
シャッター４を開けて該基板３上にＰｒＦ3 の単結晶薄
膜を成長させる。In forming the PrF 3 single crystal thin film, a LaF 3 (0001) substrate or an alkaline earth metal fluoride (111) substrate 3 is placed on the heater 2 and
A predetermined amount of a solid source of PrF 3 is charged into the evaporation cell 6. Then, the substrate 3 is heated to a predetermined temperature by the heater 2, and the evaporation cell 6 is heated by the heater to evaporate PrF 3 , so that the inside of the vacuum chamber 1 has a predetermined PrF 3 vapor pressure. Thereafter, the shutter 5 and the main shutter 4 of the evaporation cell 6 are opened to grow a PrF 3 single crystal thin film on the substrate 3.
【００１２】なお、ＰｒＦ3 の蒸発は、蒸発セルによる
他、カーボン坩堝等の容器内のＰｒＦ3 固体ソースに電
子ビームを照射して加熱蒸発させるものであっても良
い。[0012] Incidentally, the evaporation of PrF 3, the other by evaporation cell, the PrF 3 solid source in the container, such as a carbon crucible may be one for heating vaporized by irradiation of electron beam.
【００１３】本発明においては、成膜に当り、ＬａＦ3
（０００１）基板又はアルカリ土類金属フッ化物（１１
１）基板の加熱温度を２００〜８５０℃とし、ＰｒＦ3
の蒸気圧を５．０×１０-8〜１．０×１０-4Ｔｏｒｒの
範囲とする。この基板温度及びＰｒＦ3 の蒸気圧の設定
条件は極めて重要であり、上記範囲をはずれる条件で
は、結晶性の良好なＰｒＦ3 単結晶薄膜を成膜すること
はできない。In the present invention, LaF 3 is used for film formation.
(0001) substrate or alkaline earth metal fluoride (11
1) The heating temperature of the substrate is 200 to 850 ° C., and PrF 3
Is in the range of 5.0 × 10 −8 to 1.0 × 10 −4 Torr. The setting conditions of the substrate temperature and the vapor pressure of PrF 3 are extremely important, and a PrF 3 single crystal thin film with good crystallinity cannot be formed under the conditions outside the above range.
【００１４】例えば、基板温度が２００℃未満では、ア
モルファス状となるか又は単結晶であっても結晶性の良
好な薄膜を形成し得ず、基板温度が８５０℃を超えると
単結晶であっても結晶性が悪くなる。また、ＰｒＦ3 蒸
気圧が５．０×１０-8ｔｏｒｒ未満でも、１．０×１０
-4ｔｏｒｒを超えても、結晶性の良好なＰｒＦ3 単結晶
薄膜の成膜は困難となる。For example, if the substrate temperature is less than 200 ° C., the film becomes amorphous or a single crystal cannot form a thin film having good crystallinity. If the substrate temperature exceeds 850 ° C., the substrate becomes a single crystal. Also has poor crystallinity. Further, even when the PrF 3 vapor pressure is less than 5.0 × 10 −8 torr, 1.0 × 10 −8
Even if the pressure exceeds -4 torr, it becomes difficult to form a PrF 3 single crystal thin film having good crystallinity.
【００１５】このようにしてＬａＦ3 （０００１）基板
又はアルカリ土類金属フッ化物（１１１）基板上に成膜
されたＰｒＦ3 単結晶薄膜は、異種材料のフッ化物結晶
を積層したヘテロ多層構造よりなる新規高性能光機能材
料としての用途が大いに期待される。The PrF 3 single crystal thin film formed on the LaF 3 (0001) substrate or the alkaline earth metal fluoride (111) substrate in this manner has a hetero multilayer structure in which fluoride crystals of different materials are laminated. The use as a new high-performance optical functional material is greatly expected.
【００１６】なお、本発明において、アルカリ土類金属
フッ化物（１１１）基板としては、ＭｇＦ2 、Ｃａ
Ｆ2 、ＳｒＦ2 、ＢａＦ2 基板等を用いるのが好まし
い。In the present invention, as the alkaline earth metal fluoride (111) substrate, MgF 2 , Ca
It is preferable to use an F 2 , SrF 2 , BaF 2 substrate or the like.
【００１７】[0017]
【実施例】以下に実施例を挙げて本発明をより具体的に
説明する。The present invention will be described more specifically with reference to the following examples.
【００１８】実施例１〜５ 図１に示す装置を用いてＰｒＦ3 単結晶薄膜の成膜を行
った。Examples 1 to 5 A single crystal PrF 3 thin film was formed using the apparatus shown in FIG.
【００１９】なお、基板としては下記のものを用いた。The following substrate was used.
【００２０】実施例１：ＬａＦ3 （０００１）基板 実施例２：ＭｇＦ2 （１１１）基板 実施例３：ＣａＦ2 （１１１）基板 実施例４：ＳｒＦ2 （１１１）基板 実施例５：ＢａＦ2 （１１１）基板 まず、真空チャンバー１内に、基板ホルダーにセットし
たＬａＦ3 （０００１）基板又はアルカリ土類金属フッ
化物（１１１）基板３を搬送し、加熱ヒータ２により該
基板３を６５０℃に加熱して基板表面を清浄状態にし
た。その後、基板３を表１〜５に示す温度に加熱した。
そして真空チャンバー１内が表１〜５に示すＰｒＦ3 蒸
気圧になるように、蒸発セル６内のＰｒＦ3 固体ソース
をヒータ加熱した。この状態で蒸発セル６のシャッター
５とメインシャッター４を開け、成膜を開始し、膜厚
０．１〜５．０μｍのＰｒＦ3 薄膜を形成した。Example 1: LaF 3 (0001) substrate Example 2: MgF 2 (111) substrate Example 3: CaF 2 (111) substrate Example 4: SrF 2 (111) substrate Example 5: BaF 2 ( 111) Substrate First, the LaF 3 (0001) substrate or the alkaline earth metal fluoride (111) substrate 3 set in the substrate holder is transported into the vacuum chamber 1, and the substrate 3 is heated to 650 ° C. by the heater 2. Thus, the substrate surface was cleaned. Thereafter, the substrate 3 was heated to the temperatures shown in Tables 1 to 5.
Then, the PrF 3 solid source in the evaporation cell 6 was heated with a heater so that the inside of the vacuum chamber 1 had the PrF 3 vapor pressure shown in Tables 1 to 5. In this state, the shutter 5 and the main shutter 4 of the evaporation cell 6 were opened to start film formation, and a PrF 3 thin film having a thickness of 0.1 to 5.0 μm was formed.
【００２１】得られたＰｒＦ3 薄膜について、反射高速
電子線回折（ＲＨＥＥＤ）により結晶の成長状態を調べ
ると共に、単結晶薄膜が得られたものについて、Ｘ線回
折により結晶性を調べ、結果を表１〜５に示した。な
お、結晶性は回折ピークの半値幅の狭いものを「良」、
該回折ピークの半値幅が比較的ブロードなものを「悪」
として評価した。For the obtained PrF 3 thin film, the crystal growth state was examined by reflection high-energy electron diffraction (RHEED), and for the single crystal thin film obtained, the crystallinity was examined by X-ray diffraction. 1 to 5. The crystallinity is defined as “good” when the half width of the diffraction peak is narrow,
If the half-width of the diffraction peak is relatively broad,
Was evaluated.
【００２２】[0022]
【表１】 [Table 1]
【００２３】[0023]
【表２】 [Table 2]
【００２４】[0024]
【表３】 [Table 3]
【００２５】[0025]
【表４】 [Table 4]
【００２６】[0026]
【表５】 [Table 5]
【００２７】表１〜５より、基板温度２００〜８５０
℃，ＰｒＦ3 蒸気圧５．０×１０-8〜１．０×１０-4Ｔ
ｏｒｒとする本発明のＭＢＥ成膜法によれば、結晶性の
良いＰｒＦ3 単結晶薄膜を成膜することができることが
明らかである。As shown in Tables 1 to 5, the substrate temperature was 200 to 850.
° C, PrF 3 vapor pressure 5.0 × 10 -8 to 1.0 × 10 -4 T
According to the MBE film forming method of the present invention having an orr, it is apparent that a PrF 3 single crystal thin film having good crystallinity can be formed.
【００２８】[0028]
【発明の効果】以上詳述した通り、本発明のＰｒＦ3 単
結晶薄膜の成膜方法によれば、ＬａＦ 3 （０００１）基
板又はアルカリ土類金属フッ化物（１１１）基板上に、
結晶性の良いＰｒＦ3 単結晶薄膜を効率的に成膜するこ
とができ、フッ化物結晶系ヘテロ多層構造よりなる新規
高性能光機能材料開発における大きな進展が図れる。As described in detail above, the PrF of the present inventionThreesingle
According to the method for forming a crystalline thin film, LaF Three(0001) group
On a plate or an alkaline earth metal fluoride (111) substrate,
PrF with good crystallinityThreeEfficient deposition of single crystal thin film
New, consisting of a fluoride crystal based hetero multilayer structure
Great progress can be made in the development of high-performance optical functional materials.
【図１】本発明のＰｒＦ3 単結晶薄膜の成膜方法の実施
に好適な成膜装置を示す模式図である。FIG. 1 is a schematic view showing a film forming apparatus suitable for carrying out a method for forming a PrF 3 single crystal thin film of the present invention.
１ 真空チャンバー ２ 加熱ヒータ ３ ＬａＦ3 （０００１）基板又はアルカリ土類金属フ
ッ化物（１１１）基板 ４ メインシャッター ５ シャッター ６ 蒸発セルREFERENCE SIGNS LIST 1 vacuum chamber 2 heater 3 LaF 3 (0001) substrate or alkaline earth metal fluoride (111) substrate 4 main shutter 5 shutter 6 evaporation cell
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 // Ｇ０２Ｂ 1/00 Ｇ０２Ｂ 1/00 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 6 Identification number Agency reference number FI Technical display location // G02B 1/00 G02B 1/00
Claims (1)
り加熱蒸発させて、ＬａＦ3 （０００１）基板又はアル
カリ土類金属フッ化物（１１１）基板上にＰｒＦ3 単結
晶薄膜を成膜させる方法であって、該基板温度を２００
〜８５０℃、ＰｒＦ3 の蒸気圧を５．０×１０-8〜１．
０×１０-4Ｔｏｒｒの範囲で膜成長させることを特徴と
するＰｒＦ3 単結晶薄膜の成膜方法。1. A method of forming a PrF 3 single crystal thin film on a LaF 3 (0001) substrate or an alkaline earth metal fluoride (111) substrate by heating and evaporating PrF 3 using an evaporation cell or an electron beam. The substrate temperature to 200
850 ° C., the vapor pressure of PrF 3 is 5.0 × 10 −8 −1.
A method for forming a PrF 3 single crystal thin film, comprising: growing a film in a range of 0 × 10 −4 Torr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21119596A JPH1053491A (en) | 1996-08-09 | 1996-08-09 | Method for forming PrF3 single crystal thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21119596A JPH1053491A (en) | 1996-08-09 | 1996-08-09 | Method for forming PrF3 single crystal thin film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH1053491A true JPH1053491A (en) | 1998-02-24 |
Family
ID=16601957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21119596A Withdrawn JPH1053491A (en) | 1996-08-09 | 1996-08-09 | Method for forming PrF3 single crystal thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH1053491A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005119952A (en) * | 2003-09-24 | 2005-05-12 | Hokushin Ind Inc | Fluoride single crystal for radiation detection and radiation detector |
| KR102000882B1 (en) * | 2018-11-13 | 2019-10-01 | 포항공과대학교 산학협력단 | Preparation method of high sensitivity LaF3 thin film, the high sensitivity LaF3 thin film prepared thereby and sensor comprising the same |
| CN116024659A (en) * | 2022-12-27 | 2023-04-28 | 北京工业大学 | A kind of preparation method of hexagonal phase tantalum pentoxide single crystal thin film |
-
1996
- 1996-08-09 JP JP21119596A patent/JPH1053491A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005119952A (en) * | 2003-09-24 | 2005-05-12 | Hokushin Ind Inc | Fluoride single crystal for radiation detection and radiation detector |
| KR102000882B1 (en) * | 2018-11-13 | 2019-10-01 | 포항공과대학교 산학협력단 | Preparation method of high sensitivity LaF3 thin film, the high sensitivity LaF3 thin film prepared thereby and sensor comprising the same |
| CN116024659A (en) * | 2022-12-27 | 2023-04-28 | 北京工业大学 | A kind of preparation method of hexagonal phase tantalum pentoxide single crystal thin film |
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