JP4378527B2 - Manufacturing method of optical fiber having a plurality of cores and manufacturing method of columnar glass body usable for manufacturing the same - Google Patents
Manufacturing method of optical fiber having a plurality of cores and manufacturing method of columnar glass body usable for manufacturing the same Download PDFInfo
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- JP4378527B2 JP4378527B2 JP2004027263A JP2004027263A JP4378527B2 JP 4378527 B2 JP4378527 B2 JP 4378527B2 JP 2004027263 A JP2004027263 A JP 2004027263A JP 2004027263 A JP2004027263 A JP 2004027263A JP 4378527 B2 JP4378527 B2 JP 4378527B2
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- 239000011521 glass Substances 0.000 title claims description 85
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000013307 optical fiber Substances 0.000 title claims description 15
- 150000002500 ions Chemical class 0.000 claims description 90
- 238000001237 Raman spectrum Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 230000001133 acceleration Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- OHENQANLQNOMAO-UHFFFAOYSA-N oxaborole Chemical group O1B=CC=C1 OHENQANLQNOMAO-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000007175 bidirectional communication Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000006854 communication Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 230000005469 synchrotron radiation Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/60—Silica-free oxide glasses
- C03B2201/62—Silica-free oxide glasses containing boron
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/34—Plural core other than bundles, e.g. double core
Description
本発明は柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本有する柱状ガラス体の製造方法及び複数のコアを有する光ファイバーの製造方法に関する。 The present invention relates to a method for producing a columnar glass body having a plurality of regions having a high heavy ion concentration continuous in the longitudinal direction of the columnar glass body, and a method for producing an optical fiber having a plurality of cores.
古来、ガラスはその美しさと耐久性により美術品あるいは美術品を兼ねた日用品として用いられてきた。それはガラスが本質的に透明であり、極めて平滑な表面を作ることが出来ることに由来している。現在はその新たな機能が見直され、光学的機能ガラスとして光集積回路、光ファイバー、フォトマスク等の分野で、電気・電子的機能ガラスとしてディスプレイ、透明導電性膜等の分野で実用化されている。 Traditionally, glass has been used as a work of art or a daily necessities that also serves as a work of art due to its beauty and durability. It stems from the fact that glass is essentially transparent and can produce extremely smooth surfaces. At present, the new functions are reviewed, and they are put into practical use in the fields of optical integrated circuits, optical fibers and photomasks as optical functional glasses, and in the fields of displays and transparent conductive films as electrical and electronic functional glasses. .
これまでイオン加速器は原子炉材料のイオン照射効果を解析して新規材料を開発するために、あるいは放射光発生装置の一部として利用されてきた。イオン加速器を利用して電気的に高速イオンを作り出し、これを材料中に打ち込む（インプランテーション）ことにより、材料の部分的改質を図ることができる。また、ガラスに他の原子をドープすることも提案されている（例えば、特許文献１及び２参照。）。
Until now, ion accelerators have been used to analyze the effects of ion irradiation on reactor materials to develop new materials or as part of synchrotron radiation generators. The material can be partially modified by creating fast ions electrically using an ion accelerator and implanting them into the material (implantation). It has also been proposed to dope other atoms into the glass (see, for example,
本発明は、イオン加速器を用いて重イオンを細いビームの状態で長い柱状ガラス体中の所定の位置に注入する技術を利用することによる、複数のコアを有する光ファイバーの製造方法並びにその製造に用い得る柱状ガラス体の製造方法を提供することを目的としている。 The present invention uses a technique for injecting heavy ions into a predetermined position in a long columnar glass body in a thin beam state using an ion accelerator, and a method for manufacturing an optical fiber having a plurality of cores. It aims at providing the manufacturing method of the columnar glass body to obtain.
本発明者は、上記の目的を達成するために鋭意検討した結果、イオン加速器を用いて柱状ガラス体外壁に重イオンを照射する際に、重イオンの加速エネルギーと照射時間を適宜換えることにより、重イオンの浸透深さを任意に制御することができるので、同じ操作をイオン加速器と柱状ガラス体との相対位置を柱状ガラス体の長手方向に順次変化させて実施することにより柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を形成することができ、また、以上の操作を柱状ガラス体中の他の位置で繰り返すことにより柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本形成することができ、更に、柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本有する柱状ガラス体を長手方向に延伸処理することにより複数のコアを有する光ファイバーを製造し得ることを見いだし、本発明を完成した。 As a result of intensive studies to achieve the above object, the present inventor changed the acceleration energy and irradiation time of heavy ions appropriately when irradiating heavy ions to the outer wall of a columnar glass body using an ion accelerator, Since the penetration depth of heavy ions can be arbitrarily controlled, the same operation is performed by sequentially changing the relative position between the ion accelerator and the columnar glass body in the longitudinal direction of the columnar glass body. A region having a high heavy ion concentration continuous in the direction can be formed, and a region having a high heavy ion concentration continuous in the longitudinal direction of the columnar glass body can be formed by repeating the above operation at other positions in the columnar glass body. Further, a columnar glass body having a plurality of regions having a high heavy ion concentration continuous in the longitudinal direction of the columnar glass body is stretched in the longitudinal direction. Found that it is possible to manufacture an optical fiber having a plurality of cores by, the present invention has been completed.
即ち、本発明の柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本有する柱状ガラス体の製造方法は、イオン加速器を用いて重イオンを細いビームの状態で長い柱状ガラス体中の所定の位置に注入して重イオン濃度の高い領域を形成し、該イオン加速器と該柱状ガラス体との相対位置を該柱状ガラス体の長手方向に順次変化させて重イオンを細いビームの状態で該柱状ガラス体中に順次注入して該柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を形成し、以上の操作を該柱状ガラス体中の他の位置で、好ましくは円周に沿って一定間隔で複数回繰り返して、該柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本形成することを特徴とする。 That is, the method for producing a columnar glass body having a plurality of regions having a high heavy ion concentration continuous in the longitudinal direction of the columnar glass body according to the present invention is a method of producing heavy ions in a long columnar glass body in a thin beam state using an ion accelerator. A region having a high heavy ion concentration is formed by injecting the ion accelerator into a predetermined position, and the relative position between the ion accelerator and the columnar glass body is sequentially changed in the longitudinal direction of the columnar glass body so that heavy ions are in a thin beam state. In order to form a region having a high concentration of heavy ions continuous in the longitudinal direction of the columnar glass body by sequentially injecting into the columnar glass body, the above operation is preferably performed at other positions in the columnar glass body. A plurality of regions having a high heavy ion concentration continuous in the longitudinal direction of the columnar glass body are formed by repeating a plurality of times at regular intervals along.
また、本発明の複数のコアを有する光ファイバーの製造方法は、柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本有する柱状ガラス体を長手方向に延伸処理することを特徴とする。 The method for producing an optical fiber having a plurality of cores according to the present invention is characterized in that a columnar glass body having a plurality of regions having a high heavy ion concentration continuous in the longitudinal direction of the columnar glass body is stretched in the longitudinal direction. .
例えば、本発明の複数のコアを有する光ファイバーの製造方法は、イオン加速器を用いて重イオンを細いビームの状態で長い柱状ガラス体中の所定の位置に注入して重イオン濃度の高い領域を形成し、該イオン加速器と該柱状ガラス体との相対位置を該柱状ガラス体の長手方向に順次変化させて重イオンを細いビームの状態で該柱状ガラス体中に順次注入して該柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を形成し、以上の操作を該柱状ガラス体中の他の位置で、好ましくは円周に沿って一定間隔で複数回繰り返して、該柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本形成し、その後該柱状ガラス体を長手方向に延伸処理することを特徴とする。 For example, in the method of manufacturing an optical fiber having a plurality of cores according to the present invention, an ion accelerator is used to inject heavy ions into a predetermined position in a long columnar glass body in a thin beam state to form a region having a high heavy ion concentration. Then, the relative position between the ion accelerator and the columnar glass body is sequentially changed in the longitudinal direction of the columnar glass body so that heavy ions are sequentially injected into the columnar glass body in a thin beam state. A region having a high heavy ion concentration continuous in the longitudinal direction is formed, and the above operation is repeated several times at other positions in the columnar glass body, preferably at regular intervals along the circumference. A plurality of regions having a high heavy ion concentration continuous in the longitudinal direction are formed, and then the columnar glass body is stretched in the longitudinal direction.
本発明の製造方法により、一本の柱状ガラス体の中に光ファイバー状の光の通り道を多数作り出すことができ、これを長手方向に延伸処理することにより複数のコアを有する光ファイバーを得ることができる。 According to the manufacturing method of the present invention, a large number of optical fiber-like light paths can be created in a single columnar glass body, and an optical fiber having a plurality of cores can be obtained by stretching this in the longitudinal direction. .
本発明の柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本有する柱状ガラス体の製造方法を図１に基づいて説明する。最初に、イオン加速器、例えばタンデム加速器を用いて重イオンを細いビームの状態で長い柱状ガラス体（光ファイバーに用いられている通常のガラス体）中の所定の位置（普通には柱状ガラス体の端部、例えば図１（ａ）に示す点Ａの位置）に注入して重イオン濃度の高い領域を形成し、引き続いて該イオン加速器と該柱状ガラス体との相対位置を該柱状ガラス体の長手方向に順次変化させて重イオンを細いビームの状態で該柱状ガラス体中に順次注入して該柱状ガラス体の長手方向に連続した重イオン濃度の高い領域（図１（ｂ）に示す１の領域）を該柱状ガラス体の一端（図１（ｂ）に示す点Ａの位置）から他端（図１（ｂ）に示す点Ｂの位置）まで形成する。 A method for producing a columnar glass body having a plurality of regions having a high heavy ion concentration continuous in the longitudinal direction of the columnar glass body of the present invention will be described with reference to FIG. First, an ion accelerator, for example, a tandem accelerator is used to place heavy ions in a thin beam state in a long columnar glass body (ordinary glass body used for optical fibers) (usually the end of the columnar glass body). A region having a high heavy ion concentration is formed, and subsequently the relative position between the ion accelerator and the columnar glass body is determined by the length of the columnar glass body. In the state where the heavy ions are successively injected into the columnar glass body in the state of a thin beam by changing in the direction, the heavy ion concentration is continuous in the longitudinal direction of the columnar glass body (1 shown in FIG. 1B). A region) is formed from one end (position of point A shown in FIG. 1 (b)) to the other end (position of point B shown in FIG. 1 (b)) of the columnar glass body.
次いで、以上の操作を該柱状ガラス体中の他の位置で、好ましくは、図１（ｃ）に示すように、円周に沿って一定間隔で複数回繰り返して、該柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本形成する（図１（ｃ）には内部の重イオン濃度の高い領域を３本のみ示し、他は省略してある）。以上の操作で本発明の柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本有する柱状ガラス体を得ることができる。なお、重イオンの種類や加速エネルギーを適宜換えることで目的に即したインプランテーションを容易に遂行することができる。 Next, the above operation is repeated at other positions in the columnar glass body, preferably a plurality of times at regular intervals along the circumference, as shown in FIG. A plurality of continuous regions with high heavy ion concentration are formed (FIG. 1 (c) shows only three regions with high internal heavy ion concentration, others are omitted). By the above operation, a columnar glass body having a plurality of regions having a high heavy ion concentration continuous in the longitudinal direction of the columnar glass body of the present invention can be obtained. In addition, the implantation suitable for the objective can be easily performed by changing the kind and acceleration energy of heavy ion suitably.
本発明の上記の製造方法により、柱状ガラス体中にその長手方向に連続した重イオン濃度の高い領域を複数本平行に形成することができ、この重イオン濃度の高い領域は高い光屈折率を持つので、ここを通過する光は全反射により重イオン濃度の低い部分にもれることはない。つまり、一本のガラス体の中に光ファイバー状の光の通り道を多数作り出すことができる。 According to the manufacturing method of the present invention, a plurality of regions having a high heavy ion concentration continuous in the longitudinal direction can be formed in parallel in the columnar glass body, and the region having a high heavy ion concentration has a high photorefractive index. Therefore, the light passing through the light source does not leak into a portion having a low heavy ion concentration due to total reflection. That is, many optical fiber-like light paths can be created in one glass body.
本発明の複数のコアを有する光ファイバーの製造方法においては、上記のようにして又はその他の方法で製造された柱状ガラス体の長手方向に連続した重イオン濃度の高い領域を複数本有する柱状ガラス体を長手方向に加熱延伸処理して複数のコアを有する光ファイバーを形成する。 In the method for producing an optical fiber having a plurality of cores of the present invention, a columnar glass body having a plurality of regions having a high heavy ion concentration in the longitudinal direction of the columnar glass body produced as described above or by other methods. Is heated and stretched in the longitudinal direction to form an optical fiber having a plurality of cores.
柱状ガラス体を長手方向に加熱延伸処理することで実際の光ファイバーの細さまで容易に引き伸ばすことができる。このようにして作製される光ファイバーは多数の光のパスを内包することで、その通信量を飛躍的に向上させることができ、大量情報の双方向通信が期待できる。 By heating and stretching the columnar glass body in the longitudinal direction, it can be easily stretched to the actual thinness of the optical fiber. An optical fiber manufactured in this way can greatly increase the amount of communication by enclosing a large number of light paths, and can expect bidirectional communication of a large amount of information.
＜重イオンの照射＞
下記組成のガラスを調製し、直径約１０ｍｍ、長さ約５０ｍｍの柱状ガラス体に成形した。それらの柱状ガラス体にタンデム加速器を用いて室温で下記の照射条件下で重イオン照射を行った。
<Irradiation of heavy ions>
A glass having the following composition was prepared and formed into a columnar glass body having a diameter of about 10 mm and a length of about 50 mm. These columnar glass bodies were irradiated with heavy ions at room temperature under the following irradiation conditions using a tandem accelerator.
ガラス組成：
（１）０.９９(０.８Ｂ2Ｏ3−０.２ＰｂＯ)−０.０１ＣｕＣｌ
（２）０.９９(０.８Ｂ2Ｏ3−０.２ＰｂＯ)−０.０１ＬｉＣｌ
（３）０.８Ｂ2Ｏ3−０.２ＰｂＯ
Glass composition:
(1) 0.99 (0.8B 2 O 3 -0.2PbO) -0.01CuCl
(2) 0.99 (0.8B 2 O 3 -0.2PbO) -0.01LiCl
(3) 0.8B 2 O 3 -0.2PbO
照射条件：
各ガラスに共通
照射イオン：Ｘｅ14+（加速エネルギー １６０ＭｅＶ）
照射時間：１時間
照射中の試料電流：１２５ｎＡ
照射面積：０.６４ｃｍ2（照射エリア：直径９ｍｍの円）
ガラス（１）
照射イオン数：４５０５４×１０-8クーロン＝２.０１×１０14イオン
単位面積当たりの照射イオン数：３.１４×１０14 イオン／ｃｍ2
ガラス（２）及び（３）
照射イオン数：４４３３６×１０-8クーロン＝１.９８×１０14イオン
単位面積当たりの照射イオン数：３.０９×１０14 イオン／ｃｍ2
Irradiation conditions:
Common to all glasses Irradiated ions: Xe 14+ (acceleration energy 160 MeV)
Irradiation time: 1 hour Sample current during irradiation: 125 nA
Irradiation area: 0.64 cm 2 (Irradiation area: Circle with a diameter of 9 mm)
Glass (1)
Number of irradiated ions: 45054 × 10 −8 coulomb = 2.01 × 10 14 ions Number of irradiated ions per unit area: 3.14 × 10 14 ions / cm 2
Glass (2) and (3)
Number of irradiated ions: 44336 × 10 −8 coulomb = 1.98 × 10 14 ions Number of irradiated ions per unit area: 3.09 × 10 14 ions / cm 2
なお、上記のタンデム加速器とはペレットチェーンに電荷を乗せて高電圧端子に運び上げ、高電圧を発生させてイオンを加速させる装置で、一つの高電圧で一回目は負イオンを加速し、途中でイオンの電荷を負から正へ変換して、２回目は正イオ ンを加速する装置である。負イオン源では電子に原子を結合させて負イオンを生成し、これを加速するために超高真空に保たれた初段加速管に入射し負イオン加速管入口まで到達させる。負イオン加速管まで到達した負イオンを、正の高電圧端子に向け加速させる。高電圧端子に到達した負イオンは、電子ストリッパー（炭素薄膜または窒素ガス層）で多数の電子がはぎとられ正イオンに変換後、正イオン加速管で再び加速され高エネルギーのイオンビームが得られる。 The tandem accelerator mentioned above is a device that puts charges on the pellet chain and transports them to the high voltage terminal to generate high voltage and accelerate the ions. The second is a device that accelerates positive ions by converting the charge of ions from negative to positive. In the negative ion source, atoms are combined with electrons to generate negative ions, and in order to accelerate them, the negative ions are incident on the first stage accelerator tube maintained in an ultra-high vacuum and reach the negative ion accelerator tube entrance. Negative ions that have reached the negative ion accelerator tube are accelerated toward the positive high-voltage terminal. Negative ions that have reached the high voltage terminal are stripped off by the electron stripper (carbon thin film or nitrogen gas layer) and converted to positive ions, and then accelerated again by the positive ion accelerator tube to obtain a high-energy ion beam.
上記のような条件でガラス試料にＸｅ14+を照射したところ、ガラス試料に外見上の変化はほとんど認められなかった。しかし、高エネルギーでのイオン照射であるのでガラス体へのＸｅ14+の注入が起こっていることが十分に予想される。そこで、深さあたりの試料に付与されるエネルギーをＳＲＩＭ２０００（計算コード）により計算した結果を図２及び図３に示す。図２は電子的エネルギーＳｅを表しており、図３は核的エネルギーＳｎを表している。 When the glass sample was irradiated with Xe 14+ under the above conditions, almost no change in appearance was observed in the glass sample. However, since ion irradiation is performed at a high energy, it is sufficiently expected that Xe 14+ is implanted into the glass body. Therefore, the results of calculating the energy applied to the sample per depth by SRIM2000 (calculation code) are shown in FIGS. FIG. 2 represents the electronic energy Se, and FIG. 3 represents the nuclear energy Sn.
図２及び図３から明らかなように、Ｘｅ14+はガラス試料表面から１０μmの深さにまで注入され、そのあたりで濃度が高くなっていることがわかった。むしろ表面に近いほど濃度が低くなっていた。いずれにせよ、ガラスのごく表面付近にのみ重イオンが分布して存在することがわかった。計算コードから推察すると、加速粒子の質量が小さくなるほど、加速エネルギーが大きくなるほど、イオン注入の深さが深くなることが予想される。このことは、材料の局所構造を、つまり局所的な特性を制御し得ることを示している。 As is apparent from FIGS. 2 and 3, Xe 14+ was injected to a depth of 10 μm from the glass sample surface, and it was found that the concentration increased around that. Rather, the closer to the surface, the lower the concentration. In any case, it was found that heavy ions are distributed only near the very surface of the glass. As inferred from the calculation code, it is expected that the ion implantation depth increases as the mass of the accelerated particles decreases and the acceleration energy increases. This indicates that the local structure of the material, that is, the local properties can be controlled.
＜ラマン分光実験＞
ラマン分光器によりラマンスペクトルを測定し、イオン照射前後のガラス構造の変化を調べた。ここでは日本分光工業（株）製のＮＲ−１８００型レーザーラマン分光光度計を用い、光源には波長５１４.５ｎｍのＡｒ+レーザーを使用した。ガラス試料にレーザー光を水平に照射させ、同じ平面上で入射光に対して垂直方向にあるレンズにより散乱光を集光する水平直角散乱法によりスペクトル測定を行った。ラマン分光実験の測定条件を第１表に示す。
<Raman spectroscopy experiment>
The Raman spectrum was measured with a Raman spectrometer, and the change in the glass structure before and after ion irradiation was examined. Here, an NR-1800 type laser Raman spectrophotometer manufactured by JASCO Corporation was used, and an Ar + laser having a wavelength of 514.5 nm was used as a light source. A glass sample was irradiated with laser light horizontally, and the spectrum was measured by a horizontal right-angle scattering method in which scattered light was collected by a lens perpendicular to the incident light on the same plane. Table 1 shows the measurement conditions for the Raman spectroscopic experiment.
Ｂ2Ｏ3−ＰｂＯ系のガラスにおいてはＰｂＯの含有量の少ない組成で、５００、７７０、８１０ｃｍ-1付近に目立ったピークが認められ、その含有量が増えるにつれて、三配位型ホウ素に由来する振動である８１０ｃｍ-1付近のピーク強度が減少し、四配位型ホウ素の出現によって起こる振動である７７０ｃｍ-1付近のピーク強度の増大が報告されている。また１４００ｃｍ-1付近のピークはオルソボレイトの振動である。 In the B 2 O 3 —PbO-based glass, a conspicuous peak is observed in the vicinity of 500, 770, and 810 cm −1 with a composition having a low PbO content. As the content increases, it is derived from tricoordinate boron. It has been reported that the peak intensity near 810 cm −1, which is a vibration, decreases, and the peak intensity near 770 cm −1, which is a vibration caused by the appearance of tetracoordinated boron, is increased. The peak near 1400 cm −1 is orthoborate vibration.
本実験では特に７７０および８１０ｃｍ-1のピークの変化に注目し、Ｘｅ14+イオンの照射がそれぞれの試料のボロキソル環型構造に及ぼす影響について調べた。図４に０.８Ｂ2Ｏ3-０.２ＰｂＯ、０.９９(０.８Ｂ2Ｏ3-０.２ＰｂＯ)-０.０１ＬｉＣｌおよび ０.９９(０.８Ｂ2Ｏ3-０.２ＰｂＯ)-０.０１ＣｕＣｌガラスのイオン照射前後のラマンスペクトルを示す。 In this experiment, focusing on changes in peaks at 770 and 810 cm −1 , the influence of Xe 14+ ion irradiation on the boroxol ring structure of each sample was investigated. FIG. 4 shows 0.8B 2 O 3 -0.2PbO, 0.99 (0.8B 2 O 3 -0.2PbO) -0.01LiCl and 0.99 (0.8B 2 O 3 -0.2PbO)- The Raman spectrum before and behind ion irradiation of 0.01 CuCl glass is shown.
０.８Ｂ2Ｏ3-０.２ＰｂＯ系ガラスは照射によるスペクトルに変化はあまり認められなかったのに対し、０.９９(０.８Ｂ2Ｏ3-０.２ＰｂＯ)-０.０１ＬｉＣｌおよび０.９９(０.８Ｂ2Ｏ3-０.２ＰｂＯ)-０.０１ＣｕＣｌガラスのスペクトルは大きな変化がみられた。次にバックグラウンドの補正を行い、７７０および８１０ｃｍ-1のピークを分離し照射前後のピークの変化を解析した。照射前後のラマンススペクトルをピーク分離した結果の一例を図５に示す。 The 0.8B 2 O 3 -0.2PbO glass did not show much change in the spectrum due to irradiation, whereas 0.9 (0.8B 2 O 3 -0.2PbO) -0.01LiCl and 0.0L The spectrum of 99 (0.8B 2 O 3 -0.2PbO) -0.01CuCl glass changed significantly. Next, the background was corrected, peaks at 770 and 810 cm −1 were separated, and changes in the peaks before and after irradiation were analyzed. An example of the result of peak separation of the Raman spectra before and after irradiation is shown in FIG.
ピーク分離した後、それぞれのピーク面積の分率を求めた。すべての系において、イオン照射によりスペクトルの強度がおしなべて減少していた。照射前後での面積の分率には大きな変化はみられなかったので、ガラス構造全体が照射の影響を受けているものと考えられる。イオン照射によりガラス中で形成されていたボロキソル環型構造やＢＯ4四面体が少し変形し、全体としてガラス構造がよりランダムになったと考えられる。 After peak separation, the fraction of each peak area was determined. In all systems, the intensity of the spectrum was generally reduced by ion irradiation. Since there was no significant change in the area fraction before and after irradiation, the entire glass structure is considered to be affected by irradiation. It is considered that the boroxol ring structure and the BO 4 tetrahedron formed in the glass by ion irradiation were slightly deformed, and the glass structure as a whole became more random.
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