JPH0422906A - Production of rare earth element-added waveguide - Google Patents
Production of rare earth element-added waveguideInfo
- Publication number
- JPH0422906A JPH0422906A JP2128317A JP12831790A JPH0422906A JP H0422906 A JPH0422906 A JP H0422906A JP 2128317 A JP2128317 A JP 2128317A JP 12831790 A JP12831790 A JP 12831790A JP H0422906 A JPH0422906 A JP H0422906A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- tablet
- earth element
- manufacturing
- tablets
- 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.)
- Granted
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 22
- 150000002910 rare earth metals Chemical class 0.000 title claims description 11
- 239000011521 glass Substances 0.000 claims abstract description 46
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 20
- 238000001704 evaporation Methods 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 claims description 8
- 238000005566 electron beam evaporation Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000001312 dry etching Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000000206 photolithography Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 239000010419 fine particle Substances 0.000 abstract description 10
- 238000010894 electron beam technology Methods 0.000 abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- 230000001678 irradiating effect Effects 0.000 abstract description 5
- 229910052681 coesite Inorganic materials 0.000 abstract description 3
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 229910052682 stishovite Inorganic materials 0.000 abstract description 3
- 229910052905 tridymite Inorganic materials 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 description 16
- 229910052779 Neodymium Inorganic materials 0.000 description 4
- 229920002120 photoresistant polymer Polymers 0.000 description 4
- 229910052691 Erbium Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- -1 etc. may be used Inorganic materials 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Optical Integrated Circuits (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、希土類元素を添加した低損失ガラス導波路の
製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for manufacturing a low-loss glass waveguide doped with rare earth elements.
Ｅ従来の技術］
近年、光ファイバのコアに希土類元素を添加した光フア
イバ増幅器及びレーザの研究が活発化し、光波通信用増
幅器及びレーザが注目されてきている。これに伴い、ガ
ラス導波路の光伝搬部分であるコア部分に希土類元素を
添加して、レーザ、増幅器、或いは増幅機能付きの各種
光回路を構成する構想もなされている。E. Prior Art] In recent years, research into optical fiber amplifiers and lasers in which the core of the optical fiber is doped with rare earth elements has become active, and amplifiers and lasers for light wave communications are attracting attention. Along with this, there are also plans to add rare earth elements to the core portion, which is the light propagation portion, of the glass waveguide to construct lasers, amplifiers, or various optical circuits with amplification functions.
本発明者は、希土類元素を添加したガラス導波路の製造
方法として、次のような方法を提案しな。The present inventor proposes the following method as a method for manufacturing a glass waveguide doped with rare earth elements.
この方法は、低屈折率層を有する基板上に、電子ビーム
蒸着装置を用いて希土類元素を含むコア用ガラス膜を形
成し、その後、高温熱処理、ホトリングラフィ及びドラ
イエツチングによるコアの加工並びに低屈折率ガラス膜
被覆工程を経て埋込型ガラス導波路を製造するものであ
り、特にコア用ガラス膜の形成方法に特徴がある。This method involves forming a core glass film containing a rare earth element on a substrate having a low refractive index layer using an electron beam evaporation device, and then processing the core by high-temperature heat treatment, photolithography, and dry etching. A buried glass waveguide is manufactured through a refractive index glass film coating process, and is particularly characterized by the method of forming the core glass film.
その方法は、希土類元素、屈折率制御用酸化物及び５ｉ
ｎ２の粉末を混合し、ホットプレスで焼き固めた後、更
に焼結して粒状、板状、或いは棒状のタブレットとし、
このタブレットを電子ビーム蒸着装置の高真空酸素分圧
化で蒸発させてコア用ガラス膜を形成する方法である。The method includes rare earth elements, refractive index controlling oxides and 5i
After mixing the n2 powder and hardening it with a hot press, it is further sintered to form a granular, plate-shaped, or rod-shaped tablet,
In this method, this tablet is evaporated using high vacuum oxygen partial pressure using an electron beam evaporation device to form a glass film for the core.
ここで、希土類元素とは、Ｅｒ、Ｎｄ、Ｙｂ、Ｃｅ、Ｈ
ｏ、Ｔｍなどを少なくとも一種類含んだしのをいい、屈
折率制御用酸化物とは、Ｐ、Ｇｅ、Ｔｉ、ＡＩ、Ｚｎ、
Ｂ、Ｆなどを少なくとも一種類含んな酸化物をいう。Here, the rare earth elements are Er, Nd, Yb, Ce, H
Oxide containing at least one kind of oxide, Tm, etc., and the refractive index controlling oxide is P, Ge, Ti, AI, Zn,
Refers to an oxide containing at least one type of B, F, etc.
［発明が解決しようとする課題］
しかし、上記製造方法においては、顕Ｒ鏡による暗視野
像を観察しな結果、コア用ガラス膜中に第４図に示すよ
うに粒径が数μｍの微粒子が混入することが分かった。[Problems to be Solved by the Invention] However, in the above manufacturing method, as a result of observing a dark field image with an R microscope, fine particles with a particle size of several μm were found in the core glass film as shown in FIG. was found to be mixed in.
その原因を調べたところ、タブレットが第５図に示すよ
うに数μｍの微粒子の焼結体からなり、これに電子ビー
ムを照射すると、照射部分は溶融し、蒸発原子となって
基板表面に膜を形成するが、照射部分の周辺の微粒子が
同時に飛散してコア用ガラス膜に混入することが荊明し
た。When we investigated the cause of this, we found that the tablet is made of a sintered body of fine particles of several micrometers in size, as shown in Figure 5. When the tablet is irradiated with an electron beam, the irradiated part melts and becomes evaporated atoms, forming a film on the substrate surface. However, it was revealed that fine particles around the irradiated area were scattered at the same time and mixed into the core glass film.
このようなコア用ガラス膜を用いてガラス導波路を作成
すると、散乱損失の大きいガラス導波路となり、レーザ
、増幅器などを実現することが国数である。When a glass waveguide is created using such a core glass film, it becomes a glass waveguide with large scattering loss, and many countries are now using it to realize lasers, amplifiers, and the like.
そこで、本発明の目的は、上記問題点を解決し、低損失
のガラス導波路を製造することができる希土類元素添加
導波路の製造方法を提供することにある。SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide a method for manufacturing a rare earth element-doped waveguide that can solve the above problems and manufacture a glass waveguide with low loss.
「課題を解決するための手段］
上記目的を達成するために本発明に係る希土類元素添加
導波路の製造方法は、希土類元素及びＳ ｉ Ｏ２を含
み、焼結密度が９０％以上で粒径が１０μｍ以上の粒子
の塊からなるタブレットを電子ビーム蒸着法により蒸発
させて低屈折率層を有する基板上に希土類元素を含むｓ
ｉｏ、のコア用ガラス膜を形成する工程と、その基板全
体を高温熱処理する工程と、上記コア用ガラス膜をホト
リングラフィ及びドライエツチングにより断面略矩形の
コアに加工する工程と、基板上のコア全体に低屈折率の
ガラス膜を被覆する工程とからなっている。"Means for Solving the Problems" In order to achieve the above object, the method for manufacturing a rare earth element-doped waveguide according to the present invention includes a rare earth element and SiO2, a sintered density of 90% or more, and a grain size of S containing rare earth elements is deposited on a substrate having a low refractive index layer by evaporating a tablet consisting of agglomerates of particles of 10 μm or more using an electron beam evaporation method.
io, a step of heat-treating the entire substrate at a high temperature, a step of processing the core glass film into a core having a substantially rectangular cross section by photolithography and dry etching, and a step of forming a core glass film on the substrate. The process consists of a step of coating the entire core with a glass film having a low refractive index.
５作用〕
かかる製造方法によれば、タブレットに電子ビームを照
射して基板表面に膜を形成する際、タブレットが１０μ
ｍ以上の粒子の塊からなっているため、照射部分の周辺
の粒子が同時に飛散することがなくなり、従って微粒子
の混入しないコア用ガラス膜を形成することができ、低
損失のガラス導波路を作成することができる。5 Effect] According to this manufacturing method, when the tablet is irradiated with an electron beam to form a film on the substrate surface, the tablet has a thickness of 10 μm.
Since it is made up of agglomerates of particles larger than m, particles around the irradiated area will not be scattered at the same time, making it possible to form a core glass film that does not contain fine particles, creating a low-loss glass waveguide. can do.
「実施例］
以下、本発明の一実施例を添付図面に基づいて詳述する
。``Example'' Hereinafter, an example of the present invention will be described in detail based on the accompanying drawings.
（実施例１）
第１図は最初の工程を実施するための電子ビーム蒸着装
置１を示している０図示するように上記装Ｗ１のハウジ
ング２内の下方には遮蔽板３により隔てられた２個の蒸
発源４ａ、４ｂが配置され、上方には複数枚の基板５を
保持する凹面状の基板ホルダ６が配置されている。また
、ハウジング２には酸素ガスを供給する供給ガス系７及
びハウジング２内を真空にする真空排気系８が接続され
ている。一方の蒸発源４ａにはＳｉＯ□とＴｉ０ｚを混
合したタブレット９が収容され、他方の蒸発源４ｂには
Ｅ ｒ ２０ ｓのタブレット１０が収容されている。(Embodiment 1) FIG. 1 shows an electron beam evaporation apparatus 1 for carrying out the first step. Evaporation sources 4a and 4b are arranged, and a concave substrate holder 6 for holding a plurality of substrates 5 is arranged above. Further, a supply gas system 7 for supplying oxygen gas and a vacuum exhaust system 8 for evacuating the inside of the housing 2 are connected to the housing 2 . One evaporation source 4a accommodates a tablet 9 containing a mixture of SiO□ and Ti0z, and the other evaporation source 4b accommodates a tablet 10 of E r 20 s.
前者のタブレット９は重量比率９９％のＳｉＯ□の粉末
中に１％のＴｉＯ□の粉末を混合し、これを１０００℃
の温度で圧力を加えてホットプレスすることにより焼結
密度的９０％とされている。The former tablet 9 is made by mixing 1% TiO□ powder into SiO□ powder with a weight ratio of 99%, and heating it at 1000°C.
The sintering density is said to be 90% by hot pressing at a temperature of .
この状態のタブレットは第５図に示すように数μｍの微
粒子の塊からなる焼結体であるが、これを更に約１７０
０℃の温度で熱処理することにより第３図に示すように
数１０μｍの粒子の塊からなる焼結体のタブレットとさ
れている。後者のタブレット１０も同様に数１０μｍの
粒子の塊からなる焼結体となるように融点よりも僅かに
低い温度で熱処理されている。低屈折率層を有する基板
５としては、直径３インチ、厚さ１ｍｍの石英ガラスが
用いられている。As shown in Figure 5, the tablet in this state is a sintered body made up of agglomerates of fine particles of several micrometers in size.
By heat-treating at a temperature of 0° C., a sintered tablet consisting of agglomerates of particles several tens of micrometers in size is obtained, as shown in FIG. The latter tablet 10 is similarly heat-treated at a temperature slightly lower than the melting point so as to form a sintered body consisting of agglomerates of particles several tens of micrometers in size. As the substrate 5 having the low refractive index layer, quartz glass with a diameter of 3 inches and a thickness of 1 mm is used.
そして、上記ハウジング２内を１０−’Ｔｏｒｒの高真
空状態下で酸素ガスを流量調節して供給することにより
真空度が５Ｘ１０−’Ｔｏｒｒになるようにし、この状
態で蒸発源内４ａ、４ｂのタブレット９．１０に電子ビ
ームをそれぞれ同時に照射することにより、基板５の表
面にＥｒイオンを含むＳｉＯ□−ＴｉＯ□のコア用ガラ
スＷ！Ａ１１を形成する（第２図の（ａ）参照）、この
場合、コア用ガラスＩｆ！１１中へのＥｒイオンの添加
量を制御するには、Ｅｒ２Ｏ３のタブレット１０に照射
する電子ビームのｔ流値を制御すればよく、この制御方
法によりＥｒイオンの添加量を数ｐｐｍから数％まで制
御することができる６
次いで、このコア用ガラス膜１１の形成された基板５全
体を１０００℃以上の温度で高温熱処理することにより
、波長が０．６３μｍで屈折率が１．４６５１の緻密な
膜１１を得る（ｂ）、その後、上記１１１１の表面に膜
厚的１μｍのＷＳｆ膜１２をスパッタリングにより形成
しく同図（ｃ））、そのＷＳｉ！１１２の表面にホトレ
ジストを塗布し、ホトリングラフフィによりホトレジス
ト膜１３のパターニングを行い（ｄ）、ドライエツチン
グによりＮ Ｆ ｓガスを用いてＷ Ｓ ｉ Ｉｌｌ
２のパターニングを行う（ｅ）。次いで、ホトレジスト
ＩＩ！１３及びＷ Ｓ ｉ Ｈ１２をマスクにしてドラ
イエツチングによりＣＨＦ ｓカスを用いてコア用ガラ
ス膜１１のパターニングを行い（ｆ）、コア１４を形成
する。Then, oxygen gas is supplied inside the housing 2 under a high vacuum state of 10-' Torr so that the degree of vacuum becomes 5 x 10-' Torr, and in this state, the tablets in the evaporation sources 4a and 4b are By simultaneously irradiating 9.10 with an electron beam, the core glass W of SiO□-TiO□ containing Er ions on the surface of the substrate 5! A11 (see FIG. 2(a)), in this case, the core glass If! In order to control the amount of Er ions added to the Er2O3 tablet 10, it is sufficient to control the t current value of the electron beam irradiated to the Er2O3 tablet 10, and by this control method, the amount of Er ions added can be adjusted from several ppm to several percent. Next, the entire substrate 5 on which the core glass film 11 is formed is subjected to high-temperature heat treatment at a temperature of 1000° C. or higher to form a dense film with a wavelength of 0.63 μm and a refractive index of 1.4651. 11 (b), then a WSf film 12 with a thickness of 1 μm is formed on the surface of the above-mentioned 1111 by sputtering (FIG. 2(c)), and the WSi! A photoresist is applied to the surface of the film 112, the photoresist film 13 is patterned by photolithography (d), and dry etching is performed using NFs gas.
2. Perform patterning (e). Next, Photoresist II! 13 and W Si H 12 as masks, the core glass film 11 is patterned by dry etching using CHF s residue (f) to form the core 14.
次いで、ホトレジスト膜１３及びＷ Ｓ ｉ Ｈ１２を
除去した後（ｇ）、基板５上のコア１４全体に屈折率が
１．４５８０ （波長が０．６３μｍでの値）のＳｆＯ
□−Ｐ２０ｓＢ２０ｓ系のガラス１１１１５を被覆して
埋込型導波路が完成する（ｈ）。Next, after removing the photoresist film 13 and W S i H 12 (g), SfO with a refractive index of 1.4580 (value at a wavelength of 0.63 μm) is deposited over the entire core 14 on the substrate 5.
A buried waveguide is completed by covering with □-P20sB20s glass 11115 (h).
かかる製造方法によれば、特にタブレット９゜１０を融
点よりも僅かに低い温度で熱処理したので、焼結密度を
高めることができ、少なくとも１０μｍの粒子の塊から
なるタブレット９，１０を得ることができる。従って、
タブレット９，１０に電子ビームを照射して基板５表面
に膜１１を形成する際、タブレット９，１０が１０μｍ
以上の粒子の塊からなっているため、照射部分の周辺の
粒子が同時に飛散することがなくなり、第４図に示した
ような数μｍの微粒子の混入しないコア用ガラス膜１１
を形成することができ、低損失の埋込型導波路を作成す
ることができる。According to this manufacturing method, in particular, since the tablets 9 and 10 are heat-treated at a temperature slightly lower than their melting point, the sintered density can be increased, and tablets 9 and 10 consisting of agglomerates of particles of at least 10 μm can be obtained. can. Therefore,
When forming the film 11 on the surface of the substrate 5 by irradiating the tablets 9 and 10 with an electron beam, the tablets 9 and 10 have a thickness of 10 μm.
Since it is made up of agglomerates of the above particles, particles around the irradiated area will not be scattered at the same time, and the core glass film 11 will not be contaminated with fine particles of several μm as shown in Fig. 4.
can be formed, making it possible to create a low-loss buried waveguide.
この導波路のＥｒイオン以外による吸収損失は０．１ｄ
Ｂ／ｃｍ以下であった。また、散乱中心となる導波路の
梢遣不均−性も殆ど見られなかった。The absorption loss due to other than Er ions in this waveguide is 0.1d
B/cm or less. In addition, almost no unevenness in the waveguide distribution, which is the center of scattering, was observed.
Ｅ、 ｒイオンによる１、５３μｍ帯での吸収損失はＥ
ｒの添加量により数ｄＢから１０数ｄＢの値を実現する
ことができた。従って、この導波路により１．５３μｍ
帯の信号光と、０゜０９８μｍ或いは１．４６μｍの励
起光を重畳して伝搬させれば、１．５３μｍ帯の信号光
を増幅させることが可能である。The absorption loss in the 1.53 μm band due to E, r ions is E
Depending on the amount of r added, it was possible to achieve a value of several dB to more than ten dB. Therefore, with this waveguide, 1.53μm
By superimposing and propagating the band signal light and the 0°098 μm or 1.46 μm pump light, it is possible to amplify the 1.53 μm band signal light.
（実施例２）
上記実施例１では２個の蒸発源４ａ、４ｂによる二源蒸
着法を採用したが、本実施例では一方の蒸発源４ａのみ
にタブレットを入れて一源蒸着法により、Ｅｒイオンを
添加したＳｉＯ□−Ｇｅ０２ Ｐ２Ｏ５のコア用ガラ
ス膜１１を基板５の表面に形成した。タブレットとして
、スート状のファイバコア母材（Ｓ ｉ ＯｓにＧｅＯ
□及びＰ２Ｏ、を添加したもの）にＥ ｒ ＣＩ ｓの
溶液を含浸させ、乾燥、固化後、焼結して透明にガラス
化したファイバコア母材（直径１５ｍｍ、波長０．６３
μｍでの屈折率１．４６２０、Ｅｒイオンの添加量３０
００ｐｐｍ）を用いた４
その結果、Ｅｒイオンの添加量が約１８００ｐｐｍの均
一なＳ Ｓ Ｏｘ Ｇ ｅ Ｏ２Ｐ ２０ ｓのコア
用ガラス膜１１を基板５上に厚さ７μｍ形成することが
できた。このコア用ガラス膜１１の屈折率は波長０．６
３μｍで１．４６１２であった。そして、このコア用ガ
ラス膜１１を有する基板５を用いて上記実施例１と同様
の方法により埋込型導波路を作成した結果、散乱損失の
極めて少ない導波路を得ることができた。(Example 2) In the above-mentioned Example 1, a two-source evaporation method using two evaporation sources 4a and 4b was adopted, but in this example, a tablet was put in only one evaporation source 4a and a single-source evaporation method was used. A core glass film 11 of SiO□-Ge02P2O5 doped with ions was formed on the surface of the substrate 5. As a tablet, a soot-like fiber core matrix (SiOs and GeO
A fiber core base material (diameter 15 mm, wavelength 0.63
Refractive index in μm 1.4620, amount of Er ions added 30
As a result, a core glass film 11 of S S Ox G e O2P 20 s having a uniform addition amount of Er ions of approximately 1800 ppm could be formed on the substrate 5 to a thickness of 7 μm. The refractive index of this core glass film 11 is 0.6 at wavelength.
It was 1.4612 at 3 μm. Then, as a result of creating a buried waveguide using the substrate 5 having this core glass film 11 in the same manner as in Example 1, a waveguide with extremely low scattering loss could be obtained.
（実施例３）
本実施例では上記実施例２と同様に−ｍ蒸着法によりＥ
ｒイオンの添加された５１０２ ＴｉＯ□のコア用ガ
ラスＷＡ１１を基板５上に形成した。(Example 3) In this example, as in Example 2 above, E
A core glass WA11 of 5102 TiO□ doped with r ions was formed on the substrate 5.
この場合に用いたタブレットは次のように形成されてい
る。先ず、ＳｉＯ２とＴ ｔ Ｏ２の粉末を重量比９９
対１の割合で混合し、これを１００℃でホットプレスし
た後、１５００°Ｃの温度で熱処理してタブレットを得
る。このタブレットをＥ ｒ Ｃ］ ｓを無水アルコー
ル液に０．５Ｑ、／溶かした府中に２４時間浸した後、
０□とＨｅの雰囲気中で乾城し、再度１７００℃の温度
で熱処理することにより焼結密度か９３％で１００μｍ
程度の粒子の塊からなる焼結体のタブレットとした。The tablet used in this case was formed as follows. First, the weight ratio of SiO2 and T t O2 powders was 99.
They are mixed at a ratio of 1:1, hot pressed at 100°C, and then heat treated at a temperature of 1500°C to obtain tablets. After soaking this tablet in Fuchu for 24 hours, in which 0.5 Q of E r C]s was dissolved in anhydrous alcohol solution,
By dry casting in an atmosphere of 0□ and He and heat-treating again at a temperature of 1700°C, the sintered density was 93% and 100 μm.
It was made into a sintered body tablet consisting of a mass of particles of about 100 mL.
このタブレットを用いた場合にも、基板５上に形成され
たコア用ガラスｐｉ！１１中には数μｍの微粒子は全く
混入せず、透明で均質なコア用ガラス１１１１を形成す
ることができ、低損失の導波路を作成することができた
。なお、コア用ガラス膜１１中へのＥｒイオンの添加量
は約２０００ｐ ｐ ｍであった。Even when this tablet is used, the core glass pi! formed on the substrate 5! No fine particles of several μm were mixed in the core glass 1111, which was transparent and homogeneous, and a waveguide with low loss could be created. Note that the amount of Er ions added into the core glass film 11 was about 2000 ppm.
（実施例４）
本実施例では実施例２と同様に一源蒸着法によりＥｒイ
オンとＦイオンの添加されたＳ ｉ Ｏ２Ｔ ｆ Ｏ２
のコア用ガラス膜１１を基板５上に厚さ７μｍ形成した
。この場合に用いたタブレットは次のように形成されて
いる。先ず、Ｓ ｉ Ｏ２、Ｔ ｉ Ｏ２及びＥｒＦｚ
の粉末を重量比８９：１：１０の割合で混合し、これを
１０００℃でホットプレスした後、１７００℃の温度で
熱処理することにより焼結密度９０％以上で１００μｍ
程度の粒子の塊からなる焼結体のタブレットとした。(Example 4) In this example, as in Example 2, S i O2T f O2 to which Er ions and F ions were added by the single-source evaporation method was used.
A core glass film 11 was formed on the substrate 5 to a thickness of 7 μm. The tablet used in this case was formed as follows. First, S i O2, T i O2 and ErFz
The powders were mixed at a weight ratio of 89:1:10, hot pressed at 1000°C, and then heat treated at 1700°C to achieve a sintered density of 90% or more and 100 μm.
It was made into a sintered body tablet consisting of a mass of particles of about 100 mL.
このタブレットを用いることにより散乱中心となる微粒
子の混入がなく、約５００ｐｐｍのＥｒイオンと、Ｆイ
オンの添加された５ｉＯ２−ＴＭ０１のコア用ガラス膜
１１を得ることができ、低損失の導波路を作成すること
ができた。By using this tablet, it is possible to obtain a core glass film 11 of 5iO2-TM01 doped with approximately 500 ppm of Er ions and F ions without the inclusion of fine particles that become scattering centers, and to create a low-loss waveguide. I was able to create it.
（実施例５）
本実施例では実施例２と同様に一源蒸着法によりＥｒ−
Ｎｄ及びＦイオンの添加されたＳ ｉ Ｏ２Ｔ ｉ Ｏ
ｔのコア用ガラスＭ１１を基板５上に厚さ１μｍ形成し
た。この場合には、タブレットとして、５ｔｏ２、Ｔｉ
１２、ＥｒＦｚ及びＮｄＦ、の粉末を重量比８５：１：
１０：４の割合で混合し、これを実施例４と同様に熱処
理したものを用いた。(Example 5) In this example, Er-
S i O2T i O doped with Nd and F ions
Core glass M11 of t was formed on the substrate 5 to a thickness of 1 μm. In this case, as a tablet, 5to2, Ti
12, ErFz and NdF powder at a weight ratio of 85:1:
They were mixed at a ratio of 10:4 and heat treated in the same manner as in Example 4.
これにより作成されたのＥｒ、Ｎｄ及びＦイオンの添加
した導波路は、波長１．３μｍ帯及び１．５μｍ帯での
増幅器用として期待することができる。The thus created waveguide doped with Er, Nd, and F ions can be expected to be used in amplifiers in the wavelength band of 1.3 μm and 1.5 μm.
なお、本発明は上記実施例に限定されるものではなく、
例えば希土類元素としてＥｒ、Ｎｄ以外に、Ｙｂ、Ｃｅ
、Ｈｏ、Ｔｍなどを用いてもよく、また屈折率制御用酸
化物として、Ｐ、Ｇｅ、Ｔｉ−Ａ１．Ｚｎ、Ｂ−Ｆなど
を少なくとも一種類含んだ酸化物を用いるようにしても
よい。Note that the present invention is not limited to the above embodiments,
For example, in addition to Er and Nd, rare earth elements include Yb and Ce.
, Ho, Tm, etc. may be used, and P, Ge, Ti-A1. An oxide containing at least one type of Zn, B-F, etc. may be used.
［発明の効果］
以上要するに本発明によれば、タブレットに電子ビーム
を照射して基板表面に膜を形成する際、タブレットが１
０μｍ以上の粒子の塊からなっているなめ、照射部分の
周辺の粒子が同時に飛散することがなくなり、従って微
粒子の混入しないコア用ガラス膜を形成することができ
、低損失のガラス導波路を作成することができる。[Effects of the Invention] In summary, according to the present invention, when forming a film on the substrate surface by irradiating the tablet with an electron beam, the tablet
Since the lick is made up of agglomerates of particles of 0 μm or larger, particles around the irradiated area will not be scattered at the same time, making it possible to form a glass film for the core that does not contain fine particles, creating a glass waveguide with low loss. can do.
第１図は本発明に係る希土類元素添加導波路の製造方法
において用いられる電子ビーム蒸着装置の概略断面図、
第２図は同製造方法の工程を示す図、第３図は同製造方
法において用いたタブレフトの表面構造を示す図、第４
図は本発明者が先に提案した製造方法で作成したコア用
ガラス膜の表面構造を示す図、第５図は同製造方法にお
いて用いたタプレ・ソトの表面構造を示す図である。
図中、１は電子ビーム蒸着装！、４ａ、４ｂは蒸発源、
５は基板、９．１０はタブレット、１１はコア用ガラス
膜、１４はコア、１５はガラス膜である。FIG. 1 is a schematic cross-sectional view of an electron beam evaporation apparatus used in the method for manufacturing a rare earth element-doped waveguide according to the present invention;
Fig. 2 is a diagram showing the steps of the same manufacturing method, Fig. 3 is a diagram showing the surface structure of the tab left used in the same manufacturing method, and Fig. 4 is a diagram showing the surface structure of the tab left used in the same manufacturing method.
The figure shows the surface structure of a core glass film produced by the production method previously proposed by the present inventor, and FIG. 5 shows the surface structure of Taplet-Soto used in the same production method. In the figure, 1 is an electron beam evaporation system! , 4a, 4b are evaporation sources,
5 is a substrate, 9.10 is a tablet, 11 is a glass film for core, 14 is a core, and 15 is a glass film.
Claims (1)
％以上で粒径が１０μｍ以上の粒子の塊からなるタブレ
ットを電子ビーム蒸着法により蒸発させて低屈折率層を
有する基板上に希土類元素を含むＳｉＯ＿２のコア用ガ
ラス膜を形成する工程と、その基板全体を高温熱処理す
る工程と、上記コア用ガラス膜をホトリングラフィ及び
ドライエッチングにより断面略矩形のコアに加工する工
程と、基板上のコア全体に低屈折率のガラス膜を被覆す
る工程とからなる希土類元素添加導波路の製造方法。 ２、上記タブレットが、希土類元素を含むタブレットと
ＳｉＯ＿２を含むタブレットとからなり、これらが個別
の蒸発源から蒸発される請求項１記載の希土類元素添加
導波路の製造方法。 ３、上記タブレットが、少なくとも２種類の希土類元素
を含んでいる請求項１記載の希土類元素添加導波路の製
造方法。 ４、上記タブレットが、ガラス化されている請求項１記
載の希土類元素添加導波路の製造方法。 ５、上記タブレットが、Ｆを含んでいる請求項１記載の
希土類元素添加導波路の製造方法。 ６、上記タブレットが、多孔質タブレットに希土類元素
を含んだ液体を含浸させ、これを乾燥及び高温熱処理し
て形成されている請求項１記載の希土類元素添加導波路
の製造方法。 ７、上記タブレットが、原料粉末を混合し、ホットプレ
スにより焼き固めて形成されている請求項１記載の希土
類元素添加導波路の製造方法。[Claims] 1. Contains rare earth elements and SiO_2, and has a sintered density of 90
% or more and a particle size of 10 μm or more by electron beam evaporation to form a core glass film of SiO_2 containing a rare earth element on a substrate having a low refractive index layer; a step of heat-treating the entire substrate at a high temperature; a step of processing the core glass film into a core having a substantially rectangular cross section by photolithography and dry etching; and a step of coating the entire core on the substrate with a glass film with a low refractive index. A method for manufacturing a rare earth element-doped waveguide comprising: 2. The method for manufacturing a rare earth element-doped waveguide according to claim 1, wherein the tablet is composed of a rare earth element-containing tablet and a SiO_2-containing tablet, and these tablets are evaporated from separate evaporation sources. 3. The method for manufacturing a rare earth element-doped waveguide according to claim 1, wherein the tablet contains at least two types of rare earth elements. 4. The method for manufacturing a rare earth element-doped waveguide according to claim 1, wherein the tablet is vitrified. 5. The method for manufacturing a rare earth element-doped waveguide according to claim 1, wherein the tablet contains F. 6. The method for manufacturing a rare earth element-doped waveguide according to claim 1, wherein the tablet is formed by impregnating a porous tablet with a liquid containing a rare earth element, drying it, and subjecting it to high-temperature heat treatment. 7. The method of manufacturing a rare earth element-doped waveguide according to claim 1, wherein the tablet is formed by mixing raw material powders and baking and solidifying the mixture using a hot press.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2128317A JP2747359B2 (en) | 1990-05-18 | 1990-05-18 | Manufacturing method of rare earth element doped waveguide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2128317A JP2747359B2 (en) | 1990-05-18 | 1990-05-18 | Manufacturing method of rare earth element doped waveguide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0422906A true JPH0422906A (en) | 1992-01-27 |
| JP2747359B2 JP2747359B2 (en) | 1998-05-06 |
Family
ID=14981784
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2128317A Expired - Fee Related JP2747359B2 (en) | 1990-05-18 | 1990-05-18 | Manufacturing method of rare earth element doped waveguide |
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| Country | Link |
|---|---|
| JP (1) | JP2747359B2 (en) |
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| KR101386523B1 (en) | 2011-12-30 | 2014-04-18 | 한국세라믹기술원 | Low density ingot for electron beam evaporation and method for manufacturing the same |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61139637A (en) * | 1984-12-12 | 1986-06-26 | Hitachi Metals Ltd | Target for sputter and its manufacture |
| JPS63111135A (en) * | 1986-10-29 | 1988-05-16 | Hitachi Metals Ltd | Manufacture of rare earth-transition metal target |
| JPS63290272A (en) * | 1987-05-21 | 1988-11-28 | Hitachi Metals Ltd | Production of rare earth element-transition metal target material |
| JPH01142078A (en) * | 1987-11-27 | 1989-06-02 | Matsushita Electric Ind Co Ltd | Sputtering target |
| JPH01287206A (en) * | 1988-05-13 | 1989-11-17 | Kobe Steel Ltd | Porous sintered body for infiltrated complex target material and manufacture thereof |
| JPH02146504A (en) * | 1988-11-29 | 1990-06-05 | Fujikura Ltd | Production of nonlinear light guide |
| JPH0353202A (en) * | 1989-07-21 | 1991-03-07 | Hitachi Cable Ltd | Production of waveguide added with rare earth element |
-
1990
- 1990-05-18 JP JP2128317A patent/JP2747359B2/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61139637A (en) * | 1984-12-12 | 1986-06-26 | Hitachi Metals Ltd | Target for sputter and its manufacture |
| JPS63111135A (en) * | 1986-10-29 | 1988-05-16 | Hitachi Metals Ltd | Manufacture of rare earth-transition metal target |
| JPS63290272A (en) * | 1987-05-21 | 1988-11-28 | Hitachi Metals Ltd | Production of rare earth element-transition metal target material |
| JPH01142078A (en) * | 1987-11-27 | 1989-06-02 | Matsushita Electric Ind Co Ltd | Sputtering target |
| JPH01287206A (en) * | 1988-05-13 | 1989-11-17 | Kobe Steel Ltd | Porous sintered body for infiltrated complex target material and manufacture thereof |
| JPH02146504A (en) * | 1988-11-29 | 1990-06-05 | Fujikura Ltd | Production of nonlinear light guide |
| JPH0353202A (en) * | 1989-07-21 | 1991-03-07 | Hitachi Cable Ltd | Production of waveguide added with rare earth element |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2747359B2 (en) | 1998-05-06 |
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