JPH03139593A - Manufacture of electron beam sensor comprising oxide single crystal - Google Patents
Manufacture of electron beam sensor comprising oxide single crystalInfo
- Publication number
- JPH03139593A JPH03139593A JP27579889A JP27579889A JPH03139593A JP H03139593 A JPH03139593 A JP H03139593A JP 27579889 A JP27579889 A JP 27579889A JP 27579889 A JP27579889 A JP 27579889A JP H03139593 A JPH03139593 A JP H03139593A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- oxide single
- electron beam
- beam sensor
- thickness
- 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 42
- 238000010894 electron beam technology Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims abstract description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 5
- 238000003754 machining Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 7
- 238000007788 roughening Methods 0.000 abstract description 5
- 238000003486 chemical etching Methods 0.000 abstract 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 238000005136 cathodoluminescence Methods 0.000 description 7
- 238000005498 polishing Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 5
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 4
- 238000005530 etching Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006332 epoxy adhesive Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
- ing And Chemical Polishing (AREA)
- Measurement Of Radiation (AREA)
- 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、走査型電子顕微鏡（ＳＥＭ）等に用いられる
電子線センサに関し、詳しくは薄板状の酸化物Ｉｌｌ結
晶蛍光体の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to an electron beam sensor used in a scanning electron microscope (SEM), etc., and more particularly to a method for manufacturing a thin plate-shaped oxide Ill crystal phosphor.
［従来の技術］
従来、電子線センサとして、蛍光体粉末（Ｐ−４６）を
用いた場合、紫外線や電子線によって劣化するため数年
ごとに交換しなければならなかった。そのため、蛍光イ
オンをドーブした酸化物単結晶から切出し加工後、熱処
理し、メカノケミカルポリッシング法により表面を鏡面
仕上げて用いている。[Prior Art] Conventionally, when phosphor powder (P-46) is used as an electron beam sensor, it has to be replaced every few years because it deteriorates due to ultraviolet rays and electron beams. Therefore, the material is cut out from an oxide single crystal doped with fluorescent ions, heat-treated, and finished with a mirror-like surface using a mechanochemical polishing method.
［発明が解決しようとする課題］
酸化物単結晶は、蛍光体粉末（製品名、Ｐ−４６）に比
べて耐久力はあるが、一般に単結晶の屈折率が大きいた
めに、結晶内から十分な光信号を取り出せなかった。[Problems to be Solved by the Invention] Oxide single crystals are more durable than phosphor powders (product name: P-46), but because the refractive index of single crystals is generally large, they cannot be easily removed from within the crystal. I couldn't get a proper optical signal.
即ち、電子線センサ材料として、酸化物単結晶板が用い
られているが、この酸化物単結晶板は屈折率が大きいた
めに、厚さが厚い程入射光線が全反射によって結晶内に
閉込められるので、できるだけ厚さが薄いもの程、光が
透過しやすく有利である。また、結晶内での反射に関し
ても薄いほど、その反射回数が多くなり感度を高めるこ
とができる。In other words, an oxide single crystal plate is used as an electron beam sensor material, but since this oxide single crystal plate has a large refractive index, the thicker the thickness, the more the incident light rays are confined within the crystal due to total reflection. Therefore, the thinner the material is, the easier it is for light to pass through, which is advantageous. Also, regarding reflection within the crystal, the thinner the crystal, the more times the crystal will be reflected, and the sensitivity can be increased.
酸化物単結晶の厚さは、電子線の波長１μｍ程度が理想
的であるが、従来は研磨等の加工上の問題から厚さ１０
０μｍ程度が限界であった。The ideal thickness of an oxide single crystal is about 1 μm at the wavelength of the electron beam, but conventionally it has been reduced to a thickness of about 10 μm due to processing problems such as polishing.
The limit was about 0 μm.
そこで、本発明の技術的課題は、電子線センサとして耐
久力のある酸化物単結晶を加工法の改良により、高効率
化し、耐久力のある高効率な電子線センサを提供するこ
とにある。Therefore, a technical problem of the present invention is to improve the efficiency of a durable oxide single crystal as an electron beam sensor by improving the processing method, and to provide a durable and highly efficient electron beam sensor.
［課題を解決するための手段］
本発明によれば、電子線センサに用いる蛍光イオンをド
ーブした酸化物単結晶からなる電子線センサの製造方法
において、該酸化物単結晶を機械加工により厚みを数十
μｍの円板状に成形し、表面を鏡面仕上げした後、両面
を粗面仕上げし、熱リン酸でケミカルエツチングしたこ
とを特徴とする酸化物単結晶電子線センサの製造方法が
得られる。[Means for Solving the Problems] According to the present invention, in a method for manufacturing an electron beam sensor made of an oxide single crystal doped with fluorescent ions for use in an electron beam sensor, the thickness of the oxide single crystal is reduced by machining. A method for manufacturing an oxide single crystal electron beam sensor is obtained, which is characterized in that it is formed into a disk shape of several tens of micrometers, the surface is mirror-finished, then both sides are rough-finished and chemically etched with hot phosphoric acid. .
本発明は、向上した研磨技術、即ち、酸化物単結晶板の
平面性と接着技術とにより、厚さ数十μｍ程度に形成さ
れた単結晶板を使用した。The present invention uses a single-crystal plate formed to a thickness of about several tens of μm using improved polishing technology, that is, flatness of the oxide single-crystal plate and adhesion technology.
また、酸化物単結晶板は鏡面加工後、電子線照射面に粗
面加工を施すと、エネルギー効率が上昇する、即ち、カ
ソードルミネッセンス強度が増加することは、知られて
いる。Furthermore, it is known that when an oxide single crystal plate is mirror-finished and then subjected to roughening on the electron beam irradiated surface, the energy efficiency increases, that is, the cathodoluminescence intensity increases.
本発明では、電子線照射面に対向する面に、即ち、両面
に粗面加工を施すことにより、カソードルミネッセンス
強度がさらに向上することを見出し、本発明を完成する
に至ったものである。In the present invention, the present invention was completed based on the discovery that the cathode luminescence intensity can be further improved by roughening the surface facing the electron beam irradiation surface, that is, both surfaces.
［作 用］
本発明の電子線センサの両表面を荒らすことにより、電
子線の吸収量が大きくなり、高効率となる。[Function] By roughening both surfaces of the electron beam sensor of the present invention, the amount of electron beam absorption increases, resulting in high efficiency.
さらに、加工歪層を除去することによって、結晶中での
エネルギーの伝播がスムーズになり、有効に発行イオン
を励起できるため、発光効率が向上する。Furthermore, by removing the process-strained layer, energy propagation in the crystal becomes smoother and emitted ions can be excited effectively, resulting in improved luminous efficiency.
［実施例］ 次に、本発明の実施例について説明する。[Example] Next, examples of the present invention will be described.
蛍光イオンとして、Ｃｅ ”を有する酸化物単結晶であ
るＣｅ：ＹＡＧ原石より、超音波ロータリー加工機で打
抜いた単結晶（φ３Ｘ２ｍｍ）を素材として用いた。蛍
光イオンとしてＣｅを含有する酸化物単結晶であるＣｅ
：ＹＡＧ原石より、題名波ロータリ加工機で打抜いた単
結晶（φ３×１ｍｍ）を用いた。薄板状に加工する際、
問題となるのは、接着剤や加工歪層による板の反りで、
これを防ぐために次のような加工を行った。As a fluorescent ion, we used a single crystal (φ3 x 2 mm) punched from Ce:YAG raw stone, which is an oxide single crystal containing Ce'', using an ultrasonic rotary processing machine.As a fluorescent ion, we used an oxide single crystal containing Ce. Crystal Ce
: A single crystal (φ3 x 1 mm) punched from YAG raw stone using a title wave rotary processing machine was used. When processing into a thin plate,
The problem is the warping of the board due to the adhesive and the processed strained layer.
To prevent this, the following processing was performed.
平面度λ／１０（λ−０．６３μｍ）で仕上げられたφ
１０１０Ｘ２０のＹＡＧ円板上に、粘性の小さなワック
スを用いて、φ３Ｘ２ｍｍのＣｅ：ＹＡＧを接着してか
ら、平面度λ／１０の精度でメカノケミカル仕上げを行
った。φ finished with flatness λ/10 (λ-0.63μm)
Ce:YAG of φ3×2 mm was adhered onto a 1010×20 YAG disk using wax with low viscosity, and then mechanochemical finishing was performed with a flatness accuracy of λ/10.
この試料をＹＡＧ円板より取外して、裏返して接着した
。この場合、ＹＡＧ円板及び試料の表面状態が、λ／１
０であるため、真空接着が可能であり、接着剤を使わず
に接着できる。This sample was removed from the YAG disk, turned over, and bonded. In this case, the surface condition of the YAG disk and sample is λ/1
Since it is 0, vacuum bonding is possible and bonding can be performed without using adhesive.
但し、加工率に剥離する場合があるので、試料の側面だ
けをエポキシ系の接着剤で接着した。この結晶を粗加工
で１００μｍまで研磨した後、鏡面研磨で５０μｍ薄く
してから、メカノケミカルポリッシングを行った。研磨
終了後、有機溶剤中で加熱剥離して、両面を＃３０００
の研磨材で加工した。However, since peeling may occur due to the processing rate, only the sides of the sample were adhered with an epoxy adhesive. This crystal was roughly polished to a thickness of 100 μm, mirror polished to a thickness of 50 μm, and then mechanochemical polishing was performed. After polishing, heat peeling in an organic solvent and coat both sides with #3000.
Processed with abrasive material.
メカノケミカルポリッシング鏡面仕上げした試料１、こ
の単結晶板の両面（電子線照射面）を＃４００研磨材で
、厚さ数十μｍに、粗削りした試料２、さらに粗削りし
た試料２を１８０℃の熱リン酸でエツチングし、該酸化
物単結晶蛍光体の表面を加工歪み層を取り除くことによ
って、φ３Ｘ２５μｍの両面が荒れた（ｅ：ＹＡＧ素子
試料３が得られた。Sample 1 was mechanochemically polished to a mirror finish, Sample 2 was rough-ground to a thickness of several tens of micrometers on both sides (electron beam irradiated surface) of this single crystal plate with #400 abrasive, and Sample 2 was further rough-ground and heated at 180°C. By etching the surface of the oxide single crystal phosphor with phosphoric acid and removing the strained layer, both surfaces of φ3×25 μm were roughened (e: YAG element sample 3 was obtained).
さらに熱リン酸で３分間程度エツチングし、及び蛍光粉
末（Ｐ−４６）の４種類を用意し、各々の電子線センサ
の電子線蛍光強度（カソードルミネッセンス）をＥＰＭ
Ａ装置で評価した。Furthermore, etching was performed for about 3 minutes with hot phosphoric acid, four types of fluorescent powder (P-46) were prepared, and the electron beam fluorescence intensity (cathode luminescence) of each electron beam sensor was measured by EPM.
Evaluation was made using A device.
尚、上記のエツチングした試料の表面は、荒削りした試
料よりも凹凸状態が更に、明確になっている。It should be noted that the surface of the etched sample has more pronounced irregularities than the rough-cut sample.
電子線ビーム径は、１００μｍ、繰返し１００Ｈｚ、加
速電圧１０ｋＶで測定した。The electron beam diameter was 100 μm, the repetition rate was 100 Hz, and the acceleration voltage was 10 kV.
その結果を第１図に示す。The results are shown in FIG.
尚、研磨は単結晶を接着し、平担面になるようにして、
平面性を高めた。In addition, when polishing, the single crystal is glued together so that it becomes a flat surface.
Improved flatness.
ケミカルポリッシングした試料１のカソードルミネッセ
ンス強度を１とすると、荒削りした試料２では３、荒削
り後、エツチングした試料３で６、蛍光粉末体４で５．
１のカソードルミネセンス強度が得られた。If the cathodoluminescence intensity of chemically polished sample 1 is 1, rough-cut sample 2 has an intensity of 3, rough-cut and etched sample 3 has an intensity of 6, and fluorescent powder 4 has an intensity of 5.
A cathodoluminescence intensity of 1 was obtained.
蛍光粉末体４は、測定開始時に、試料３と路間等のカソ
ードルミネッセンス強度を示すが、測定開始の３分後に
は、試料３の１／３までカソードルミネッセンス強度が
減少低下する。The fluorescent powder 4 exhibits a cathodoluminescence intensity between the sample 3 and the path at the start of the measurement, but the cathodoluminescence intensity decreases to 1/3 of that of the sample 3 three minutes after the start of the measurement.
また、酸化物単結晶電子線センサ（試料１，２゜３）で
は、このような出力の低下が、全く見られなかった。Further, in the oxide single crystal electron beam sensors (Samples 1 and 2°3), such a decrease in output was not observed at all.
［発明の効果コ
以上述べたように、本発明の電子線センサの製造方法に
よれば、酸化物単結晶を機械加工により厚みを数十μｍ
の円板状に成形した後、両面を粗面仕上げし、ケミカル
エツチングすることにより、蛍光体粉末に比べて高い発
光効率を呈する酸化物単結晶蛍光体？Ｗ板が得られる。[Effects of the Invention] As described above, according to the method for manufacturing an electron beam sensor of the present invention, an oxide single crystal is machined to a thickness of several tens of μm.
An oxide single-crystal phosphor that exhibits higher luminous efficiency than phosphor powder by forming it into a disk shape, roughening both sides, and chemically etching it. A W plate is obtained.
第１図はカソードルミネッセンスの時間変化を示す図で
ある。
図中、１は表面を鏡面研磨したＣｅ：ＹＡＧ単結晶、２
は表面を＃４００研磨材で研磨したＣｅ：Ｙ Ａ Ｇ
１１１結晶、３１；！ ＃ ４００研磨材で研磨した後
、ケミカルエツチングしたＣｅ：ＹＡＧ単結晶、４は粉
末蛍光体（Ｐ−４６）て夫々のカソードルミネッセンス
強度を示す。FIG. 1 is a diagram showing changes in cathodoluminescence over time. In the figure, 1 is a Ce:YAG single crystal with mirror polished surface, 2
Ce: Y A G whose surface was polished with #400 abrasive
111 crystals, 31;! #4 shows the cathodoluminescence intensity of a chemically etched Ce:YAG single crystal after polishing with a 400 abrasive, and 4 is a powdered phosphor (P-46).
Claims (1)
物単結晶からなる電子線センサの製造方法において、該
酸化物単結晶を機械加工により厚みを数十μｍの円板状
に成形し、表面を鏡面仕上げした後、両面を粗面仕上げ
し、熱リン酸でケミカルエツチングしたことを特徴とす
る酸化物単結晶電子線センサの製造方法。1. In a method for manufacturing an electron beam sensor made of an oxide single crystal doped with fluorescent ions used in an electron beam sensor, the oxide single crystal is formed into a disk shape with a thickness of several tens of micrometers by machining, and the surface is mirror-finished. A method for manufacturing an oxide single crystal electron beam sensor, characterized in that after finishing, both surfaces are roughened and chemically etched with hot phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27579889A JPH03139593A (en) | 1989-10-25 | 1989-10-25 | Manufacture of electron beam sensor comprising oxide single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27579889A JPH03139593A (en) | 1989-10-25 | 1989-10-25 | Manufacture of electron beam sensor comprising oxide single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03139593A true JPH03139593A (en) | 1991-06-13 |
Family
ID=17560562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27579889A Pending JPH03139593A (en) | 1989-10-25 | 1989-10-25 | Manufacture of electron beam sensor comprising oxide single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03139593A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5105751A (en) * | 1988-05-05 | 1992-04-21 | Pfaff Industriemaschinen Gmbh | Process for carrying out a sewing operation with a sewing machine with needle feed |
| CZ305614B6 (en) * | 2014-11-07 | 2016-01-06 | Crytur, Spol.S R.O. | Modification method of monocrystalline scintillator surface and monocrystalline scintillator with surface modified by such a method |
-
1989
- 1989-10-25 JP JP27579889A patent/JPH03139593A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5105751A (en) * | 1988-05-05 | 1992-04-21 | Pfaff Industriemaschinen Gmbh | Process for carrying out a sewing operation with a sewing machine with needle feed |
| CZ305614B6 (en) * | 2014-11-07 | 2016-01-06 | Crytur, Spol.S R.O. | Modification method of monocrystalline scintillator surface and monocrystalline scintillator with surface modified by such a method |
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