JPH02263800A - Production of oxide single crystal electron beam sensor - Google Patents
Production of oxide single crystal electron beam sensorInfo
- Publication number
- JPH02263800A JPH02263800A JP8155889A JP8155889A JPH02263800A JP H02263800 A JPH02263800 A JP H02263800A JP 8155889 A JP8155889 A JP 8155889A JP 8155889 A JP8155889 A JP 8155889A JP H02263800 A JPH02263800 A JP H02263800A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- electron beam
- oxide single
- beam sensor
- production
- 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 37
- 238000010894 electron beam technology Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000007788 roughening Methods 0.000 claims abstract description 4
- 238000003486 chemical etching Methods 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims description 5
- 239000000843 powder Substances 0.000 abstract description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 9
- 238000005530 etching Methods 0.000 abstract description 2
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 238000005136 cathodoluminescence Methods 0.000 description 7
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000004453 electron probe microanalysis Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 125000003821 2-(trimethylsilyl)ethoxymethyl group Chemical group [H]C([H])([H])[Si](C([H])([H])[H])(C([H])([H])[H])C([H])([H])C(OC([H])([H])[*])([H])[H] 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000002123 temporal effect Effects 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、走査型電子顕微鏡（ＳＥＭ）や、ＥＰＭＡ装
置等に用いられる電子線センサに関し、特にその酸化物
単結晶螢光体の製造方法に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to an electron beam sensor used in a scanning electron microscope (SEM), an EPMA device, etc., and particularly relates to a method for manufacturing an oxide single crystal phosphor thereof. It is related to.
［従来の技術］
従来、電子線センサとして蛍光体粉末をそのまま用いる
場合と、蛍光イオンをドープした酸化物単結晶から切り
出し加工したものを熱処理し、その後メカノケミカルボ
リジング法により表面を鏡面仕上して用いる場合とがあ
った。しかし、後者の酸化物単結晶は、前者の蛍光体粉
末（製品名、Ｐ−４７）に比べ耐久力はあるが発光効率
が悪い。[Prior art] Conventionally, phosphor powder has been used as an electron beam sensor as it is, or it has been cut and processed from an oxide single crystal doped with fluorescent ions, heat-treated, and then the surface has been mirror-finished using a mechanochemical boriding method. There were cases where it was used. However, the latter oxide single crystal is more durable than the former phosphor powder (product name: P-47) but has poor luminous efficiency.
そのため、高エネルギー電子線を用いるＴＥＭ装置など
では酸化物単結晶を用いることができるが、エネルギー
の低い電子線を用いるＳＥＭ等では酸化物中結晶は用い
ることができず、蛍光体粉末が用いられている。Therefore, oxide single crystals can be used in TEM devices that use high-energy electron beams, but crystals in oxides cannot be used in SEMs that use low-energy electron beams, and phosphor powders are used. ing.
［発明が解決しようとする課題］
しかしながら、蛍光体粉末（Ｐ−４７）の場合、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
ればならないという不都合が生じた。[Problems to be Solved by the Invention] However, in the case of the phosphor powder (P-47), it deteriorates due to ultraviolet rays and electron beams, so it has to be replaced every few years.
そのために高エネルギー及び低エネルギーのいずれにお
いても使用でき、電子線、及び紫外線に耐久力がある高
効率の電子線センサが要求されている。Therefore, there is a need for a highly efficient electron beam sensor that can be used at both high and low energy and is resistant to electron beams and ultraviolet rays.
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方法の改良により高効率
化し、耐久力のある高効率な酸化物単結晶電子線センサ
を提供することにある。Therefore, the 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 oxide single crystal electron beam sensor. It is in.
［課題を解決するための手段］
本発明によれば、蛍光イオンをドープした酸化物単結晶
よりなる電子線センサの製造方法において、前記酸化物
単結晶の板の両面を鏡面研磨し、該鏡面研磨した両面の
電子線の照射面となる面を粗面加工し、その後、ケミカ
ルエツチングを行う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, both sides of the oxide single crystal plate are mirror-polished, and the mirror-finished A method for manufacturing an oxide single crystal electron beam sensor is obtained, which comprises roughening the polished surfaces of both surfaces to be irradiated with an electron beam, and then chemically etching them.
［作 用］
本発明においては、電子線センサとして用いられる酸化
物単結晶の表面を荒すことにより、電子線の吸収量が大
きくなり高効率となる。さらに、ケミカルエツチングで
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、有効に螢光イオンを励起で
きるため、発光効率が向上する。[Function] In the present invention, by roughening the surface of the oxide single crystal used as an electron beam sensor, the amount of electron beam absorption increases, resulting in high efficiency. Furthermore, by removing the process-strained layer by chemical etching, energy propagation in the crystal becomes smoother and fluorescent ions can be excited effectively, thereby improving 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.
本実施例では、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、超音波ロータリー
加工機で打抜いた単結晶板（直径３ｍｍ、厚さ１ｍｍ）
を用いた。この単結晶板の両面をメカノケミカルボリジ
ングして鏡面仕上げした試料、この鏡面仕上げした単結
晶板の片面（電子線照射面）を＃４００研磨材で荒削り
した試料、さらにこの荒削りした単結晶をリン酸中に浸
漬して加熱し３分程度エツチングし、表面の加工歪み層
を取り除いた試料、及び蛍光粉末（Ｐ−４７）の４種類
を用意し、各々の電子線センサの電子線発光強度（カソ
ードルミネッセンス）をＥＰＭＡ装置で評価した。In this example, a single crystal plate (diameter 3 mm, thickness 1 mm) was punched from Ce:YAG raw stone, which is an oxide single crystal containing Ce as a fluorescent ion, using an ultrasonic rotary processing machine.
was used. A sample in which both sides of this single crystal plate were mechanochemically borated to a mirror finish, a sample in which one side (electron beam irradiation surface) of this mirror finished single crystal plate was roughly ground with #400 abrasive, and a sample in which this rough ground single crystal was Four types of samples were prepared: a sample whose surface was immersed in phosphoric acid, heated and etched for about 3 minutes to remove the processed strain layer, and a fluorescent powder (P-47), and the electron beam emission intensity of each electron beam sensor was measured. (Cathodoluminescence) was evaluated using an EPMA apparatus.
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となっている。電子線のビ
ーム径は１００μｍ、繰り返し１００Ｈｚ、加速電圧１
０ｋＶで測定した。その結果を第１図に示す。It should be noted that the surface of the etched sample has more pronounced irregularities than the rough-cut sample. The beam diameter of the electron beam is 100 μm, the repetition rate is 100 Hz, and the acceleration voltage is 1.
Measured at 0kV. The results are shown in FIG.
ケミカルポリシン・グした試料■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■では２．２、
荒削り後エツチングした試料■で４、蛍光粉末体（Ｐ−
４７）■で５，１のカソードルミネッセンス強度が夫々
得られた。蛍光粉末体■は測定開始時に試料■の１．２
倍のカソードルミネッセンス強度を示すが、測定開始の
４０秒後には試料■と同程度まで低下する。更に時間が
経過すると、試料■の１／２にまでカソードルミネッセ
ンス強度が低下する。酸化物単結晶電子線センサ（試料
■、■、■）では、この様な出力の低下が全く見られな
かった。If the cathodoluminescence intensity of the chemically polished sample (■) is 1, that of the rough-cut sample (■) is 2.2,
4. Fluorescent powder (P-
47) Cathodoluminescence intensities of 5 and 1 were obtained in (1) and 1, respectively. Fluorescent powder ■ is 1.2% of sample ■ at the start of measurement.
Although it shows twice the cathodoluminescence intensity, it drops to the same level as sample ① 40 seconds after the start of the measurement. As time further elapses, the cathodoluminescence intensity decreases to 1/2 of that of sample (2). No such decrease in output was observed in the oxide single crystal electron beam sensors (samples ①, ②, ②).
［発明の効果］
以上述べたごとく、本発明の酸化物単結晶電子線センサ
の製造方法によれば、鏡面加工した電子線センサの電子
線照射面を荒削りした後ケミカルエツチングすることに
より、蛍光体粉末と同程度の発光効率を示す酸化物単結
晶電子線センサを得ることができる。[Effects of the Invention] As described above, according to the method for manufacturing an oxide single crystal electron beam sensor of the present invention, the electron beam irradiation surface of the mirror-finished electron beam sensor is rough-cut and then chemically etched to form a phosphor. An oxide single crystal electron beam sensor that exhibits luminous efficiency comparable to that of powder can be obtained.
第１図は本発明の実施例に係る酸化物単結晶電子ｉセン
サのカソードルミネッセンスの時間変化を示す図で、比
較例として従来の螢光体粉末、鏡面加工した酸化物単結
晶試料、・及びこの鏡面加工した酸化物単結晶を荒削り
した試料についても併せて示した。
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：ＹＡＧ単結晶、
３は＃４００研磨材で研磨した後、ケミカルエツチング
したＣｅ：ＹＡＧ単晶、４は粉末蛍光体（Ｐ−４７）で
、それぞれのカソードルミネッセンス強度を示す。
以下余゛白FIG. 1 is a diagram showing the temporal change in cathodoluminescence of an oxide single crystal electronic i-sensor according to an example of the present invention.As a comparative example, a conventional phosphor powder, a mirror-finished oxide single crystal sample, and A rough-cut sample of this mirror-finished oxide single crystal is also shown. In the figure, 1 is a Ce:YAG single crystal whose surface has been mirror-polished, 2 is a Ce:YAG single crystal whose surface has been polished with #400 abrasive,
3 is a Ce:YAG single crystal that has been chemically etched after polishing with a #400 abrasive, and 4 is a powdered phosphor (P-47), and the cathodoluminescence intensity of each is shown. Below is the margin
Claims (1)
線センサの製造方法において、前記酸化物単結晶の板の
両面を鏡面研磨し、該鏡面研磨した両面の電子線の照射
面となる面を粗面加工し、その後、ケミカルエッチング
を行う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, both sides of the oxide single crystal plate are mirror-polished, and the surfaces of the mirror-polished surfaces that will be irradiated with an electron beam are A method for manufacturing an oxide single crystal electron beam sensor, comprising roughening the surface and then performing chemical etching.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8155889A JPH02263800A (en) | 1989-04-03 | 1989-04-03 | Production of oxide single crystal electron beam sensor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8155889A JPH02263800A (en) | 1989-04-03 | 1989-04-03 | Production of oxide single crystal electron beam sensor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02263800A true JPH02263800A (en) | 1990-10-26 |
Family
ID=13749619
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8155889A Pending JPH02263800A (en) | 1989-04-03 | 1989-04-03 | Production of oxide single crystal electron beam sensor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02263800A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106270523A (en) * | 2016-09-30 | 2017-01-04 | 中国人民大学 | A kind of large-area ultrathin monocrystalline and method for fast growing thereof |
-
1989
- 1989-04-03 JP JP8155889A patent/JPH02263800A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106270523A (en) * | 2016-09-30 | 2017-01-04 | 中国人民大学 | A kind of large-area ultrathin monocrystalline and method for fast growing thereof |
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