JP2001262321A - Evaporating source in vacuum vapor deposition apparatus, and heating method thereof - Google Patents

Evaporating source in vacuum vapor deposition apparatus, and heating method thereof

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Publication number
JP2001262321A
JP2001262321A JP2000073500A JP2000073500A JP2001262321A JP 2001262321 A JP2001262321 A JP 2001262321A JP 2000073500 A JP2000073500 A JP 2000073500A JP 2000073500 A JP2000073500 A JP 2000073500A JP 2001262321 A JP2001262321 A JP 2001262321A
Authority
JP
Japan
Prior art keywords
evaporation source
heater
container
metal foil
evaporating source
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
Application number
JP2000073500A
Other languages
Japanese (ja)
Other versions
JP3438024B2 (en
Inventor
Kazuo Saito
和雄 斎藤
Takeshi Mizota
武志 溝田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
National Institute of Advanced Industrial Science and Technology AIST
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Priority to JP2000073500A priority Critical patent/JP3438024B2/en
Publication of JP2001262321A publication Critical patent/JP2001262321A/en
Application granted granted Critical
Publication of JP3438024B2 publication Critical patent/JP3438024B2/en
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Abstract

PROBLEM TO BE SOLVED: To provide an evaporating source in a vacuum vapor deposition apparatus, and a heating method thereof. SOLUTION: The evaporating source in the vacuum vapor deposition apparatus to efficiently heat the evaporating source comprises an evaporating source container formed of a conductive substance having a high melting point, an evaporating source supporting metal bar to support the container, a heater formed of a metal foil having a high melting point disposed below the evaporating source container, a heater power source to energize the heater, and an electron acceleration power source to apply to power between the evaporating source container and the heater. In the heating method using the evaporating source, the metal foil having a high melting point is energized and heated, the evaporating source container is radiated and heated by the radiation heat therefrom, the voltage is applied between the evaporating source container and the heater to a accelerate the electrons emitted from the surface of the metal foil and allow the evaporating source container irradiated therewith, and the vacuum evaporating source is efficiently heated.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、各種材料表面のコ
ーティングを行うための真空蒸着装置中の蒸発源の加熱
をより効率的に行うための技術に関するものであり、更
に詳しくは、真空蒸着装置中の蒸発源をより効率的に加
熱し得ると共に、装置の簡便な設計を可能とする蒸発
源、及びその加熱方法に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a technique for more efficiently heating an evaporation source in a vacuum evaporation apparatus for coating the surface of various materials, and more particularly, to a vacuum evaporation apparatus. The present invention relates to an evaporation source capable of heating an evaporation source therein more efficiently and enabling a simple design of an apparatus, and a heating method thereof.

【0002】[0002]

【従来の技術】従来、各種材料表面にコーティングを行
い、薄膜を形成する真空蒸着方式として、種々の方法が
開発されている。以下に、上記薄膜を製造するために従
来とられていた方法を列記する。 (1)通電加熱式蒸着法 この方法ではタングステン、モリブデン等のヒーターを
用い、これ自身を蒸発源容器として用いている。この方
法は、蒸発源の加熱方法としては最も簡便であるが、蒸
発源容器の形状の制限から、通常、50A以上の大電流
電源が必要とされる。また、大電流を真空中に導くため
の電極も大電流に耐えるために大型のものを使用しなけ
ればならないため、装置の小規模化に制限がある。 (2)電子ビーム加熱方式蒸着法 本方式では、電子銃から得られる数keVの電子ビーム
を蒸発源に直接照射する。この方法は、蒸発源の効率的
な加熱方法であるが、電子ビームを作り出すために数k
Vの電圧を真空中の電極に印加し、また、電子ビームを
蒸発源に導くために、永久磁石などの部品を真空中で用
いる必要がある。 (3)その他の蒸着方法 上記以外に、スパッタ法、イオンプレーティング法、C
VD法等が考えられるが、これらは装置の小規模化に制
約があり、装置の簡便さの点から詳細な記述は省略す
る。このように、従来、真空蒸着装置における蒸発源の
加熱方式として、上記加熱方式が開発されているが、い
ずれの方法も、装置全体を簡便なものとするには、改良
すべき問題があった。
2. Description of the Related Art Conventionally, various methods have been developed as a vacuum deposition method for forming a thin film by coating the surface of various materials. The following is a list of conventional methods for producing the thin film. (1) Electric heating type evaporation method In this method, a heater made of tungsten, molybdenum, or the like is used, and the heater itself is used as an evaporation source container. This method is the simplest method for heating the evaporation source, but usually requires a large current power supply of 50 A or more due to the limitation of the shape of the evaporation source container. In addition, a large electrode must be used to withstand a large current for conducting a large current into a vacuum, which limits the miniaturization of the apparatus. (2) Electron Beam Heating Deposition Method In this method, an evaporation source is directly irradiated with an electron beam of several keV obtained from an electron gun. This method is an efficient method of heating the evaporation source, but requires several kilograms to create an electron beam.
In order to apply a voltage of V to an electrode in a vacuum and guide an electron beam to an evaporation source, it is necessary to use a component such as a permanent magnet in a vacuum. (3) Other vapor deposition methods In addition to the above, sputtering, ion plating, C
Although the VD method and the like are conceivable, these methods are limited in terms of downsizing of the apparatus, and a detailed description is omitted from the viewpoint of simplicity of the apparatus. As described above, conventionally, as the heating method of the evaporation source in the vacuum evaporation apparatus, the above-described heating method has been developed. However, any method has a problem to be improved in order to simplify the entire apparatus. .

【0003】[0003]

【発明が解決しようとする課題】本発明者らは、国立機
関における原子力試験研究において、「速中性子による
固体中軽元素の動的挙動の測定技術に関する研究」を行
って来た。この研究においては、高エネルギーイオンビ
ームを照射することにより中性子を発生するためのリチ
ウムや重水素化チタン等のターゲット薄膜を作製する必
要があった。当初、既存の真空蒸着装置を用いてターゲ
ット作製を行っていたが、実験が進むにつれて、ターゲ
ット薄膜作製は高エネルギーイオン照射装置の周辺で行
うことが好ましいことが明らかになった。この要請に応
えるため、可搬型の簡便な真空蒸着装置を設計していた
が、この段階で(1) 通電式加熱法のような50Aを越え
るような大電流を用いることを避けること、(2) 電子線
加熱方式のような1kVを越えるような高電圧を用いる
ことや永久磁石などの使用を避けること、(3) これによ
り装置全体を簡便なものとしうる効率的な蒸発源の加熱
を実現することを、等を主要な課題として鋭意検討を進
めた結果、簡便な機構を持つ新しい蒸発源及びその加熱
方法を開発することに成功し、本発明を完成するに至っ
た。すなわち、本発明の目的は、真空蒸着装置中の蒸発
源をより効率的に加熱し、装置の簡便な設計を可能とす
る蒸発源を開発し、提供することである。
DISCLOSURE OF THE INVENTION The present inventors have conducted "research on technology for measuring dynamic behavior of light elements in solids by fast neutrons" in nuclear test research at national organizations. In this research, it was necessary to prepare a target thin film such as lithium or titanium deuteride for generating neutrons by irradiating a high energy ion beam. Initially, the target was produced using an existing vacuum deposition apparatus. However, as the experiment progressed, it became clear that the target thin film was preferably produced around the high energy ion irradiation apparatus. In order to meet this demand, a portable and simple vacuum deposition apparatus was designed.At this stage, (1) avoid using a large current exceeding 50 A as in the current-carrying heating method, (2) ) Use of high voltage exceeding 1 kV as in the electron beam heating method and avoiding the use of permanent magnets, etc. (3) This enables efficient heating of the evaporation source that can simplify the entire apparatus As a result, the present inventors have succeeded in developing a new evaporation source having a simple mechanism and a heating method thereof, and have completed the present invention. That is, an object of the present invention is to develop and provide an evaporation source that more efficiently heats an evaporation source in a vacuum evaporation apparatus and enables a simple design of the apparatus.

【0004】[0004]

【課題を解決するための手段】上記課題を解決するため
の本発明は、以下の技術的手段から構成される。 (1)真空蒸着装置中の蒸発源の加熱を効率よく行うた
めの蒸発源であって、次の手段;導電性高融点物質から
なる蒸発源容器、該容器を支持する金属製の蒸発源支持
棒、蒸発源容器下部に配置した高融点金属箔からなる加
熱用ヒーター、該ヒーターに通電するヒーター電源、蒸
発源容器とヒーターとの間に印加する電子加速電源、を
構成要素として具備してなり、上記高融点金属箔を通電
加熱し、これからの放射熱により蒸発源容器を放射加熱
するとともに、蒸発源容器とヒーターとの間に電圧を印
加し、金属箔表面から放出される電子を加速して蒸発源
容器に照射し、効率よく真空蒸発源を加熱するように構
成したことを特徴とする蒸発源。 (2)金属箔表面の一部に異種物質を被覆することによ
り、熱電子の局所的な放出効率を高めるようにしたこと
を特徴とする前記(1)記載の蒸発源。 (3)前記(1)又は(2)記載の蒸発源を用いて、蒸
発源を加熱する方法であって、高融点金属箔を通電加熱
し、これからの放射熱により蒸発源容器を放射加熱する
とともに、蒸発源容器とヒーターとの間に電圧を印加
し、金属箔表面から放出される電子を加速して蒸発源容
器に照射し、真空蒸発源を加熱することを特徴とする蒸
発源の加熱方法。
The present invention for solving the above-mentioned problems comprises the following technical means. (1) An evaporation source for efficiently heating an evaporation source in a vacuum evaporation apparatus, comprising: an evaporation source container made of a conductive high melting point material; and a metal evaporation source supporting the container. It comprises a rod, a heater for heating made of a high melting point metal foil disposed under the evaporation source container, a heater power supply for supplying electricity to the heater, and an electron accelerating power supply for application between the evaporation source container and the heater. The high-melting point metal foil is electrically heated, and the evaporation source container is radiatively heated by radiant heat therefrom, and a voltage is applied between the evaporation source container and the heater to accelerate electrons emitted from the metal foil surface. The evaporation source is configured to irradiate the evaporation source container to heat the vacuum evaporation source efficiently. (2) The evaporation source according to the above (1), wherein a part of the surface of the metal foil is coated with a different substance to enhance the local emission efficiency of thermoelectrons. (3) A method of heating the evaporation source using the evaporation source according to the above (1) or (2), wherein the high melting point metal foil is electrically heated, and the evaporation source container is radiated by the radiant heat. At the same time, a voltage is applied between the evaporation source container and the heater, the electrons emitted from the surface of the metal foil are accelerated and irradiated to the evaporation source container, and the vacuum evaporation source is heated. Method.

【0005】[0005]

【発明の実施の形態】次に、本発明について更に詳細に
説明する。本発明は、蒸着方式として、高融点物質から
なる小さな蒸発源容器を用い、蒸発源容器の下部に配置
したヒーターから熱放射と電子線衝撃の2種類の方法で
加熱する方式をとる。蒸発源は、導電性高融点物質から
なる微小な容器とし、放射加熱及び電子線衝撃加熱が行
えるような形状とする。上記導電性高融点物質として
は、グラファイト、タングステン、モリブデン、タンタ
ル、炭化ケイ素が例示される。容器の形状は、円筒状容
器あるいは角筒状容器が例示される。また、蒸発源は、
熱伝導による放熱を最小にするために、金属製の細い支
持棒等により支持する。加熱用のヒーターとして、数m
m程度の幅で、薄いの高融点金属箔を蒸発源容器下部に
配置する。この金属箔としては、タングステン、モリブ
デン、グラファイト、タンタルが例示される。また、金
属箔の厚さは50μm以下、2〜10mm幅、長さ20
〜50mmが好ましい。このヒーターを通電加熱するこ
とにより蒸発源容器を放射加熱する。蒸発源容器とヒー
ターとの間に数100Vの高電圧を印加し、ヒータから
放出される熱電子を加速して蒸発源容器を加熱する。こ
の場合、高電圧として、300〜800V、電流容量と
して1〜5Aの電源を用いる。ヒーター表面の熱電子放
出部に、好適には、異種物質を被覆し、熱電子放出の効
率を向上させることが望ましい。異種物質としては、高
融点で仕事関数の低い、トリウム入りタングステン、6
ホウ化ランタン、酸化カルシウム、酸化バリウム、モリ
ブデン、ジルコニウムが例示される。この異種物質の被
覆方法はスパッタ法が好ましく、その条件は、膜厚が1
〜100nmで、面積は蒸発源容器底面と同程度であ
る。
Next, the present invention will be described in more detail. The present invention employs, as a vapor deposition method, a method in which a small evaporation source container made of a high melting point material is used, and heating is performed by a heater disposed at a lower portion of the evaporation source container by two types of heat radiation and electron beam impact. The evaporation source is a small container made of a conductive high-melting substance, and has a shape capable of performing radiant heating and electron beam impact heating. Examples of the conductive high melting point material include graphite, tungsten, molybdenum, tantalum, and silicon carbide. The shape of the container is exemplified by a cylindrical container or a rectangular cylindrical container. The evaporation source is
In order to minimize heat radiation due to heat conduction, it is supported by a thin metal support rod or the like. Several meters as heater for heating
A thin, high melting point metal foil having a width of about m is arranged below the evaporation source container. Examples of the metal foil include tungsten, molybdenum, graphite, and tantalum. The thickness of the metal foil is 50 μm or less, a width of 2 to 10 mm, and a length of 20 μm.
~ 50 mm is preferred. The evaporation source container is radiatively heated by electrically heating the heater. A high voltage of several hundred volts is applied between the evaporation source container and the heater to accelerate the thermoelectrons emitted from the heater to heat the evaporation source container. In this case, a power supply having a high voltage of 300 to 800 V and a current capacity of 1 to 5 A is used. It is desirable that the thermoelectron emission portion on the heater surface be coated with a different substance to improve the efficiency of thermoelectron emission. Dissimilar substances include tungsten with thorium, which has a high melting point and a low work function.
Examples include lanthanum boride, calcium oxide, barium oxide, molybdenum, and zirconium. As a method for coating this different substance, a sputtering method is preferable.
At 〜100 nm, the area is comparable to the bottom of the evaporation source container.

【0006】本発明は、上記のように、(1) タングステ
ンなどの高融点金属箔を発熱源及び電子線源として用い
ること、(2) 熱容量の小さな高融点蒸発源容器を用いる
こと、(3) ヒーターの電子放出部に異種物質を被覆する
ことにより電子発生効率を向上させること、を特徴とし
ている。以上のように、本発明により、簡便な機構を持
つ蒸発源及びその加熱方法が提供される。本発明では、
真空中で薄い高融点金属箔を通電加熱することによる放
射加熱効果及び放出する熱電子を電場で加速し衝撃する
ことにより得られる電子線加熱効果の両者を有効に作用
させることにより、より効率的な真空蒸発源の加熱を実
現することができる。また、金属箔表面の一部に異種物
質を被覆することにより、熱電子発生効率を向上させる
ことができる。
According to the present invention, as described above, (1) using a high melting point metal foil such as tungsten as a heat source and an electron beam source, (2) using a high melting point evaporation source container having a small heat capacity, (3) The electron emission portion of the heater is coated with a different kind of substance to improve the electron generation efficiency. As described above, the present invention provides an evaporation source having a simple mechanism and a heating method thereof. In the present invention,
Efficient use of both the radiant heating effect of energizing and heating the thin refractory metal foil in vacuum and the electron beam heating effect obtained by accelerating and impacting the emitted thermoelectrons with an electric field The heating of the vacuum evaporation source can be realized. In addition, by covering a part of the surface of the metal foil with a different kind of substance, the efficiency of generating thermoelectrons can be improved.

【0007】[0007]

【実施例】実施例に基づいて本発明をさらに具体的に説
明するが、本発明は以下の実施例により何ら限定される
ものではない。 実施例 図1に本発明の蒸発源の構造、すなわち、加熱用ヒータ
と蒸発源容器の配置及び電気的な結線図を示した。高融
点金属ヒータは、50mm×5mm×0.05mmの矩
形のタングステン箔を用いた。蒸発源容器は、外径25
mm、高さ15mm、肉厚約1mmの円筒状のグラファ
イト容器である。このヒータに最高40Aまでの電流を
通じ、10mm上方に置かれた蒸発源容器との間に最高
500Vの電圧を印加した。ヒーターの中心約25平方
ミリの領域にモリブデンを約1nmの厚さでイオンビー
ムスパッタ法により被覆した。これにより被覆部分の電
子放出効率が、2〜5倍程度に向上した。上記の方法に
より、ヒーター電力約1500W(50V、30A)、
電子線加熱電力300W(600V,0. 5A)でグラ
ファイト蒸発源容器を最高1500℃まで加熱すること
が出来た。
EXAMPLES The present invention will be described more specifically based on examples, but the present invention is not limited to the following examples. Embodiment FIG. 1 shows the structure of the evaporation source of the present invention, that is, the arrangement of the heater for evaporation and the evaporation source container and the electrical connection diagram. As the high melting point metal heater, a rectangular tungsten foil of 50 mm × 5 mm × 0.05 mm was used. The evaporation source container has an outer diameter of 25.
mm, a height of 15 mm, and a wall thickness of about 1 mm. A current of up to 40 A was passed through the heater, and a voltage of up to 500 V was applied between the heater and the evaporation source container placed 10 mm above. Molybdenum was coated to a thickness of about 1 nm by an ion beam sputtering method in an area of about 25 mm 2 at the center of the heater. Thereby, the electron emission efficiency of the coated portion was improved to about 2 to 5 times. According to the above method, the heater power is about 1500 W (50 V, 30 A),
The graphite evaporation source container could be heated up to 1500 ° C. with an electron beam heating power of 300 W (600 V, 0.5 A).

【0008】上記結果は、本発明の一例であり、本発明
は、さらに下記の特徴を有する。 (1) ヒータ箔の厚さを0.05mm以下にすることによ
り、ヒーター電流を下げることが出来る。 (2) 蒸発源容器の熱容量を小さくすることが出来る。 (3) 加速電圧を数100V高めることにより、電子線加
熱電力を数10%高めることが出来る (4) ヒーター表面の被覆物質にモリブデン以外の物質、
トリウム入りタングステン、ホウ化ランタン、酸化カル
シウム、酸化バリウム、ジルコニウムを用い、これによ
りより効率的な熱電子放出表面を形成することが出来
る。 以上の点から、本発明により、1500℃以上に加熱で
きる蒸発源が実現できる、簡便な真空蒸着装置の設計が
可能となる。
The above result is an example of the present invention, and the present invention further has the following features. (1) The heater current can be reduced by setting the thickness of the heater foil to 0.05 mm or less. (2) The heat capacity of the evaporation source container can be reduced. (3) By increasing the acceleration voltage by several hundred volts, electron beam heating power can be increased by several tens of percent. (4) Materials other than molybdenum may be
Tungsten-containing tungsten, lanthanum boride, calcium oxide, barium oxide, and zirconium are used, whereby a more efficient thermionic emission surface can be formed. In view of the above, the present invention makes it possible to design a simple vacuum evaporation apparatus that can realize an evaporation source that can be heated to 1500 ° C. or higher.

【0009】[0009]

【発明の効果】本発明により、1)ヒーター加熱電流を
50A以下にし、電子線加速電源電圧を1KV以下(数
A)にできる、2)高温加熱が必要な蒸発源及び関連部
品の簡素化、簡略化が図れる、3)装置の小型化、コス
トの低減化が図れる、等の効果が得られる。
According to the present invention, 1) the heater heating current can be reduced to 50 A or less, and the electron beam acceleration power supply voltage can be reduced to 1 KV or less (several A). 2) The simplification of the evaporation source and related parts that require high-temperature heating, It is possible to obtain effects such as simplification, 3) downsizing of the device and reduction of cost.

【図面の簡単な説明】[Brief description of the drawings]

【図1】電子線源ヒーター及び蒸着用坩堝の配置及び断
面図と電源用結線図を示す。
FIG. 1 shows an arrangement and a cross-sectional view of an electron beam source heater and a deposition crucible, and a power supply connection diagram.

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 真空蒸着装置中の蒸発源の加熱を効率よ
く行うための蒸発源であって、次の手段;導電性高融点
物質からなる蒸発源容器、該容器を支持する金属製の蒸
発源支持棒、蒸発源容器下部に配置した高融点金属箔か
らなる加熱用ヒーター、該ヒーターに通電するヒーター
電源、蒸発源容器とヒーターとの間に印加する電子加速
電源、を構成要素として具備してなり、上記高融点金属
箔を通電加熱し、これからの放射熱により蒸発源容器を
放射加熱するとともに、蒸発源容器とヒーターとの間に
電圧を印加し、金属箔表面から放出される電子を加速し
て蒸発源容器に照射し、効率よく真空蒸発源を加熱する
ように構成したことを特徴とする蒸発源。
1. An evaporation source for efficiently heating an evaporation source in a vacuum evaporation apparatus, comprising: an evaporation source container made of a conductive high-melting substance; and a metal evaporation supporting the container. A source support rod, a heater for heating made of a high melting point metal foil disposed under the evaporation source container, a heater power supply for supplying electricity to the heater, and an electron acceleration power supply for applying between the evaporation source container and the heater are provided as constituent elements. The above-mentioned high melting point metal foil is electrically heated, and the evaporation source container is radiatively heated by radiant heat from this, and a voltage is applied between the evaporation source container and the heater to generate electrons emitted from the metal foil surface. An evaporation source characterized in that it is configured to accelerate and irradiate an evaporation source container to efficiently heat a vacuum evaporation source.
【請求項2】 金属箔表面の一部に異種物質を被覆する
ことにより、熱電子の局所的な放出効率を高めるように
したことを特徴とする請求項1記載の蒸発源。
2. The evaporation source according to claim 1, wherein a part of the surface of the metal foil is coated with a different kind of material to enhance the local emission efficiency of thermoelectrons.
【請求項3】 請求項1又は2記載の蒸発源を用いて、
蒸発源を加熱する方法であって、高融点金属箔を通電加
熱し、これからの放射熱により蒸発源容器を放射加熱す
るとともに、蒸発源容器とヒーターとの間に電圧を印加
し、金属箔表面から放出される電子を加速して蒸発源容
器に照射し、真空蒸発源を加熱することを特徴とする蒸
発源の加熱方法。
3. Use of the evaporation source according to claim 1 or 2,
A method of heating an evaporation source, in which a high-melting-point metal foil is electrically heated, a radiation heat is applied to the evaporation source container by radiant heat, and a voltage is applied between the evaporation source container and the heater, and the surface of the metal foil is heated. A method for heating an evaporation source, comprising: irradiating the evaporation source container with accelerated electrons emitted from a vacuum evaporation source and heating the vacuum evaporation source.
JP2000073500A 2000-03-16 2000-03-16 Evaporation source in vacuum evaporation apparatus and heating method thereof Expired - Lifetime JP3438024B2 (en)

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