WO2012118129A1

WO2012118129A1 - Vacuum processing device and vacuum processing method

Info

Publication number: WO2012118129A1
Application number: PCT/JP2012/055123
Authority: WO
Inventors: 佐竹　徹
Original assignee: 株式会社アルバック
Priority date: 2011-03-01
Filing date: 2012-02-29
Publication date: 2012-09-07
Also published as: CN103392027A; JPWO2012118129A1

Abstract

[Problem] To provide a vacuum processing device and a vacuum processing method which are capable of knowing the concentration of impurities contained in an object to be irradiated while heating the object to be irradiated by irradiating the object to be irradiated with an electron beam to thereby vaporize a specific constituent contained in the object to be irradiated. [Solution] A vacuum processing device comprising a vacuum chamber (11), and an electron gun (20) which heats an object to be irradiated that is disposed in the vacuum chamber (11) by irradiating the object to be irradiated with an electron beam to thereby vaporize a specific constituent contained in the object to be irradiated, said vacuum processing device comprising an X-ray measurement unit (62) which measures the relationship between the energy and the intensity of X-rays within a predetermined energy range, and an attenuation filter (61) on which X-rays emitted from the object to be irradiated (50) by the irradiation with the electron beam are incident, and which causes the incident X-rays to be attenuated, pass therethrough, and be incident on the X-ray measurement unit (62).

Description

Vacuum processing apparatus and vacuum processing method

The present invention relates to a vacuum processing apparatus and a vacuum processing method, and more particularly, to a technique for irradiating an irradiation object with an electron beam and heating it to vaporize a specific component contained in the irradiation object.

Currently, vacuum processing apparatuses that can irradiate and heat a relatively high energy electron beam on an irradiation object such as metal and vaporize (evaporate or sublimate) specific components contained in the irradiation object are mainly vacuum. It is used for vapor deposition and vacuum dissolution purification.

A conventional vacuum processing apparatus has a relatively large vacuum chamber having a volume of 1 m ³ or more, a vacuum exhaust device that evacuates the vacuum chamber, and an electron gun that emits an electron beam into the vacuum chamber.
The target metals in vacuum melting and refining are active metals such as titanium, vacuum materials such as stainless steel, and high melting point metals such as molybdenum and tantalum. Recently, vacuum melting and refining of silicon for solar cells has also been performed. The target metals for vacuum deposition are aluminum, titanium, copper and the like.

In the evacuated vacuum chamber, these irradiation objects are irradiated with an electron beam from an electron gun and heated, and in the step of vaporizing a specific component from the irradiation object, knowing the purity of the dissolved irradiation object, That is, it is important to know the concentration of impurities contained in the irradiation object.

In the case of conventional vacuum dissolution purification, refer to Patent Document 1 and cut out a small piece from an irradiation object that has been cooled and solidified after stopping irradiation of an electron beam, and EPMA (electron probe X-ray microanalyzer), AES The impurity concentration was measured using a surface analyzer such as an Auger electron spectrometer, an XRFS (fluorescent X-ray spectrometer), or an ICP-MASS (inductively coupled plasma mass spectrometer).

However, it takes time to measure the impurity concentration after stopping the irradiation of the electron beam, and if the purity of the irradiation object does not satisfy the specification, it is necessary to repeat the irradiation of the electron beam again. Further, setting the electron beam irradiation time has required a lot of time, for example, it is necessary to determine by performing sampling many times in advance.

In addition, in the case of conventional vacuum deposition, a film-forming material whose purity is known from the beginning has been used for the object to be irradiated. Concentration of impurity concentration occurs due to evaporation of the main component during irradiation of the line, or adhesion film deposited on the wall surface of the vacuum chamber peels off and mixes into the evaporation source. As a result, there is a problem that the performance of the film deteriorates. For example, optical materials sometimes have abnormalities in transmission characteristics, reflection characteristics, and spectral characteristics. In the case of clothing materials, the film adhesion may decrease, the hardness may deteriorate, and the decorativeness may deteriorate.

JP-A-11-209195

The present invention was created to solve the above-mentioned disadvantages of the prior art, and its purpose is to irradiate and heat an irradiation object with an electron beam while vaporizing a specific component contained in the irradiation object. An object of the present invention is to provide a vacuum processing apparatus and a vacuum processing method capable of knowing the concentration of impurities contained in an irradiation object.

In order to solve the above-described problems, the present invention provides a vacuum chamber and an electron gun that irradiates and heats an irradiation object disposed in the vacuum chamber by evaporating a specific component contained in the irradiation object. And an X-ray measuring apparatus for measuring a relationship between the energy and intensity of X-rays within a predetermined energy range, and X emitted from the irradiation object by the electron beam irradiation. It is a vacuum processing apparatus having an attenuation filter that makes a line incident, attenuates the incident X-ray, passes it, and enters the X-ray measuring apparatus.
The present invention is a vacuum processing apparatus having a calculator for determining the concentration of impurities contained in the irradiation object based on the measurement result of the X-ray measurement apparatus.
This invention is a vacuum processing apparatus, Comprising: The vacuum in which the adhesion prevention filter which attenuate | damps the vapor | steam discharged | emitted from the said irradiation target object and reaching | attains the said attenuation filter is arrange | positioned between the said irradiation target object and the said attenuation filter. It is a processing device.
This invention is a vacuum processing apparatus, The said specific component is an impurity of the said irradiation target object, The vacuum processing apparatus which reduces the density | concentration of the said impurity contained in the said irradiation target object by irradiation of the said electron beam.
The present invention is the vacuum processing apparatus, wherein the specific component is a main component of the irradiation object, a film formation object is disposed between the irradiation object and the attenuation filter, and the electron beam irradiation The vacuum processing apparatus forms a thin film by releasing the vapor of the main component from the irradiation object and causing the vapor to reach the film formation object disposed in the vacuum chamber.
The present invention is a vacuum processing apparatus, comprising: a winding shaft disposed in the vacuum chamber; and a winding shaft rotating device that rotates the winding shaft around a central axis of the winding shaft; The film formation target is a band-shaped film, and one end in the longitudinal direction of the film formation target is wound and fixed around the winding shaft, and the winding shaft is rotated by the winding shaft rotating device. The film formation object is a vacuum processing apparatus wound on the winding shaft.
The present invention is a vacuum processing method in which an irradiation target disposed in the vacuum chamber is heated by irradiating an electron beam while evacuating the vacuum chamber to vaporize a specific component contained in the irradiation target. Then, X-rays emitted from the irradiation object by the irradiation of the electron beam enter, using an attenuation filter that attenuates and passes the incident X-ray, while irradiating the irradiation object with the electron beam, In this vacuum processing method, the relationship between the intensity and intensity of X-rays within a predetermined energy range among the X-rays that have passed through the attenuation filter is measured.
The present invention is a vacuum processing method, wherein a vacuum is used to determine the concentration of impurities contained in the irradiation object based on the relationship between the measured X-ray energy and intensity while irradiating the irradiation object with an electron beam. It is a processing method.
The present invention is a vacuum processing method using a deposition filter that attenuates vapor that is emitted from the irradiation object and reaches the attenuation filter.
This invention is a vacuum processing method, Comprising: The said specific component is the impurity of the said irradiation target object, The vacuum which irradiates the electron beam to the said irradiation target object, and reduces the density | concentration of the said impurity contained in the said irradiation target object It is a processing method.
The present invention is a vacuum processing method, wherein the specific component is a main component of the irradiation object, and the irradiation object is irradiated with an electron beam to release the vapor of the main component from the film formation object. A vacuum processing method for forming a thin film by causing the vapor to reach a film formation object disposed between the irradiation object and the attenuation filter.
The present invention is a vacuum processing method, wherein the film formation target is a band-shaped film, and the vapor is incident on the movement direction of the film formation target while irradiating the irradiation target with an electron beam. This is a vacuum processing method in which the film formation target is wound on the end point side from the position where the film is formed.

In the present invention, an element contained in the irradiation object in an amount of more than 50 mol% is referred to as “main component”, and an element other than the main component among the elements contained in the irradiation object is referred to as “impurity”.
The principle of elemental analysis by X-ray will be described.
When a material is irradiated with an electron beam, braking X-rays (also called white X-rays) having a continuous range of energy having a value almost the same as the energy of the electron beam, and characteristic X-rays peculiar to the elements of the material Occurs.
Characteristic X-rays are orders of magnitude stronger than white X-rays and mainly have two types of energy. Those characteristic X-rays are called Kα-rays and Kβ-rays from the lowest energy.

Kα-rays and Kβ-rays are X-rays generated to excite and knock out K-shell electrons in the electron orbit of the element. In a heavy element, the energy required to excite K-shell electrons increases, and when the energy of the electron beam irradiated becomes lower than that energy, the electron beams cannot knock out K-shell electrons. In this case, the electron beam excites and knocks out electrons in the L shell, which is an electron orbit outside the K shell, and the characteristic X-rays generated at this time are called Lα rays and Lβ rays. Tables 1 and 2 show the characteristic X-ray energy values of each element. Tables 1 and 2 are listed in the Ministry of the Environment, “Provisional Manual for Measuring Method of Atmospheric Fine Particulate Matter (PM2.5), Revised Edition”, July 2007, Chapter 5, “4”, p. Quoted from 6-7.

Since Kα and Kβ rays have higher energy as the atomic number is larger, knowing the energy (or wavelength) of Kα and Kβ rays makes it possible to identify the element of the substance with high sensitivity.

While irradiating an object with an electron beam and heating it, it is possible to know the concentration of impurities contained in the object to be irradiated. There is no need to open the tank to the atmosphere, and production time can be greatly reduced.

When the present invention is used for vacuum melting and purification, the impurity concentration in the dissolved material can be confirmed while irradiating the electron beam, so the timing for stopping the irradiation of the electron beam can be accurately determined, and a product with stable quality can be produced. it can.
Further, when the present invention is used for vacuum deposition, the concentration of impurities in a film forming material can be confirmed while irradiating an electron beam, so that the film quality of a film to be formed can be kept constant and the yield of products can be improved.

Internal configuration diagram of the vacuum processing apparatus of the first example Internal structure of electron gun Internal configuration diagram of X-ray measurement unit Top view of anti-adhesion filter Internal configuration diagram of the vacuum processing apparatus of the second example Internal configuration diagram of the vacuum processing apparatus of the third example Internal configuration diagram of the vacuum processing apparatus of the fourth example

<Structure of vacuum processing apparatus of first example>
The structure of the vacuum processing apparatus of the first example of the present invention will be described. FIG. 1 is an internal configuration diagram of the vacuum processing apparatus 10a of the first example.
The vacuum processing apparatus 10 a of the first example includes a vacuum chamber 11, a vacuum exhaust device 12 that evacuates the vacuum chamber 11, and an electron gun 20 that emits an electron beam into the vacuum chamber 11.

Here, the material of the vacuum chamber 11 is stainless steel. The vacuum exhaust device 12 is connected to an exhaust port provided in the vacuum chamber 11, and is configured so that the vacuum chamber 11 can be evacuated.
An electron gun power source 40 is electrically connected to the electron gun 20.

FIG. 2 is an internal configuration diagram of the electron gun 20 and the electron gun power source 40.
The electron gun 20 has a bottomed cylindrical casing 21 provided with a muzzle 22 at one end.
Inside the casing 21, a gun chamber 23, a connection path 24, an intermediate chamber 25, and a discharge path 26 are lined up in this order from the bottom of the casing 21 toward the muzzle 22 on the central axis of the casing 21. Is provided. The gun chamber 23 and the intermediate chamber 25 are connected by a connection path 24, and the intermediate chamber 25 and the muzzle 22 are connected by a discharge path 26.

The gun chamber 23 and the intermediate chamber 25 are connected to electron gun

vacuum exhaust devices

27 ₁ and 27 ₂ , respectively, and the

chambers

23 and 25 can be evacuated. A partition valve 39 is provided in the connection path 24.

Hereinafter, the gun chamber 23 side of the casing 21 is referred to as upstream, and the opposite muzzle 22 side is referred to as downstream.
In the gun chamber 23, the filament 31, the cathode electrode 32, the Wehnelt electrode 33, and the anode electrode 34 are arranged in a line in this order from the upstream side to the downstream side on the central axis of the casing 21. .

Both the Wehnelt electrode 33 and the anode electrode 34 have a bottomless cylindrical shape, and the respective central axes are oriented in a direction that coincides with the central axis of the casing 21.
The Wehnelt electrode 33 is electrically connected to the cathode electrode 32, and the anode electrode 34 is electrically connected to the housing 21. The casing 21 is placed at the ground potential.

A first lens coil 36, a second lens coil 37, and a swing coil 38 are arranged in a line in this order along the central axis of the casing 21 on the downstream side of the anode electrode 34.
Here, the first lens coil 36 is disposed so as to surround the outer periphery of the connection path 24, the second lens coil 37 is disposed so as to surround the outer periphery of the discharge path 26, and the swing coil 38 is disposed around the outer periphery of the muzzle 22. It is arranged so as to surround it.

The electron gun power supply 40 includes a filament power supply 41, a cathode heating power supply 42, an extraction power supply 43, a lens power supply 44, and an oscillating coil power supply 45.
The filament power supply 41 is electrically connected to the filament 31 and can be heated by passing an electric current through the filament 31.

The cathode heating power source 42 is electrically connected to the cathode electrode 32 and the filament 31 via the Wehnelt electrode 33, so that the potential of the cathode electrode 32 is positive with respect to the filament 31. It is comprised so that a DC voltage can be applied to.

The extraction power supply 43 is electrically connected to the cathode electrode 32 and the casing 21 via the Wehnelt electrode 33 so that the potential of the cathode electrode 32 is negative with respect to the potential of the casing 21, that is, the potential of the anode electrode 34. In addition, a DC voltage can be applied between the casing 21 and the cathode electrode 32.

The lens power supply 44 is electrically connected to the first and second lens coils 36 and 37, respectively, and a current is passed through the first and second lens coils 36 and 37, so that the inside of the connection path 24 and the discharge path 26. A magnetic field can be formed respectively.

The oscillating coil power supply 45 is electrically connected to the oscillating coil 38, and allows a current to flow through the oscillating coil 38 to form a magnetic field inside the muzzle 22.
A magnetic field control device 46 is connected to the oscillating coil power supply 45. The magnetic field controller 46 is configured to determine the direction and amount of current supplied from the oscillating coil power supply 45 to the oscillating coil 38 and to control the direction and magnitude of the magnetic field formed inside the muzzle 22. Has been.

With reference to FIG. 1, the casing 21 of the electron gun 20 is inserted in an airtight manner in the vacuum chamber 11, and the muzzle 22 is exposed in the vacuum chamber 11.
The vacuum processing apparatus 10a of the first example includes a material container 13 that is disposed in the vacuum chamber 11 and holds the irradiation target object 50, and a material carry-in device 14 that loads the irradiation target object 50 into the vacuum tank 11. ing.

The material carry-in device 14 is provided airtightly through the tank wall of the vacuum tank 11, and carries the irradiation object 50 from the outside to the inside of the vacuum tank 11 while maintaining the vacuum atmosphere in the vacuum tank 11. It is comprised so that it can arrange | position in 13th.

As will be described later, when the irradiation object 50 in the material container 13 is irradiated with an electron beam from the electron gun 20 and heated, a specific component contained in the irradiation object 50 is vaporized. Further, X-rays are emitted from the irradiation object 50.

The vacuum processing apparatus 10a of the first example includes an X-ray measurement unit 60 that measures X-rays emitted from the irradiation object 50.
FIG. 3 is an internal configuration diagram of the X-ray measurement unit 60.

The X-ray measurement unit 60 receives an X-ray measurement device 62 that measures the relationship between the energy and intensity of X-rays within a predetermined energy range, and X-rays emitted from the irradiation object 50 by electron beam irradiation. And an attenuation filter 61 that attenuates the incident X-rays to pass through and makes them enter the X-ray measuring device 62.

The X-ray measurement apparatus 62 includes an X-ray detection unit 63 that generates an electrical signal according to the energy (or wavelength) of X-rays within a predetermined energy range, and an X-ray that supplies power to the X-ray detection unit 63. The power supply 64 for a detection part and the memory | storage device 68 which receives and memorize | stores the electric signal which the X-ray detection part 63 produced | generated are provided.

The X-ray detection unit 63 is airtightly fixed to a detection unit container 63a formed of a material that blocks X-rays, a spectroscopic unit 63b disposed inside the detection unit container 63a, and an opening of the detection unit container 63a. Window member 63c.

The window member 63c is a member that transmits X-rays as much as possible. Here, a metal foil (for example, Be foil) with a film thickness of 10 μm to 50 μm and a low Z (low atomic number) as much as possible is used. In order to give the window member 63c strength as a vacuum wall, a metal mesh may be fixed as a reinforcing material.

The window member 63c is hermetically adhered to the detection unit container 63a so as to close the opening of the detection unit container 63a.
The detection unit container 63a is made of a material that blocks X-rays, and only the X-rays that have passed through the window member 63c reach the spectroscopic unit 63b.

Further, the window member 63c is configured to be able to keep the inside of the detection unit container 63a airtight together with the detection unit container 63a, and when the X-ray detection unit 63 is disposed in the evacuated vacuum chamber 11, The spectroscopic unit 63 b is isolated from the vacuum atmosphere in the vacuum chamber 11.

As the spectroscopic unit 63b, a commercially available spectroscopic device for X-ray elemental analysis can be used. In this embodiment, a lithium drift type semiconductor detector is used, but wavelength dispersion type X-ray detection using a diffraction grating is used. A vessel may be used.

A lithium drift type semiconductor detector is a semiconductor having a pin junction in which Li is diffused into a Si crystal to form an intrinsic region (i layer). When X rays within a predetermined energy range enter the i layer, A number of electron-hole pairs proportional to energy are generated.

The power source 64 for the X-ray detection unit is electrically connected to the spectroscopic unit 63b. When a positive voltage is applied to the n layer with respect to the p layer, the electron-hole pair generated in the i layer is moved by the electric field, and the spectroscopic unit An electric signal having a magnitude proportional to the energy of the X-ray is extracted from the unit 63b.

The storage device 68 is connected to the spectroscopic unit 63b, receives the electric signal extracted from the spectroscopic unit 63b, and stores the number of electric signals for each magnitude of the received electric signal, that is, for each X-ray energy. Has been. Accordingly, the relationship between the energy and intensity of X-rays within a predetermined energy range incident on the X-ray detection unit 63 can be understood from the stored contents of the storage device 68.

The vacuum processing apparatus 10a of the first example has a calculator 69 that calculates the concentration of impurities contained in the irradiation object 50 based on the measurement result of the X-ray measurement apparatus 62. The computer 69 is connected to the storage device 68.
Here, the computer 69 reads out the storage content of the storage device 68, subtracts the background such as white X-rays from the storage content, extracts the relationship between the energy and intensity of the characteristic X-ray, and then extracts the extracted characteristic X-ray. Associate energy with the corresponding element. If the main component element of the irradiation object 50 is preset in the calculator 69, the calculator 69 obtains the sum of the intensity of characteristic X-rays corresponding to the elements other than the main component (referred to as impurity intensity), and the characteristic X The ratio of the intensity of the impurity to the intensity of the entire line is calculated, and the concentration of the impurity contained in the irradiation object 50 is obtained.

The attenuation filter 61 is a metal thin film, and here, a Ti foil with a thickness of 20 μm or an Al foil with a thickness of 1 mm is used. When the thickness of the attenuation filter 61 is so thin that it cannot maintain the shape against an external force such as gravity, a stainless steel mesh may be fixed to the attenuation filter 61 as a reinforcing material.

When X-rays enter the attenuation filter 61, a part of the incident X-rays is absorbed or reflected inside the attenuation filter 61, that is, the incident X-rays are attenuated.
The attenuation filter 61 is not limited to the above configuration as long as incident X-rays can be attenuated, and may be a metal plate provided with pinholes penetrating in the thickness direction. When X-rays enter the attenuating filter 61, some of the incident X-rays pass through the inside of the pinhole, and other X-rays collide with the plate outside the pinhole and are blocked. Attenuated. By changing the diameter of the pinhole, the attenuation factor of X-rays can be changed, and the attenuation factor of X-rays can be easily changed as compared with a metal thin film.

The attenuation filter 61 is disposed to face the window member 63 c of the X-ray detection unit 63. Therefore, the X-rays that have passed through the attenuation filter 61 are incident on the X-ray detection unit 63.
In the present embodiment, referring to FIG. 1, the X-ray detection unit 63 is disposed at a position facing the irradiation object 50 in a state where the window member 63 c is directed in the direction in which the irradiation object 50 is positioned in the material container 13. The attenuation filter 61 is disposed between the X-ray detection unit 63 and the irradiation object 50.

As will be described later, the intensity of the X-rays emitted from the irradiation object 50 is two or more orders of magnitude greater than the intensity of the X-rays emitted from the irradiation object in the case of X-ray analysis. When the light directly enters the X-ray detection unit 63 without being attenuated, a pile-up phenomenon occurs in which two electric signals generated in succession overlap each other, and the relationship between the X-ray energy and intensity can be measured accurately. Can not. On the other hand, in the present invention, since the X-ray attenuated by the attenuation filter 61 is incident on the X-ray detection unit 63, the pile-up phenomenon does not occur and the relationship between the X-ray energy and intensity is accurately measured. It has become.

The X-ray measurement unit 60 includes an adhesion filter 65 that attenuates the vapor emitted from the irradiation object 50 and reaching the attenuation filter 61.
FIG. 4 is a plan view of the anti-adhesion filter 65.

Here, the anti-adhesion filter 65 is made of a material that shields vapor particles, is formed in a disk shape whose radius is larger than the diameter of the attenuation filter, and a band-like opening 66 through which the vapor can pass radiates from the center of the anti-adhesion filter 65. It is provided to extend in the direction.
With reference to FIG. 1, the anti-adhesion filter 65 is disposed between the attenuation filter 61 and the irradiation object 50 in the material container 13 with the opening 66 facing the attenuation filter 61.

Referring to FIG. 3, a rotation shaft 67a is fixed at the center of the deposition filter 65 at a right angle to the surface of the deposition filter 65, and a rotation shaft rotating device 67b is connected to the rotation shaft 67a. The rotating shaft rotating device 67b is a motor, and transmits power to the rotating shaft 67a so that the anti-adhesion filter 65 can be rotated around the central axis of the rotating shaft 67a together with the rotating shaft 67a.

When the deposition filter 65 is rotated about the central axis of the rotation shaft 67a by the rotation shaft rotating device 67b, the X-ray and the vapor incident on the deposition filter 65 are blocked by the shielding portion other than the opening 66 of the deposition filter 65. When facing the attenuation filter 61, it is shielded by the shielding portion and does not reach the attenuation filter 61. When the opening 66 faces the attenuation filter 61, it passes through the opening 66 and reaches the attenuation filter 61. Yes. Therefore, the anti-adhesion filter 65 can attenuate the vapor reaching the attenuation filter 61 while allowing the X-rays to reach the attenuation filter 61.

<Vacuum processing method using the vacuum processing apparatus of the first example>
A vacuum processing method using the vacuum processing apparatus 10a of the first example will be described by taking vacuum dissolution purification of a dissolved material mainly composed of silicon as an example.

(Preparation process)
The irradiation object 50 is a melting material mainly composed of silicon. A threshold value of the impurity concentration in the dissolved material used when stopping the electron beam irradiation is determined in advance. Further, it is set in the computer 69 that the main element is silicon.
Further, the range of X-ray energy (or wavelength) measured by the X-ray measuring device 62 is set in advance to a range equal to or lower than the energy of the electron beam.

Referring to FIG. 1, the vacuum chamber 11 is evacuated by a vacuum evacuation device 12 to form a vacuum atmosphere. Thereafter, evacuation is continued and the vacuum atmosphere in the vacuum chamber 11 is maintained.
While maintaining the vacuum atmosphere in the vacuum chamber 11, the irradiation object 50 is carried into the vacuum chamber 11 by the material carry-in device 14 and placed in the material container 13.

The anti-adhesion filter 65 is rotated around the central axis of the rotary shaft 67a by the rotary shaft rotating device 67b. Power is supplied from the X-ray detection unit power supply 64 to the spectroscopic unit 63b of the X-ray detection unit 63 in advance.

(Vacuum dissolution purification process)
The vacuum chamber 11 and the material container 13 are placed at the ground potential.
Referring to FIG. 2, when the inside of the vacuum chamber 11 is evacuated, the inside of the housing 21 of the electron gun 20 is also evacuated.
When the pressure in the vacuum chamber 11 is lowered to the 10 ⁻² Pa level, evacuation in the gun chamber 23 and the intermediate chamber 25 is started by the electron gun

vacuum exhaust devices

27 ₁ and 27 ₂ .

Next, the gate valve 39 is opened. The intermediate chamber 25 is provided and has an operating exhaust structure. Thereafter, even if the pressure in the vacuum chamber 11 rises to about 1 × 10 ⁻¹ Pa by electron beam irradiation or the like, the pressure in the gun chamber 23 is reduced to 5 ×. It can be kept at ^10-3 Pa or less. Thereby, abnormal discharge in the gun chamber 23 can be prevented, and burning of the filament 31 and the cathode electrode 32 can be prevented.

The casing 21 and the anode electrode 34 are placed at the ground potential.
A DC voltage is applied between the filament 31 and the cathode electrode 32 so that the cathode electrode 32 has a positive potential with respect to the filament 31. Further, a DC voltage is applied between the cathode electrode 32 and the anode electrode 34 so that the cathode electrode 32 becomes a negative potential (−40 kV in this case) with respect to the anode electrode 34. Further, a current is passed through the first and second lens coils 36 and 37 to form magnetic fields inside the connection path 24 and the discharge path 26, respectively, and a current is passed through the rocking coil 38 and the inside of the muzzle 22. A magnetic field is formed in

When the pressure in the intermediate chamber 25 reaches the 10 ⁻³ Pa level and the pressure in the gun chamber 23 reaches the 10 ⁻⁴ Pa level, a current is supplied from the filament power source 41 to heat the filament 31. When the filament 31 reaches a high temperature (here, 2800 K), thermoelectrons are emitted from the filament 31.

The emitted thermoelectrons are accelerated toward the cathode electrode 32 and collide with the cathode electrode 32 to heat the cathode electrode 32.
When the cathode electrode 32 is heated, thermoelectrons are emitted from the cathode electrode 32. The higher the temperature of the cathode electrode 32, the greater the amount of thermoelectrons generated. The temperature of the cathode electrode 32 is controlled by the cathode heating power source 42, and thus the amount of thermoelectrons generated is controlled by the cathode heating power source 42.
The Wehnelt electrode 33 has the same potential as the cathode electrode 32, and serves to suppress the divergence of electrons from the cathode electrode 32 and lead it to the anode electrode 34.

The electrons that have passed through the anode electrode 34 are converged by the magnetic field formed by the first lens coil 36, pass through the opening of the partition valve 39, pass through the intermediate chamber 25, and then formed by the second lens coil 37. Then, the light is converged again by the magnetic field, and then the trajectory is corrected by the magnetic field formed by the oscillating coil 38 and is released from the muzzle 22 into the vacuum chamber 11.

Thus, the electrons generated from the cathode electrode 32 are linearly shaped and transported inside the casing 21 of the electron gun 20 and are therefore usually called electron beams.
As described above, the casing 21, the anode electrode 34, the vacuum chamber 11 and the material container 13 of the electron gun 20 are all placed at the ground potential, and the irradiation object 50 is also placed at the ground potential via the material container 13. ing.

The electron beam is first accelerated by the difference (40 kV) between the potential of the cathode electrode 32 (here, 40 kV) and the potential of the anode electrode 34 (0 V), and obtains 40 keV energy. Thereafter, it passes through a ground potential space (that is, an electric field free space), and with reference to FIG. 1, the irradiation object 50 placed at the ground potential is irradiated with energy of 40 keV, and the irradiation object 50 is heated.

In the present embodiment, the power of the electron beam is determined by the current of the electron beam. When the current is 1 A, 40 kV × 1 A = 40 kW.
X-rays having energy lower than that of the electron beam are emitted from the irradiation object 50 irradiated with the electron beam. The power of the electron beam irradiated to the irradiation object 50 is larger than the power of the electron beam normally used in the field of X-ray analysis, and the intensity of the X-ray emitted from the irradiation object 50 is normal in the field of X-ray analysis. Two or more orders of magnitude greater than the intensity of the X-ray to be measured.

X-rays emitted from the irradiation object 50 enter the deposition prevention filter 65. The anti-adhesion filter 65 is rotated about the central axis of the rotation shaft 67a by the rotation shaft rotating device 67b. When the opening 66 faces the attenuation filter 61, the X-rays that have passed through the opening 66 are attenuated filter 61. Is incident on.
The X-rays incident on the attenuation filter 61 are absorbed or reflected inside the attenuation filter 61 and attenuated.

The X-rays that have passed through the attenuation filter 61 enter the spectroscopic unit 63b through the window member 63c of the X-ray detection unit 63. The spectroscopic unit 63b generates an electric signal corresponding to the energy (or wavelength) of the incident X-ray, and the storage device 68 receives the electric signal generated by the spectroscopic unit 63b and generates an electric signal for each X-ray energy (or wavelength). Stores the number of signals. In this way, the X-ray measurement device 62 measures the relationship between the energy and intensity of X-rays that have passed through the attenuation filter 61.
The computer 69 reads the stored contents of the storage device 68 and obtains the concentration of an element (that is, impurity) other than the main component (silicon) contained in the irradiation object 50 based on the stored contents.

While the irradiation object 50 is irradiated with an electron beam and heated, the concentration of impurities contained in the irradiation object 50 can be known. Therefore, in order to know the concentration of impurities, the irradiation of the electron beam is stopped as in the prior art. There is no need to open the vacuum chamber 11 to the atmosphere, and production time can be greatly reduced.

The irradiation object 50 irradiated with the electron beam and heated is melted, the impurities contained in the irradiation object 50 are evaporated, and the concentration of the impurities contained in the irradiation object 50 is reduced.
An anti-adhesion filter 65 is disposed between the irradiation object 50 and the attenuation filter 61. When the shielding part other than the opening 66 of the attenuation filter 61 and the anti-adhesion filter 65 faces each other, the vapor is shielded by the shielding part. Thus, the vapor does not reach the attenuation filter 61 and the vapor that has passed through the opening 66 reaches the attenuation filter 61 when the attenuation filter 61 and the opening 66 face each other.

If the vapor adheres to and accumulates on the attenuation filter 61, the X-ray attenuation rate of the attenuation filter 61 increases, leading to a decrease in measurement accuracy in the X-ray measuring device 62. The vapor reaching the pressure is attenuated, and the vapor is prevented from adhering to and depositing on the attenuation filter 61.

The vacuum chamber 11 is evacuated, and the impurity vapor is evacuated by the vacuum evacuation device 12 and removed from the vacuum chamber 11.
A controller 17 is connected to the computer 69. When the impurity concentration obtained by the computer 69 becomes a predetermined threshold value or less, the control device 17 sends a control signal to the electron gun power supply 40 to stop the irradiation of the electron beam from the electron gun 20.

In this manner, the concentration of impurities contained in the irradiation object 50 can be confirmed while irradiating the irradiation object 50 with an electron beam, and the irradiation of the electron beam can be stopped at an appropriate timing. Therefore, products with stable quality can be produced.

(Dissolved material recovery process)
A mold container 19 is disposed in the vacuum chamber 11, and an inclination mechanism 18 for inclining the material container 13 is provided in the material container 13.

After stopping the irradiation of the electron beam, the material container 13 is tilted by the tilt mechanism 18, and the purified irradiation object 50 in the material container 13 is put into the mold container 19.
Next, the orientation of the material container 13 is returned to the original by the tilt mechanism 18, the unpurified irradiation object 50 is arranged in the material container 13 by the material carry-in device 14, and the above-described vacuum dissolution and purification process is repeated.

After the vacuum dissolution and purification step and the dissolved material recovery step are repeated a predetermined number of times, the inside of the vacuum chamber 11 is opened to the atmosphere, the purified irradiation object is taken out from the mold container 19, and the vacuum chamber 11 is evacuated. A vacuum atmosphere is formed and the vacuum dissolution purification process is resumed.

In the above-described vacuum melting and refining, the irradiation object 50 has been described using a melting material containing silicon as a main component. However, the irradiation object 50 is not limited to this as long as the main component is a dissolving material, and titanium is not limited thereto. Alternatively, a melting material mainly composed of stainless steel, tantalum, tungsten, or the like may be used for the irradiation object 50.

Note that the power of the electron beam is adjusted according to the type of the irradiation object 50. Compared to silicon, titanium, and stainless steel, it is necessary to irradiate a higher power electron beam in order to dissolve a melting material mainly composed of tantalum or tungsten which is a high melting point metal.

<Structure of vacuum processing apparatus of second example>
The structure of the vacuum processing apparatus of the second example of the present invention will be described.
FIG. 5 is an internal configuration diagram of the vacuum processing apparatus 10b of the second example. Of the structure of the vacuum processing apparatus 10b of the second example, the same parts as those of the structure of the vacuum processing apparatus 10a of the first example are denoted by the same reference numerals and description thereof is omitted.

The vacuum processing apparatus 10b of the second example has an anti-adhesion filter 65 ′ having another structure instead of the anti-adhesion filter 65 of the vacuum processing apparatus 10a of the first example.
The anti-adhesion filter 65 ′ is a substance that shields vapor particles and transmits X-rays. Here, a plastic film having a thickness of 1 μm to 10 μm is used. The anti-adhesion filter 65 ′ is formed in a band shape whose width is larger than the diameter of the attenuation filter 61, and is wound around in a roll shape around one end in the longitudinal direction.

A driven shaft 68b is inserted into the center of the roll of the anti-adhesion filter 65 ', and a drive shaft 68a is fixed to the longitudinal end of the anti-adhesion filter 65' drawn out from the outer periphery of the roll.
The drive shaft 68a and the driven shaft 68b are arranged opposite to each other in parallel with each other across the position facing the attenuation filter 61. The drive shaft 68a is connected to the drive shaft 68a and the central axis of the drive shaft 68a. A drive shaft rotating device 68c that rotates around is connected.

When the drive shaft 68a is rotated by the drive shaft rotating device 68c, the anti-adhesion filter 65 'is pulled by the drive shaft 68a and taken up, and the driven shaft 68b is rotated by the force and the anti-adhesion filter 65' is fed out from the roll. It is. At this time, a force opposite to the rotational force of the pulling force generated by the drive shaft 68a is generated on the driven shaft 68b, and the anti-adhesion filter 65 ′ between the drive shaft 68a and the driven shaft 68b is generated by the two forces. It is designed to be stretched flat.

In the vacuum processing apparatus 10b of the second example, unlike the vacuum processing apparatus 10a of the first example, the vapor incident on the deposition preventing filter 65 ′ is attached to and shielded by the deposition preventing filter 65 ′, and the damping filter 61 Is not to reach.

On the other hand, the X-rays incident on the deposition prevention filter 65 ′ pass through the deposition prevention filter 65 ′ and reach the attenuation filter 61. More X-rays can reach the attenuation filter 61 than the deposition filter 65 of the vacuum processing apparatus 10a of the first example, and X-ray detection with higher sensitivity is possible.

When vapor adheres to and accumulates on the portion of the anti-adhesion filter 65 'facing the attenuation filter 61, the X-rays are attenuated by the adhesion film, but the portion to which the vapor adheres is wound around the drive shaft 68a. Therefore, vapor does not continue to adhere to and accumulate on the part facing the attenuation filter 61, and even if the electron beam irradiation is continued, the deposition prevention filter 65 ′ transmits X-rays at a constant rate and reaches the attenuation filter 61. be able to.
The vacuum processing method using the vacuum processing apparatus 10b of the second example is the same as the vacuum processing method using the vacuum processing apparatus 10a of the first example, and description thereof is omitted.

<Structure of the vacuum processing apparatus of the third example>
The structure of the vacuum processing apparatus of the third example of the present invention will be described.
FIG. 6 is an internal configuration diagram of the vacuum processing apparatus 10c of the third example. Of the structure of the vacuum processing apparatus 10c of the third example, the same parts as those of the structure of the vacuum processing apparatus 10a of the first example are denoted by the same reference numerals and description thereof is omitted.

In the vacuum processing apparatus 10c of the third example, the deposition prevention filter 65 of the vacuum processing apparatus 10a of the first example is omitted, and the attenuation filter 61 and the X-ray detection unit 63 are made of material in the lateral direction (horizontal direction) of the material container 13. It is arranged as far as possible from the container 13.

In general, the amount of vapor reached is inversely proportional to the square of the distance from the irradiation object 50. Further, the vapor angle distribution is proportional to cos ⁿ Φ where the direction directly above the irradiation object 50 is 0 degree and the angle from the angle is Φ (n takes a value of 4 to 8). Therefore, the amount of steam released in the lateral direction is cos ⁿ 90 ° = 0. Moreover, since the vapor | steam which reaches | attains the wall surface of the vacuum chamber 11 adheres to a wall surface and accumulates, it hardly reflects on a wall surface.
Therefore, in the vacuum processing apparatus 10c of the third example, the vapor hardly reaches the attenuation filter 61 without using the deposition prevention filter 65.

On the other hand, X-rays are emitted from the irradiation object 50 because the ratio of reflection on the walls of the vacuum chamber 11 and other structural members (that is, the casing 21 of the electron gun 20, the material carry-in device 14, and the material container 13) is large. The X-rays thus made enter the attenuation filter 61, and the X-rays that have passed through the attenuation filter 61 are measured by the X-ray measuring device 62.

In the vacuum processing apparatus 10c of the third example, the deposition preventing filter 65 can be omitted as compared with the vacuum processing apparatus 10a of the first example, so that the cost is reduced.
The vacuum processing method using the vacuum processing apparatus 10c of the third example is the same as the vacuum processing method using the vacuum processing apparatus 10a of the first example, and description thereof is omitted.

<Structure of the vacuum processing apparatus of the fourth example>
The structure of the vacuum processing apparatus of the fourth example of the present invention will be described.
FIG. 7 is an internal configuration diagram of the vacuum processing apparatus 10d of the fourth example. Of the structure of the vacuum processing apparatus 10d of the fourth example, the same parts as those of the vacuum processing apparatus 10a of the first example are denoted by the same reference numerals, and description thereof is omitted.

In the vacuum processing apparatus 10d of the fourth example, a film formation target holding unit 70 that holds the film formation target 55 is added as compared with the vacuum processing apparatus 10a of the first example.
In this embodiment, the film formation target 55 is a band-shaped film, and is configured to be wound in a roll shape around one end in the longitudinal direction. Here, films such as PET, PP, and polyimide having a width of 600 to 1200 mm, a thickness of 2 to 3 μm, and a roll length of about 1600 m are used.

The vapor incident on the film formation target 55 adheres to the film formation target 55 to form a thin film, and X-rays incident on the film formation target 55 are transmitted through the film formation target 55.
The film formation target holding unit 70 includes a winding shaft 71 disposed in the vacuum chamber 11 and a winding shaft rotating device 73 that rotates the winding shaft 71 about the central axis of the winding shaft 71. ing.

A roll made of the film formation target 55 is disposed in the vacuum chamber 11, and a roll holding shaft 72 is inserted in the center of the roll.
The winding shaft 71 and the roll holding shaft 72 are arranged opposite to each other in parallel and facing each other across the flight path of the steam emitted from the irradiation object 50. The longitudinal end of the film formation target 55 drawn from the outer periphery of the roll held by the roll holding shaft 72 is wound around and fixed to the take-up shaft 71 in a state of crossing the flight path of the steam. .

When the take-up shaft 71 is rotated by the take-up shaft rotating device 73, the film formation target 55 is pulled and taken up by the take-up shaft 71, and the roll holding shaft 72 is rotated by the force and the film formation target is removed from the roll. Object 55 is paid out. At this time, a force opposite to the rotational force of the pulling force generated by the take-up shaft 71 is generated on the roll holding shaft 72, and the film is formed between the take-up shaft 71 and the roll holding shaft 72 by the two forces. The object 55 is stretched flat.

Between the film formation target 55 and the material container 13, a deposition preventing plate 75 that shields vapor is disposed so as to cover the surface of the film formation target 55 exposed on the material container 13 side. The material of the deposition preventive plate 75 is molybdenum here, and an opening 76 that allows X-rays and steam to pass therethrough is provided at a position of the deposition preventive plate 75 that faces the irradiation target 50 in the material container 13.
A part of the vapor released from the irradiation object 50 in the material container 13 passes through the opening 76 of the deposition preventing plate 75 and reaches and adheres to the part of the film formation object 55 exposed from the opening 76.

The X-ray measurement apparatus 62 is configured so that the window member 63c faces the irradiation object 50 in the material container 13 and the irradiation object 50 as viewed from the portion facing the opening 76 in the film formation object 55. Is disposed on the opposite side, and the attenuation filter 61 is disposed between the X-ray measurement apparatus 62 and the film formation target 55 so as to face the window member 63c.

That is, the attenuation filter 61 is disposed on the side opposite to the irradiation object 50 when viewed from the film formation object 55. In other words, the film formation target 55 is disposed between the irradiation target 50 and the attenuation filter 61. Therefore, the vapor that has passed through the opening 76 of the deposition preventing plate 75 adheres to the film formation target 55 and is blocked, and the vapor does not reach the attenuation filter 61.
Therefore, in this embodiment, the anti-adhesion filter 65 is omitted as compared with the vacuum processing apparatus 10a of the first example.

The film formation target 55 is not limited to a belt-shaped film but may be a plate. When there is a possibility that the vapor reaches the attenuation filter 61, the anti-adhesion filters 65 and 65 ′ may be added similarly to the

vacuum processing apparatuses

10a and 10b of the first example and the second example. Similarly to the vacuum processing apparatus of the example, the attenuation filter 61 and the X-ray detection unit 63 may be arranged as far as possible from the material container 13 in the lateral direction (horizontal direction) of the material container 13.

<Vacuum processing method using the vacuum processing apparatus of the fourth example>
A vacuum processing method using the vacuum processing apparatus 10d of the fourth example will be described taking aluminum vacuum deposition as an example.

(Preparation process)
In this embodiment, a film forming material mainly composed of aluminum is used for the irradiation object 50. The concentration of impurities contained in the irradiation object 50 before irradiation with an electron beam is known in advance.

A threshold value of the impurity concentration in the film forming material used when stopping the electron beam irradiation is determined in advance. Further, it is set in the computer 69 that the main element is aluminum.
Further, the range of X-ray energy (or wavelength) measured by the X-ray measuring device 62 is set in advance to a range equal to or lower than the energy of the electron beam.

Referring to FIG. 7, the vacuum chamber 11 is evacuated by the evacuation device 12 to form a vacuum atmosphere. Thereafter, evacuation is continued and the vacuum atmosphere in the vacuum chamber 11 is maintained.
While maintaining the vacuum atmosphere in the vacuum chamber 11, the irradiation object 50 is carried into the vacuum chamber 11 by the material carry-in device 14 and placed in the material container 13. Power is supplied from the X-ray detection unit power supply 64 to the spectroscopic unit 63b of the X-ray detection unit 63 in advance.

(Vacuum deposition process)
An electron beam is emitted from the electron gun 20. The method of emitting the electron beam from the electron gun 20 is the same as the method of emitting the electron beam from the electron gun in the vacuum processing method using the vacuum processing apparatus 10a of the first example, and the description thereof is omitted.

X-rays are emitted from the irradiation object 50 irradiated with the electron beam. The power of the electron beam irradiated to the irradiation object 50 is larger than the power of the electron beam normally used in the field of X-ray analysis, and the intensity of the X-ray emitted from the irradiation object 50 is normal in the field of X-ray analysis. Two or more orders of magnitude greater than the intensity of the X-ray to be measured.

Part of the X-rays emitted from the irradiation object 50 enters the film formation object 55 through the opening 76 of the deposition preventing plate 75. The X-rays incident on the film formation target 55 pass through the attenuation filter 61 without being attenuated.
The X-rays incident on the attenuation filter 61 are absorbed or reflected inside the attenuation filter 61 and attenuated.

The X-rays that have passed through the attenuation filter 61 enter the spectroscopic unit 63b through the window member 63c of the X-ray detection unit 63. The spectroscopic unit 63b generates an electric signal corresponding to the energy (or wavelength) of the incident X-ray, and the storage device 68 receives the electric signal generated by the spectroscopic unit 63b and generates an electric signal for each X-ray energy (or wavelength). Stores the number of signals. In this way, the X-ray measurement device 62 measures the relationship between the energy and intensity of X-rays that have passed through the attenuation filter 61.
The computer 69 reads the stored contents of the storage device 68 and obtains the concentration of an element (ie, impurity) other than the main component (aluminum) contained in the irradiation object 50 based on the stored contents.

While the irradiation object 50 is irradiated with an electron beam and heated, the concentration of impurities contained in the irradiation object 50 can be known. Therefore, in order to know the concentration of impurities, the irradiation of the electron beam is stopped as in the prior art. There is no need to open the vacuum chamber 11 to the atmosphere, and production time can be greatly reduced.
The irradiation object 50 irradiated with the electron beam and heated is melted, the main component vapor is released from the irradiation object 50, and a part of the vapor passes through the opening 76 of the deposition preventing plate 75.

The take-up shaft 71 is rotated by the take-up shaft rotating device 73 so that the film formation target 55 travels at a predetermined speed (350 m / min in this case) so as to cross the steam flight path.
The vapor that has passed through the opening 76 reaches and adheres to the portion of the film formation target 55 exposed from the opening 76, and a thin film is formed on the surface of the film formation target 55.

The film formation target 55 is wound around the winding shaft 71 on the end point side from the position where the vapor enters in the moving direction of the film formation target 55.
In this manner, an aluminum thin film having a predetermined film thickness (here, several 100 nm (film resistance is 1.6Ω)) is continuously formed on the film formation target 55.
Since the vapor is shielded by the film formation target 55 and does not reach the attenuation filter 61, the X-ray attenuation rate of the attenuation filter 61 does not increase, and the measurement accuracy of the X-ray measurement device 62 does not decrease.

After the film formation for one roll is completed, the irradiation of the electron beam is stopped, the vacuum exhaust device 12 is stopped, the inside of the vacuum chamber 11 is released to the atmosphere, and the roll formed of the film formation target 55 is vacuumed. It is carried out to the outside of the tank 11. Next, after a new roll made of an undeposited film formation target 55 is carried into the vacuum chamber 11 and mounted on the roll holding shaft 72 and the take-up shaft 71, the vacuum chamber 11 is evacuated to create a vacuum atmosphere. Form and restart the vacuum deposition process.

When the irradiation object 50 is continuously irradiated with the electron beam, the main component evaporates from the irradiation object 50, so that impurities contained in the irradiation object 50 are concentrated and the impurity concentration increases.
Further, a part of the vapor emitted from the irradiation object 50 is deposited on the surface of the deposition plate 75 and the inner wall surface of the vacuum chamber 11, but the vapor is deposited on the surface of the deposition plate 75 and the vacuum chamber 11. If it continues to deposit on the inner wall surface, the deposited adhesion film peels off and reaches the irradiation object 50, and molybdenum, which is the material of the deposition preventing plate 75, and stainless steel, which is the material of the vacuum chamber 11, enter the irradiation object 50. As a result, the impurity concentration of the irradiation object 50 increases.

The control device 17 is connected to the computer 69. When the impurity concentration obtained by the computer 69 exceeds a predetermined threshold value, the control device 17 sends a control signal to the electron gun power supply 40 to stop the irradiation of the electron beam from the electron gun 20.

After the inside of the vacuum chamber 11 is opened to the atmosphere and the irradiation object 50 mixed with impurities is replaced with a new irradiation object 50, the vacuum chamber 11 is evacuated to form a vacuum atmosphere, and a vacuum deposition process is performed. Resume.
In this way, the concentration of impurities contained in the irradiation object 50 can be confirmed while irradiating the irradiation object 50 with an electron beam, and the film quality of the film to be formed can be kept constant. Therefore, the product yield can be improved.

In the above-described vacuum deposition, the irradiation object 50 has been described using a film forming material mainly composed of aluminum, but the irradiation object 50 is not limited to this as long as the film forming material has a known main component. A film-forming material mainly composed of titanium, copper, or the like may be used for the irradiation object 50.

10a to 10d …… Vacuum processing device 11 …… Vacuum chamber 12 …… Vacuum exhaust device 20 …… Electron gun 50 …… Irradiation target 55 …… Film formation target 61 …… Attenuation filter 62 …… X-ray measurement device 65 …… Anti-adhesion filter 69 …… Computer 71 …… Take-up shaft 73 …… Take-up shaft rotating device

Claims

A vacuum chamber;
An electron gun that irradiates and heats an irradiation object disposed in the vacuum chamber and vaporizes a specific component contained in the irradiation object;
A vacuum processing apparatus comprising:
An X-ray measurement device that measures the relationship between the energy and intensity of X-rays within a predetermined energy range;
A vacuum processing apparatus comprising: an attenuation filter that makes X-rays emitted from the irradiation object incident by irradiation of the electron beam, attenuates and passes the incident X-rays, and enters the X-ray measurement apparatus.
A calculator for determining the concentration of impurities contained in the irradiation object based on the measurement result of the X-ray measurement apparatus;
The vacuum processing apparatus according to claim 1.
The adhesion prevention filter which attenuate | damps the vapor | steam discharged | emitted from the said irradiation target object and reaching | attains the said attenuation filter between the said irradiation target object and the said attenuation filter is arrange | positioned. The vacuum processing apparatus according to item.
The vacuum processing apparatus according to any one of claims 1 to 3, wherein the specific component is an impurity of the irradiation object, and the concentration of the impurity contained in the irradiation object is reduced by irradiation with the electron beam. .
The specific component is a main component of the irradiation object,
A film formation object is disposed between the irradiation object and the attenuation filter,
The thin film is formed by releasing the vapor of the main component from the irradiation object by the irradiation of the electron beam, and allowing the vapor to reach the film formation object disposed in the vacuum chamber. 4. The vacuum processing apparatus according to any one of 3 above.
A winding shaft disposed in the vacuum chamber;
A winding shaft rotating device that rotates the winding shaft around a central axis of the winding shaft;
The film formation target is a band-shaped film,
One end in the longitudinal direction of the film formation object is wound around the winding shaft and fixed,
The vacuum processing apparatus according to claim 5, wherein the film formation target is wound on the winding shaft when the winding shaft is rotated by the winding shaft rotating device.
While evacuating the inside of the vacuum chamber, the irradiation target placed in the vacuum chamber is irradiated with an electron beam and heated to vaporize a specific component contained in the irradiation target,
Using an attenuation filter that allows X-rays emitted from the irradiation object to be incident upon irradiation with an electron beam and attenuates and passes the incident X-rays.
A vacuum processing method for measuring a relationship between energy and intensity of X-rays within a predetermined energy range among X-rays passing through the attenuation filter while irradiating the irradiation object with an electron beam.
The vacuum processing method according to claim 7, wherein the concentration of impurities contained in the irradiation object is determined based on the relationship between the measured X-ray energy and intensity while irradiating the irradiation object with an electron beam.
The vacuum processing method according to any one of claims 7 and 8, wherein an anti-adhesion filter that attenuates vapor that is emitted from the irradiation object and reaches the attenuation filter is used.
The specific component is an impurity of the irradiation object, and the irradiation object is irradiated with an electron beam to reduce the concentration of the impurity contained in the irradiation object. The vacuum processing method according to item.
The specific component is a main component of the irradiation object, and the irradiation object is irradiated with an electron beam to release the vapor of the main component from the film formation object, and the irradiation object, the attenuation filter, The vacuum processing method according to claim 7, wherein the vapor is made to reach a film formation target disposed between the layers to form a thin film.
The film formation target is a band-shaped film,
The vacuum processing method according to claim 11, wherein the film formation target is wound up on the end point side from the position where the vapor is incident with respect to the moving direction of the film formation target while irradiating the irradiation target with an electron beam. .