JP2988459B2 - X-ray spectrometer and method of manufacturing the same - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to relates to a silicon spectrometer and a manufacturing method thereof for use in spectroscopy of synchrotron radiation X-rays, in particular to a bonding method between the silicon crystal and the other silicon of spectroscope.

[0002]

2. Description of the Related Art Many spectroscopes used for spectroscopy using synchrotron radiation emit white light to a crystal and take out diffraction light from the crystal to perform monochromatization. There are several types of crystals that have been put into practical use, but silicon single crystals are most widely used because crystals having a large area (about 100 to 200 mm square) with few defects can be easily obtained. .

FIG. 3 is a conceptual diagram of a silicon spectroscope using a silicon single crystal as an X-ray spectroscopy element. X-ray source 31
X-ray white light emitted from the silicon crystal 32 for diffraction
Is diffracted by the light into a single color. Subsequently, the light is diffracted again by the diffraction silicon crystal 33 and is made monochromatic with higher precision. FIG. 3 shows an example in which a spectroscope is constituted by two spectroscopic elements. However, when a spectroscope is constituted by only one spectroscopic element, the spectroscope is constituted by more elements. In some cases.

A synchrotron radiation X-ray spectroscope is an optical device to which high-intensity and high-intensity white light is directly irradiated, and thermal crystal distortion due to irradiation causes quantitative and qualitative conversion of the resulting monochromatic light. Significantly deteriorates. Therefore, it is necessary to cool the crystal, and in order to obtain high-quality monochromatic light, the performance is a major factor that determines the performance of the spectroscope itself.

FIG. 4 is a perspective view showing a silicon crystal integrated type spectroscope conventionally used. In this method, anodic bonding is performed via a glass plate 42 between a base silicon substrate 41 and a silicon crystal for diffraction 43 in which a cooling groove 43a is opened, and cooling water is circulated in the cooling groove 43a (hereinafter, referred to as "cooling water").
(Referred to as a first conventional example).

FIG. 5 is a perspective view showing a silicon crystal integrated type spectroscope according to a direct bonding method which has been conventionally used. The direct bonding method is a method in which a diffraction silicon 53 having a cooling groove 53a is superimposed on a base silicon crystal 51 and a pressure is applied at a high temperature (for example, 1200 ° C.) to bond both crystals (hereinafter referred to as a second conventional example). ).

[0007]

In the first conventional example, even though the bonding strength of a large area is strong, strain is introduced into the silicon crystal due to a difference in thermal expansion coefficient. Further, in the second conventional example, the integrity of the crystal is not maintained due to the influence of the strain due to the heat treatment at a high temperature. In addition, bonding by this method requires high surface accuracy, but it is difficult to obtain surface accuracy in a large area, and the bonding is uneven and inadequate. There is.

[0008] The performance of a silicon spectral crystal used for X-ray spectroscopy is basically determined by the crystal material and the crystal plane orientation. However, in practice, the crystal distortion of the crystal spectral surface is greatly related to the energy resolution and the light amount of monochromatic X-rays.

In other words, a spectral crystal used under the use of synchrotron radiation requires a spectral crystal with excellent cooling performance, and it is important that no distortion is introduced into the crystal itself. However, according to the conventional method for manufacturing a spectral crystal, good spectral performance cannot be obtained because many strains remain in the crystal.

SUMMARY OF THE INVENTION The present invention has been made in view of the above, and has as its object to provide an X-ray crystal having a large-area, strain-free, high-quality spectral crystal without the above-mentioned problems, provided with a cooling mechanism.
An object of the present invention is to provide an X-ray spectroscope and a method for manufacturing the same.

[0011]

The above objects and objects are solved and achieved by the present invention described below. That is, the present invention relates to an X-ray spectrometer in which a plurality of silicon crystals are interposed.
An X-ray spectrometer that is anodically bonded with a glass material
Heat treatment above the temperature at which
It discloses an X-ray spectrometer characterized by the following. And book
The X-ray spectrometer of the present invention is the same as the X-ray spectrometer of the present invention described below.
It is obtained by a manufacturing method.
According to the present invention, in the method for manufacturing an X-ray spectrometer, an X-ray spectrometer in which a glass material is sandwiched between a plurality of silicon crystals and anodically bonded is heated at a temperature equal to or higher than a temperature at which the glass material softens. It also discloses a method of manufacturing an X-ray spectrometer.

The method for manufacturing an X-ray spectrometer according to the present invention comprises:
Prior to the step of bonding the plurality of silicon crystals, a method of performing a pretreatment to remove or form an oxide film on a bonding surface of the silicon crystal, and further comprising, before the bonding step, A method characterized by removing crystal distortion of the bonding surface of the above, further comprising a step of performing the bonding and heat treatment step in air, vacuum, or an inert gas atmosphere. There is also a method wherein the glass material is selected from the group consisting of low-melting glass and borosilicate glass, and the form of the glass is from a glass layer deposited or sputtered on plate glass or silicon. A method characterized by being selected from the group consisting of:
The method is characterized in that the time of the heat treatment is set to 10 minutes or more, and the method is characterized in that the glass layer is thicker than the roughness dimension of the unevenness of the bonding surface.

In the present invention, for the purpose of producing a large-area strain-free spectral crystal having a cooling mechanism, a silicon crystal processed with a cooling mechanism is anodic-bonded, and then a heat treatment is performed at a temperature higher than a temperature at which the glass softens. Specifically, for example, FIG.
As shown in the figure, a glass plate 12 is inserted between the silicon single crystal 13 for diffraction and the base silicon crystal 11, silicon is uniformly adhered to the glass over the entire bonding surface to perform anodic bonding, and then at a temperature higher than the temperature at which the glass softens. A heat treatment is performed.

As a result, it is possible to join large-area silicon crystals without crystal distortion even after the heat treatment, and it is possible to realize silicon spectral crystals having various cooling mechanisms. The present invention uses a plurality of silicon crystals as glass
In an X-ray spectroscopic crystal anodic-bonded via a material , a heat treatment was performed using a heater at a temperature higher than the temperature at which the glass softens.
X-ray spectrometer and its manufacturing method.

Here, prior to the bonding, an oxide film is removed or formed on the bonding surface of the silicon crystal and the crystal distortion is removed, and the bonding and heat treatment are performed in the air, in a vacuum, or in an inert gas atmosphere. By maintaining for 10 minutes or more, a silicon spectral crystal without crystal distortion can be obtained.

Therefore, in the present invention, for example, a pretreatment for removing an oxide film or forming an oxide film on a crystal surface is performed in advance, and etching is performed with an acid or alkali to remove crystal distortion. In addition, the glass layer
Anodic bonding is performed with a thickness greater than the roughness of the unevenness of the bonding surface. As a result, the contact area on the bonding surface can be increased, and a uniform bonding state can be obtained over a wide area over the entire bonding surface.

[0017]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be specifically described below. The silicon dispersive crystal forms a cooling groove on the back surface of the diffraction silicon crystal by machining. In the base silicon crystal, the inlet and outlet holes of the cooling water are formed by ultrasonic processing. These two crystals are etched with an acid or an alkali after processing to remove crystal distortion introduced at the time of processing, and the bonding surface is subjected to mechanochemical polishing to suppress surface irregularities and to be in a distortion-free state.

Further, a glass layer having a thickness corresponding to the unevenness of the surface is formed on the bonding surface by vapor deposition or sputtering so that silicon and glass are uniformly contacted on the entire bonding surface. As a result, uniform bonding can be achieved even over a wide area, and at the same time, the temperature applied during bonding, which is the largest cause of bonding distortion, can be reduced.

Next, by performing a heat treatment using a heater at a temperature higher than the temperature at which the glass softens, the distortion of the silicon crystal having a diffraction surface is removed, and a high-quality spectral element can be formed. Further, bonding by glass-silicon has high mechanical strength, is stable over time, and has excellent radiation resistance, so that a highly reliable spectroscope can be provided.

[0020]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The details of the present invention will be described below with reference to the drawings based on embodiments, but the present invention is not limited to these embodiments.

[First Embodiment] FIG. 1 is a schematic diagram showing a first embodiment of the present invention. As shown in the figure,
On the base silicon crystal 11, a diffraction silicon crystal 13 in which a cooling groove 13 a has been opened in advance is interposed via a glass plate 12. Then, the temperature of the base silicon crystal 11 and the diffraction silicon crystal 13
Then, a positive voltage was applied to the glass plate 12 and a negative voltage was applied to the glass plate 12 to perform anodic bonding at a voltage of 700 V. Thereafter, a heat treatment was performed at a temperature higher than the softening temperature of the glass.

The silicon crystal for diffraction after the heat treatment was free of distortion and exhibited good spectroscopic characteristics. It was also found that the glass did not hinder the flow of the cooling water after joining.

Embodiment 2 A second embodiment of the present invention will be described with reference to FIG. As shown in FIG. 2, a glass layer 22 is formed on the diffraction silicon crystal 23 by vapor deposition. After the formation of the glass layer 22, a cooling groove 23a is opened in the silicon crystal 23 for diffraction by a dicing apparatus. Then, the cooling groove 23 is formed on the base silicon crystal 21.
The silicon crystal for diffraction 23 is overlaid with a facing downward.

Then, anodic bonding is performed by the heater 24,
Thereafter, heat treatment was performed at a temperature higher than the temperature at which the glass softens.
No distortion was introduced into the silicon crystal for diffraction 23 after the heat treatment, and it was found that the silicon crystal 23 exhibited good spectral characteristics. The mechanical strength of the joint was strong. The glass layer may be formed on the base silicon crystal 21 side.

Although the preferred embodiments of the present invention have been described above, the present invention is not limited to these embodiments, and various modifications can be made within the scope described in the claims. For example, low melting point glass and borosilicate glass can be used as the types of silicon and glass.

[0026]

As described above, according to the present invention, since it is possible to join with sufficient mechanical strength, it is possible to flow the refrigerant directly into the dispersive crystal, and therefore, the thermal load is large. The crystal can be cooled uniformly and efficiently. In addition, since bonding is performed at a low temperature, crystal distortion can be suppressed, and remarkable effects such as formation of an element having excellent spectral characteristics can be obtained.

[Brief description of the drawings]

FIG. 1 is a schematic explanatory view showing a first embodiment of the present invention.

FIG. 2 is a schematic explanatory view showing a second embodiment of the present invention.

FIG. 3 is a conceptual diagram of a silicon spectroscope constituted by two silicon crystals for diffraction.

FIG. 4 is a perspective view showing a first conventional example.

FIG. 5 is a perspective view showing a second conventional example.

[Explanation of symbols]

11,21,41,51 Base silicon crystal 12,42 Glass plate 13,23,32,33,43,53 Diffraction silicon crystal 13a, 23a, 43a, 53a Cooling groove 14,24 Heater 22 Glass layer 31 X-ray source

Claims (10)

(57) [Claims] In an X-ray spectrometer, a plurality of silicon bonds are provided.
X-ray spectrometer with glass material sandwiched between crystals and anodically bonded
Is heated above the temperature at which the glass material softens.
An X-ray spectrometer characterized in that: 2. A method for manufacturing an X-ray spectrometer, wherein an X-ray spectrometer in which a glass material is sandwiched between a plurality of silicon crystals and subjected to anodic bonding is heated at a temperature equal to or higher than a temperature at which the glass material softens. To manufacture an X-ray spectrometer. 3. A pre-treatment for removing or forming an oxide film on a bonding surface of the silicon crystals prior to the step of bonding the plurality of silicon crystals.
A method for manufacturing the X-ray spectrometer described in the above. 4. The method of manufacturing an X-ray spectrometer according to claim 2, wherein prior to the bonding step, crystal distortion at a bonding surface of the silicon crystal is removed. 5. The method for manufacturing an X-ray spectrometer according to claim 2, wherein the bonding and heat treatment steps are performed in the air, in a vacuum, or in an inert gas atmosphere. 6. The method according to claim 2, wherein the glass material is selected from the group consisting of low melting point glass and borosilicate glass. 7. The method according to claim 2, wherein the form of the glass material is selected from the group consisting of a glass layer deposited or sputtered on a sheet glass or silicon. 8. The method for manufacturing an X-ray spectrometer according to claim 2, wherein the time of the heat treatment is set to 10 minutes or more. 9. The method according to claim 7, wherein the glass layer is thicker than a roughness dimension of the unevenness of the bonding surface.
A method for manufacturing an X-ray spectrometer. 10. The X-ray spectrometer according to claim 2, wherein :
The method for producing an X-ray spectrometer according to any one of
An X-ray spectrometer characterized in that: