CN116929876A - Vacuum adsorption type spherical bending analysis crystal manufacturing method based on porous ceramics - Google Patents
Vacuum adsorption type spherical bending analysis crystal manufacturing method based on porous ceramics Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 94
- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 238000004458 analytical method Methods 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000005452 bending Methods 0.000 title claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 47
- 238000000605 extraction Methods 0.000 claims abstract description 19
- 238000007789 sealing Methods 0.000 claims abstract description 18
- 230000005540 biological transmission Effects 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 230000003287 optical effect Effects 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229920001721 polyimide Polymers 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004857 zone melting Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000004430 X-ray Raman scattering Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000003486 chemical etching Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 238000004846 x-ray emission Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 229920006332 epoxy adhesive Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses a porous ceramic-based vacuum adsorption type spherical bending analysis crystal manufacturing method, which comprises the following steps: 1) Preparing a planar pixel type crystal; 2) Selecting or preparing a shell, wherein the shell is internally provided with a light transmission structure; the plane pixel type crystal, the concave porous ceramic substrate and the air exhaust bottom plate are sequentially placed in the light transmission structure, and the fixing ring is used for pre-tightening; the concave surface of the concave porous ceramic substrate faces the plane pixel type crystal; the glass substrate of the planar pixel type crystal is connected with the bottom of the light-passing structure in a sealing way, and the side surface of the air extraction bottom plate is connected with the side wall of the light-passing structure in a sealing way; 3) And connecting an air extraction opening on the air extraction bottom plate with a vacuum pump to carry out air extraction, so that the planar pixel type crystal is bent and attached to the concave porous ceramic substrate, and a spherical bending analysis crystal is obtained. The invention enables high energy resolution analytical crystal production of <50 meV.
Description
Technical Field
The invention belongs to the technical field of optical elements, and relates to a vacuum adsorption type spherical bending analysis crystal manufacturing method based on porous ceramics.
Background
The spherical bending analysis crystal is a core optical element of an X-ray Roland circular spectrometer, has the dual functions of X-ray convergence and energy resolution, is widely applied to third and fourth generation synchronous radiation light sources, comprises a spectroscopy experimental method such as an X-ray absorption spectrum (HERFD), a resonance and non-resonance X-ray emission spectrum (XES, RXES), an X-ray Raman scattering (XRS), an inelastic scattering (IXS) and the like of high-energy resolution fluorescence detection, and can also be applied to laboratory light sources such as a desktop X-ray absorption spectrum/emission spectrum and the like. Common radii of curvature include 0.5 meters, 1 meter, and 2 meters, face-type encompasses spherical, cylindrical, ellipsoidal, toroidal, and the like, depending on the spectrometer design. The analysis crystal can be classified into a middle-low resolution analysis crystal of the order of about 1eV, a high resolution analysis crystal of the order of about 100meV, and an ultra-high resolution analysis crystal of the order of meV according to the energy resolution thereof, depending on the detected physical object. Whereas detection of resonance inelastic scattering requires a high resolution analysis crystal of about 100meV energy resolution for various magnetic excitations, charge transfer, etc. The manufacture of the crystal needs to bend high-resistance zone-melting monocrystalline silicon into a certain curvature, the wafer needs to be cut into small flat crystals with the square of 1 mm in order to eliminate stress caused by bending, the small flat crystals are tightly attached to a high-surface-type precision substrate by utilizing an anode bonding technology or an epoxy resin gluing technology to manufacture the crystal, and meanwhile, chemical etching is needed to eliminate stress and edge breakage caused by cutting. Common spherical crystal bending forming technology comprises the following steps: and (3) die bending, air film bending and vacuum adsorption bending forming technology.
Unlike such permanent bonding techniques, temporary bonding techniques, such as analytical crystal fabrication techniques based on vacuum adsorption, have also been developed in recent years, and such techniques have the advantage of flexibility and convenience in terms of exchangeable crystal materials, variable facets, and curvatures. The patent of the invention belongs to one of the emerging technologies.
The manufacture of the high-energy resolution analysis crystal needs to open a groove of a single crystal material, uniformly press-bend nearly ten thousands of small flat crystals on a substrate with a specific curvature, and requires that the orientation precision of the small flat crystals is better than 400urad, the manufacture method is complex, the success rate is extremely low, and only few synchronous radiation devices such as ESRF, APS and the like have the processing capability of the crystal at present.
The most recent approach to this patent is that described in the literature (Evan p.jahrman et al, rev.sci. Instrum.90, 0133106 (2019)), which uses a flange with polyimide film to mount and seal on a concave spherical substrate, uses a rubber gasket to seal, and uses a vacuum pump to pump air, where the polyimide film presses and bends the wafer onto the concave substrate under the action of the atmosphere. Since polyimide films are thin, little or no absorption of X-rays occurs, and thus do not affect the use of analytical crystals.
The existing method for manufacturing the spherical bending analysis crystal is only suitable for manufacturing the conventional medium-low energy resolution analysis crystal, and meanwhile, the detection of the fluorescence line in the low energy region is limited due to the existence of the polyimide film.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a vacuum adsorption type spherical bending analysis crystal manufacturing method based on porous ceramics. The invention adopts the porous ceramic material as the substrate, the porous ceramic material has the characteristics of easy polishing and good vacuum compatibility, the vacuum adsorption effect can be realized by utilizing the micropores of the porous ceramic, and the crystal material is bent and molded on the ceramic substrate, so that the analysis crystal energy resolution is better than 100meV.
The invention utilizes the principle of micropore ventilation of porous ceramic materials to realize the manufacture of vacuum adsorption type analysis crystals without film protection; a similar porous material is used as a concave substrate for the fabrication of spherical bending analysis crystals.
According to the invention, thin glass is used as a buffer layer of a monocrystalline material and a concave substrate, so that on one hand, a vacuum sealing effect is realized, and on the other hand, tens of thousands of small flat crystals are connected together, so that a flexible substrate is realized.
The technical scheme of the invention is as follows:
a vacuum adsorption type spherical bending analysis crystal manufacturing method based on porous ceramics comprises the following steps:
1) Preparing a planar pixel type crystal;
2) Selecting or preparing a shell, wherein the shell is internally provided with a light transmission structure; the plane pixel type crystal, the concave porous ceramic substrate and the air exhaust bottom plate are sequentially placed in the light transmission structure; the concave surface of the concave porous ceramic substrate faces the plane pixel type crystal; the glass substrate of the planar pixel type crystal is connected with the bottom of the light-passing structure in a sealing way, the side surface of the air extraction bottom plate is connected with the side wall of the light-passing structure in a sealing way, and the fixing ring is connected with the top of the light-passing structure and used for pre-tightening the planar pixel type crystal, the concave porous ceramic substrate and the air extraction bottom plate in the light-passing structure;
3) And connecting an air extraction opening on the air extraction bottom plate with a vacuum pump to carry out air extraction, so that the planar pixel type crystal is bent and attached to the concave porous ceramic substrate, and a spherical bending analysis crystal is obtained.
Further, the concave porous ceramic substrate is made of porous ceramic with a thickness of 9.5 mm and a diameter of 150 mm, the curvature radius of the concave porous ceramic substrate is R, and the R is determined according to the curvature of the spherical bending analysis crystal.
Further, the surface type precision of the concave porous ceramic substrate is 1/4 wavelength.
Further, a first rubber ring is arranged at the bottom of the light transmission structure, and the glass substrate of the planar pixel type crystal is connected with the bottom of the light transmission structure in a sealing way through the first rubber ring; the side face of the air extraction bottom plate is connected with the side wall of the light transmission structure in a sealing mode through a second rubber ring.
Further, the shell is a cylindrical aluminum shell.
Further, a porous ceramic having a thickness of 9.5 mm and a diameter of 150 mm was processed into a concave porous ceramic substrate having a radius of curvature R by an optical polishing method.
Further, the light-transmitting structure is a through hole.
Drawings
FIG. 1 is a flow chart of a planar pixel type crystal manufacturing process.
FIG. 2 is an assembled view of a vacuum adsorption type analytical crystal.
FIG. 3 is a schematic view of an aluminum housing and a sealing rubber ring.
FIG. 4 is a graph showing the change in vacuum degree with time of a vacuum adsorption type analysis crystal.
Fig. 5 is a graph of measured reflectance curves and fitted half-widths.
Detailed Description
The invention will now be described in further detail with reference to the accompanying drawings, which are given by way of illustration only and are not intended to limit the scope of the invention.
The invention relates to two links of manufacturing and packaging pixel type spherical crystals, wherein the first link is the manufacturing of planar pixel type crystals, and the second link is the assembly of vacuum adsorption type analysis crystals. Wherein fig. 1 is a process flow of manufacturing a planar pixel type crystal, which comprises the following steps: preparing a silicon single crystal material and a glass substrate with specific index surfaces, wherein the selected silicon single crystal material is a zone-melting intrinsic silicon single crystal, the resistivity is larger than 3000 ohm/cm, the index surface of the silicon single crystal material is determined according to a measuring object, for example, the 553 crystal orientation of silicon is selected when the copper element is measured, and the 531 crystal orientation of silicon is selected when the iron element is measured; the preferred Si (553) crystal orientation zone-melting high-resistance silicon single crystal material of this patent is illustrated as an example, wherein the crystal thickness is 3 mm and the crystal diameter is 4 inches; the glass substrate was selected from borosilicate glass with a thickness of 0.5 mm. The second step is to integrate the selected silicon single crystal material and the glass substrate using an anodic bonding or epoxy adhesive process. Thirdly, slotting, namely fully scribing monocrystalline silicon with the thickness of 3 mm by using a diamond scribing machine, and simultaneously keeping the glass substrate not broken as much as possible; the cutting width is 1.5X1.5mm 2 . Fourth stepThe chemical etching treatment is performed to eliminate stress introduced by cutting and to eliminate physical edge breakage effect, and the energy resolution of the analysis crystal is improved.
The etching solution used here was 40% nitric acid and 40% hydrofluoric acid, both 93:7 volume ratio, and etching time is 10 minutes.
The assembly of the vacuum adsorption type analysis crystal is shown in fig. 2, and the vacuum adsorption type analysis crystal comprises an aluminum shell, a planar pixel type crystal, a concave porous ceramic substrate, an air extraction bottom plate and a fixing ring from top to bottom; the aluminum shell is internally provided with a light transmission structure; the key material is a concave porous ceramic substrate, wherein porous ceramic with a thickness of 9.5 mm and a diameter of 150 mm is selected as a processing material, and the processing material is processed into a concave porous ceramic substrate with a radius of curvature R (R is determined according to the curvature of a spherical bending analysis crystal, R=2000 mm in the embodiment) by optical polishing, and the surface type precision is 1/4 wavelength (1 wavelength=632 nm). When the device is assembled, an aluminum shell is placed on a tabletop, a planar pixel type crystal, a concave porous ceramic substrate, an air exhaust bottom plate and a fixing ring are sequentially placed in the tabletop, the concave surface of the concave porous ceramic substrate faces to the planar pixel type crystal, an M6 inner hexagonal screw is arranged on a screw hole of the fixing ring and connected with the aluminum shell, and the whole device is fastened gradually; the fixed ring plays a pre-tightening role, the fixed ring enables the planar pixel analysis crystal and the porous ceramic to be closely attached through the extrusion of the air extraction bottom plate, and meanwhile, the lateral rubber ring (namely the second rubber ring) is pressed to enable the planar pixel analysis crystal and the porous ceramic to play a sealing role. And then, the suction opening of the KF16 welded on the suction bottom plate is connected with a vacuum pump through a corrugated pipe, and a valve is gradually opened to finish suction, so that the planar pixel type crystal is bent and attached to the concave porous ceramic substrate by atmospheric pressure.
The vacuum sealing of the whole device is realized through two rubber rings, and the first rubber ring is used for sealing the aluminum shell and the glass substrate of the planar pixel type crystal on the front surface, so that gas is ensured not to be sucked from the front surface. The second rubber ring is used for laterally sealing the joint of the air suction bottom plate and the aluminum shell. The invention sets the first rubber ring at the bottom of the light transmission structure, the glass substrate of the plane pixel type crystal is connected with the bottom of the light transmission structure through the seal of the first rubber ring; the side surface of the air extraction bottom plate is connected with the side wall of the light transmission structure in a sealing way through a second rubber ring; the machining precision, the error and the size of the rubber ring are required to be selected during assembly, so that the whole device can be conveniently installed and has good sealing performance, as shown in fig. 3.
Effect analysis of the invention:
1. vacuum maintenance effect:
the vacuum is applied by a vacuum dry pump, the final vacuum being about 1.2Pa. The vacuum level was about 720Pa after one week of standing with the bleed valve closed, and a vacuum leak of approximately 3.7Pa per hour was achieved. The actual requirement of vacuumizing once and maintaining a few weeks of experiments is met, as shown in fig. 4.
2. Vacuum adsorption type analysis of crystal energy resolution:
energy resolution testing was performed in japanese SPring8 BL11XU, the test conditions are shown in table 1; after the total energy resolution is 65.3meV, the deconvolution incident bandwidth, the light spot contribution and the detector pixel contribution are measured, the energy resolution of the analysis crystal reaches about 41meV, and the result meets the experimental requirement of resonance inelastic scattering.
Fig. 5 shows the energy resolution function (or reflectance curve) of vacuum adsorption type analytical crystal Si (553) made of porous ceramic substrate as concave substrate, and it can be seen that the full-peak half-width at half maximum of the curve reaches 65.3meV, where the broadening of the analytical crystal itself is about 41meV, very close to dar Wen Kuandu of planar crystal itself, and this experimental result shows that the present invention can realize the production of high energy resolution analytical crystal of <50 meV.
TABLE 1 test conditions and contributions of factors to energy resolution
Although specific embodiments of the invention have been disclosed for illustrative purposes, it will be appreciated by those skilled in the art that the invention may be implemented with the help of a variety of examples: various alternatives, variations and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out this invention, but that the invention will have the scope indicated by the scope of the appended claims.
Claims (7)
1. A vacuum adsorption type spherical bending analysis crystal manufacturing method based on porous ceramics comprises the following steps:
1) Preparing a planar pixel type crystal;
2) Selecting or preparing a shell, wherein the shell is internally provided with a light transmission structure; the plane pixel type crystal, the concave porous ceramic substrate and the air exhaust bottom plate are sequentially placed in the light transmission structure; the concave surface of the concave porous ceramic substrate faces the plane pixel type crystal; the glass substrate of the planar pixel type crystal is connected with the bottom of the light-passing structure in a sealing way, the side surface of the air extraction bottom plate is connected with the side wall of the light-passing structure in a sealing way, and the fixing ring is connected with the top of the light-passing structure and used for pre-tightening the planar pixel type crystal, the concave porous ceramic substrate and the air extraction bottom plate in the light-passing structure;
3) And connecting an air extraction opening on the air extraction bottom plate with a vacuum pump to carry out air extraction, so that the planar pixel type crystal is bent and attached to the concave porous ceramic substrate, and a spherical bending analysis crystal is obtained.
2. The method of claim 1, wherein the material of the concave porous ceramic substrate is a porous ceramic having a thickness of 9.5 mm and a diameter of 150 mm, and the radius of curvature of the concave porous ceramic substrate is R, which is determined from the curvature of the spherically curved analytical crystal.
3. The method of claim 2, wherein the concave porous ceramic substrate has a surface area accuracy of 1/4 wavelength.
4. The method according to claim 1, 2 or 3, wherein a first rubber ring is arranged at the bottom of the light-transmitting structure, and the glass substrate of the planar pixel type crystal is connected with the bottom of the light-transmitting structure in a sealing manner through the first rubber ring;
the side face of the air extraction bottom plate is connected with the side wall of the light transmission structure in a sealing mode through a second rubber ring.
5. A method according to claim 1 or 2 or 3, wherein the housing is a cylindrical aluminium housing.
6. A method according to claim 1, 2 or 3, characterized in that a porous ceramic with a thickness of 9.5 mm and a diameter of 150 mm is processed into a concave porous ceramic substrate with a radius of curvature R by means of an optical polishing method.
7. The method of claim 1, wherein the light passing structure is a via.
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