CN108300980B - X-ray zone plate preparation system - Google Patents
X-ray zone plate preparation system Download PDFInfo
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- CN108300980B CN108300980B CN201810028022.7A CN201810028022A CN108300980B CN 108300980 B CN108300980 B CN 108300980B CN 201810028022 A CN201810028022 A CN 201810028022A CN 108300980 B CN108300980 B CN 108300980B
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- chamber
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/458—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
- C23C16/4581—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber characterised by material of construction or surface finish of the means for supporting the substrate
Abstract
The invention relates to an X-ray zone plate preparation system. The system comprises: a chamber; the first precursor introducing pipeline is communicated with one end of the chamber and is used for conveying the first precursor into the chamber; the second precursor introducing pipeline is communicated with one end of the chamber and is used for conveying a second precursor into the chamber; the clamp is arranged in the cavity and used for fixing the columnar filament-shaped substrate; the muffle furnace wraps the cavity and is used for heating the cavity; one end of the air pumping pipeline is communicated with the other end of the cavity; and the vacuum pump is connected with the other end of the air pumping pipeline and pumps the inside of the cavity into vacuum through the air pumping pipeline. The invention can realize the alternate growth of two zone plate materials on a plurality of columnar filament-shaped substrates at the same time, and improve the processing efficiency of the zone plate.
Description
Technical Field
The invention relates to the technical field of atomic layer deposition, in particular to a preparation system of an X-ray zone plate.
Background
Atomic Layer Deposition (ALD) is a thin film preparation technology that can realize growth of a monoatomic layer, and its self-limitation and complementarity make the technology have excellent controllability for the composition and thickness of a thin film, and the prepared thin film has good conformality, high purity and uniformity, and has been widely used in various fields.
At present, an atomic layer deposition technology is adopted to prepare an X-ray zone plate, and the method is an effective method for improving the resolution ratio and the diffraction efficiency of the X-ray zone plate. The X-ray zone plate is an optical element of an X-ray wave band, has functions of dispersing, focusing, imaging and the like on X-rays, and the traditional preparation methods mainly comprise a laser holography method, an electron beam lithography method, a sputtering slicing method and the like, but the traditional preparation methods only can enable the width of the outermost ring of the zone plate to be about 20nm, meanwhile, the length-diameter ratio of the laser holography method and the electron beam lithography method in the process of preparing the zone plate is limited, and the sputtering slicing method is difficult to accurately control the width of each ring of the zone plate. Therefore, the conventional method has difficulty in realizing the fabrication of a zone plate with high resolution and high diffraction efficiency.
The preparation of the zone plate by the ALD technology can accurately control the width of each ring of the zone plate, has high thickness uniformity, and can control the width of the outermost ring below 10nm, thereby realizing the high resolution of sub-10 nm. And the slice and polishing by FIB can obtain any length-diameter ratio, so that the zone plate has high diffraction efficiency.
As shown in fig. 1, in a chamber 1 of a conventional ALD apparatus, a heat distribution plate 3 is generally disposed above a heating plate 2. Such a conventional ALD apparatus chamber often heats only a substrate in a sheet form, and when a target substrate is in a filament form, the ALD apparatus chamber does not have a fixture for fixing a metal filament, and cannot realize growth of a material on the filament-form substrate.
Disclosure of Invention
The invention aims to provide an X-ray zone plate preparation system which can grow zone plate materials on a filament substrate, so that the processing efficiency is greatly improved.
In order to solve the above technical problem, the present invention provides an X-ray zone plate preparation system, comprising: a chamber; the first precursor introducing pipeline is communicated with one end of the chamber and is used for conveying a first precursor into the chamber; the second precursor introducing pipeline is communicated with one end of the chamber and is used for conveying a second precursor into the chamber; a clamp disposed within the chamber for securing a cylindrical filament-shaped substrate; a muffle enclosing the chamber for heating the chamber; one end of the air pumping pipeline is communicated with the other end of the cavity; and the vacuum pump is connected with the other end of the air pumping pipeline and pumps the inside of the cavity into vacuum through the air pumping pipeline.
Further, the jig includes: the hollow cylindrical frame comprises a first annular end, a second annular end and a connecting rod, the first annular end and the second annular end are arranged in parallel relatively, and the first annular end and the second annular end are respectively fixed at two ends of the connecting rod; the axial direction of the hollow cylindrical frame is consistent with the direction of the gas flow of the first precursor and the second precursor; the hooks are symmetrically arranged on the first annular end and the second annular end; and two ends of the columnar filament-shaped substrate are respectively fixed on the pair of symmetrical hooks.
Further, the material of the clamp is one of stainless steel, aluminum, copper and tungsten.
Further, the chamber is of a cylindrical tubular structure, the first precursor and the second precursor flow linearly in a single direction in the chamber, and the longitudinal direction of the substrate is along the direction of the gas flows of the first precursor and the second precursor.
Furthermore, the chamber is a quartz tube, the wall thickness of the quartz tube is 2-5mm, the length of the quartz tube is 0.8-2m, and the inner diameter of the quartz tube is 1-5 cm.
Further, the outer diameter dimension of the first annular end and the second annular end is 5mm smaller than the inner diameter dimension of the quartz tube.
Further, the heating temperature of the muffle furnace is 50-1200 ℃.
Further, the system further comprises: and the vacuum gauge is arranged on the air exhaust pipeline and is used for measuring the vacuum degree in the cavity in real time.
Further, the material of the clamp is one of stainless steel, aluminum, copper and tungsten.
The technical scheme provided by the invention has the following technical effects or advantages:
1. the invention adopts the clamp to fix the columnar filament-shaped substrate, and can realize the alternate growth of two zone plate materials on the substrate with the shape;
2. the chamber of the invention adopts a columnar tubular structure, the precursor inlet pipelines of two precursors are arranged at one end of the columnar tubular structure, so that the unidirectional flow of precursor airflow is realized, and the longitudinal direction of the columnar filament substrate is along the direction of the precursor airflow, so that the process purging time is shortened;
3. in the invention, a muffle furnace is adopted to wrap a chamber, so as to maintain the constant temperature of a substrate;
4. the clamp is made of stainless steel, aluminum, copper, tungsten and the like, has good heat conductivity and small thermal expansion coefficient, and is favorable for conducting heat to the substrate fixed on the clamp.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an X-ray zone plate preparation system according to an embodiment of the present invention.
Fig. 2 is a diagram of a wire clamp according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, an embodiment of the present invention provides an X-ray zone plate preparation system, including: a chamber 3; a first precursor introducing pipeline 1, wherein the first precursor introducing pipeline 1 is communicated with one end of the chamber 3 and is used for conveying a first precursor into the chamber 3; a second precursor introducing pipeline 2, wherein the second precursor introducing pipeline 2 is communicated with one end of the chamber 3 and is used for conveying a second precursor into the chamber 3; a clamp 4, the clamp 4 being disposed within the chamber 3 for holding a columnar filament-shaped substrate 9; a muffle 5, said muffle 5 enclosing said chamber 3 for heating said chamber 3; an air suction pipeline 6, wherein one end of the air suction pipeline 6 is communicated with the other end of the cavity 3; and the vacuum pump 8 is connected with the other end of the air pumping pipeline 6, and the vacuum pump 8 pumps the inside of the cavity 3 into vacuum through the air pumping pipeline 6.
In this embodiment, the chamber 3 has a cylindrical tubular structure, the first precursor and the second precursor flow linearly in a single direction in the chamber 3, and the longitudinal direction of the substrate 9 is along the flow direction of the first precursor and the second precursor.
In this embodiment, as shown in fig. 2, the jig includes: the hollow cylindrical frame comprises a first annular end 41, a second annular end 42 and a connecting rod 43, wherein the first annular end 41 and the second annular end 42 are arranged in parallel relatively, and the first annular end 41 and the second annular end 42 are respectively fixed at two ends of the connecting rod 43; the axial direction of the hollow cylindrical frame is consistent with the direction of the gas flow of the first precursor and the second precursor; a plurality of hooks 44, wherein the plurality of hooks 44 are symmetrically arranged on the first annular end 41 and the second annular end 42; the two ends of the columnar filament-shaped substrate 9 are respectively fixed on a pair of symmetrical hooks 44.
In this example, a 30 μm diameter tungsten wire was selected as the substrate, both ends of the tungsten wire were respectively wound on the tooth-like structures of the holder 4, and both ends of the tungsten wire were fixed with Kapton tape, the tungsten wire being longitudinally along the direction of the precursor gas flow.
In this embodiment, the material of the clamp 4 is stainless steel, aluminum, copper, tungsten, or other metals. Stainless steel is preferred for this embodiment.
In the embodiment, the chamber 3 is a quartz tube, the wall thickness of the quartz tube is 2-5mm, the tube length is 0.8-2m, the inner diameter is 1-5cm, and the high temperature resistance can reach 1200 ℃. The first and second annular ends 41 and 42 have an outer diameter dimension that is 5mm less than the inner diameter dimension of the quartz tube.
In this embodiment, the heating temperature of the muffle furnace 5 is 50 to 1200 ℃.
In this embodiment, the system further includes: and the vacuum gauge 7 is arranged on the air suction pipeline 6 and is used for measuring the vacuum degree in the cavity 3 in real time.
The working process of the embodiment of the invention is as follows:
fixing a plurality of tungsten filaments in the chamber 3 through a clamp 4, so that the longitudinal direction of the tungsten filaments is consistent with the flow direction of the precursor; starting a vacuum pump 8, measuring the vacuum degree in the chamber 3 in real time through a vacuum gauge 7, and when the vacuum degree in the chamber is within the rangeTo meet the requirements, the precursor is introduced into the chamber 3. The two zone plate materials deposited in the embodiment of the invention are film laminated materials, one is a material with higher X-ray transmittance, such as C, Al and Al2O3、Si3N4Etc., preferably alumina, and the other being a material having a low X-ray transmittance such as Ag, Cu, Ni, Ir, SiO2、Ta2O5、 HfO2Etc., preferably HfO2、Ta2O5. The two selected materials are respectively conveyed into a chamber 3 through a first precursor inlet pipeline 1 and a second precursor inlet pipeline 2, and the process temperature of the two selected precursor materials is 200 ℃, namely the temperature of the tungsten filament required to be used as the substrate is kept at a constant temperature of 200 ℃; at the moment, the constant temperature of the tungsten filament at 200 ℃ is maintained by the muffle furnace 5, and the two precursors alternately grow zone plate materials on the tungsten filament substrate.
One or more technical solutions provided in the embodiments of the present invention have at least the following technical effects or advantages:
1. the invention adopts the clamp to fix a plurality of columnar filament-shaped substrates, can realize the alternate growth of two zone plate materials on the substrates with the shapes, and improves the processing efficiency of the zone plates;
2. the chamber of the invention adopts a columnar tubular structure, the precursor inlet pipelines of two precursors are arranged at one end of the columnar tubular structure, so that the unidirectional flow of precursor airflow is realized, and the longitudinal direction of the columnar filament substrate is along the direction of the precursor airflow, so that the process purging time is shortened;
3. according to the invention, the muffle furnace is adopted to wrap the chamber, so that the constant temperature of the substrate is maintained, and the growth thickness of the film is accurately controlled;
4. the clamp is made of stainless steel, has good heat conductivity and small thermal expansion coefficient, and is beneficial to conducting heat on the substrate fixed on the clamp.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (6)
1. An X-ray zone plate preparation system, the system comprising:
a chamber;
the first precursor introducing pipeline is communicated with one end of the chamber and is used for conveying a first precursor into the chamber;
the second precursor introducing pipeline is communicated with one end of the chamber and is used for conveying a second precursor into the chamber;
a clamp disposed within the chamber for securing a cylindrical filament-shaped substrate;
a muffle enclosing the chamber for heating the chamber;
one end of the air pumping pipeline is communicated with the other end of the cavity;
the vacuum pump is connected with the other end of the air pumping pipeline and pumps the inside of the cavity into vacuum through the air pumping pipeline;
wherein, the anchor clamps include:
the hollow cylindrical frame comprises a first annular end, a second annular end and a connecting rod, the first annular end and the second annular end are arranged in parallel relatively, and the first annular end and the second annular end are respectively fixed at two ends of the connecting rod; the axial direction of the hollow cylindrical frame is consistent with the direction of the gas flow of the first precursor and the second precursor;
the hooks are symmetrically arranged on the first annular end and the second annular end; two ends of the columnar filament-shaped substrate are respectively fixed on the pair of symmetrical hooks;
the chamber is of a columnar tubular structure, the first precursor and the second precursor flow linearly in the chamber in a unidirectional mode, and the longitudinal direction of the substrate is along the direction of gas flows of the first precursor and the second precursor.
2. The manufacturing system of claim 1, wherein: the clamp is made of one of stainless steel, aluminum, copper and tungsten.
3. The manufacturing system of claim 1, wherein: the chamber is a quartz tube, the wall thickness of the quartz tube is 2-5mm, the length of the quartz tube is 0.8-2m, and the inner diameter of the quartz tube is 1-5 cm.
4. The manufacturing system of claim 3, wherein: the outer diameter of the first annular end and the second annular end is 5mm smaller than the inner diameter of the quartz tube.
5. The manufacturing system of claim 1, wherein: the heating temperature of the muffle furnace is 50-1200 ℃.
6. The manufacturing system of claim 1, wherein: the system further comprises: and the vacuum gauge is arranged on the air exhaust pipeline and is used for measuring the vacuum degree in the cavity in real time.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810028022.7A CN108300980B (en) | 2018-01-11 | 2018-01-11 | X-ray zone plate preparation system |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810028022.7A CN108300980B (en) | 2018-01-11 | 2018-01-11 | X-ray zone plate preparation system |
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| CN108300980A CN108300980A (en) | 2018-07-20 |
| CN108300980B true CN108300980B (en) | 2020-10-09 |
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| CN109336418A (en) * | 2018-09-13 | 2019-02-15 | 中国科学院微电子研究所 | A kind of preparation method of center cylindricality glass optical fiber |
| CN112899652A (en) * | 2019-11-19 | 2021-06-04 | 中国科学院微电子研究所 | Device and method for preparing thin film material by atomic layer deposition |
| CN112899655A (en) * | 2019-11-19 | 2021-06-04 | 中国科学院微电子研究所 | Device and method for crystallizing thin film material |
| CN112899653A (en) * | 2019-11-19 | 2021-06-04 | 中国科学院微电子研究所 | High-temperature atomic layer deposition device and method |
| CN113088924A (en) * | 2021-04-07 | 2021-07-09 | 南京工业大学 | CVD device capable of locally and directionally depositing SiC coating and deposition method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100252049B1 (en) * | 1997-11-18 | 2000-04-15 | 윤종용 | The atomic layer deposition method for fabricating aluminum layer |
| JP2005104790A (en) * | 2003-10-01 | 2005-04-21 | Sumitomo Metal Mining Co Ltd | Method of manufacturing carbon nanotube and carbon nanotube embedded material |
| JP2007162093A (en) * | 2005-12-15 | 2007-06-28 | Dialight Japan Co Ltd | Film deposition method and film deposition device practicing the same |
| WO2009111782A1 (en) * | 2008-03-07 | 2009-09-11 | Dow Agrosciences Llc | Stabilized oil-in-water emulsions including meptyl dinocap |
| DE102010010937A1 (en) * | 2009-10-26 | 2011-04-28 | MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. | Method and device for producing a Fresnel zone plate |
| CN203754804U (en) * | 2014-02-24 | 2014-08-06 | 中科联碳（北京）科技有限公司 | Hot-wire tensioning mechanism for chemical vapor deposition diamond equipment |
| CN107119264B (en) * | 2017-06-14 | 2019-03-08 | 东南大学 | Iridium-alumina high temperature coating apparatus and technique are deposited with chamber In-situ reaction |
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