CN109903877B - Manufacturing method of X-ray diffraction optical focusing element - Google Patents
Manufacturing method of X-ray diffraction optical focusing element Download PDFInfo
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Abstract
The invention discloses a method for manufacturing an X-ray diffraction optical focusing element with high diffraction efficiency and imaging resolution, which uses the technology of combining atomic layer deposition and focused ion beams, selects a metal tungsten filament as a central substrate filament of the X-ray diffraction optical focusing element to play a role of blocking zero-order light, uses a high-energy ion implanter to modify the surface of the metal tungsten filament before atomic deposition to enhance the combination firmness with an atomic deposition film, gives optimized parameters of the atomic deposition, and can obtain higher deposition rate and reliable film thickness controllability, so that the obtained optical focusing element has high diffraction efficiency and imaging resolution.
Description
Technical Field
The invention belongs to the treatment technology of ionizing radiation, in particular to a preparation method of a related element of an X-ray microscope, specifically belongs to a focusing treatment device of particles or ionizing radiation, and particularly relates to a manufacturing method of an X-ray diffraction optical focusing element applying diffraction.
Background
The X-ray has the characteristics of short wavelength, strong penetrating power and the like, and has wide application in the fields of space detection, medical treatment, energy, aerospace and the like. An X-ray spectrometer and an energy spectrometer are important tools for plasma diagnosis and space detection, an X-ray diffraction optical component serving as a core component of the X-ray spectrometer gradually becomes the core of the field of nano processing, and the X-ray diffraction optical component becomes the key of the space detection technology at the present stage. The X-ray diffraction optical component is widely applied to the fields of laser inertia about beam fusion, astronomical telescopes, synchrotron radiation, EUV lithography and the like. How to realize the X-ray diffraction optical element with high resolution and large height-width ratio provides great technical challenges for the nano-scale processing technology.
At present, the conventional preparation methods of the X-ray optical focusing element mainly include a laser holographic exposure method, an electron beam lithography method, a method combining an electron beam lithography and an X-ray lithography, a sputtering slicing method, and an atomic layer deposition cutting method starting from preliminary research make internal disorder or usurp. The laser holographic exposure method is mostly applied to the manufacture of an x-ray optical focusing element with the diameter of a few millimeters, a large area and a large number of ring zones, the processing precision of the technology is not high, only the manufacture of a periodic structure can be carried out, and the manufacture of a non-periodic pattern is very difficult. The optical focusing element prepared by the method has spherical aberration in the use process, and the spherical aberration needs to be corrected in the use process of the later optical focusing element. The electron beam lithography method has the characteristic of high precision in the field of micromachining, is very favorable for manufacturing a high-resolution soft X-ray optical focusing element, comprises various expanded preparation methods based on the electron beam lithography, and currently, the width of the outermost ring is 15nm, and the X-ray optical focusing element with the outermost ring of 12nm and the height-to-width ratio of 2.5 is prepared by adopting a secondary patterning technology in the national laboratory of Lorentsback in 2009 USA. However, due to the limitation of the technical characteristics, the technology approaches the technical limit in the aspect of simultaneously considering the small outermost ring size and the high aspect ratio, and the hard X-ray optical focusing element with the high aspect ratio is difficult to manufacture by using the method. The aspect ratio of a typical hard X-ray optical focusing element is larger than 16 to achieve high diffraction efficiency, but is still far from sufficient. The latter combination of electron beam and X-ray also does not allow for both a small outermost ring width dimension and a high aspect ratio. The sputtering slicing method is an effective means for obtaining the optical focusing element with extremely high aspect ratio, but the method is basically sputtering deposition in an inclined direction when the multi-layer film is deposited. The film thickness is difficult to realize high-precision control, the film thickness is uneven, the roughness is large, the two multi-layer film materials are seriously diffused, the boundary of the film layers is not clear, and an optical focusing element with high quality is difficult to manufacture. According to the technical scheme, an X-ray optical focusing element with the geometrical sizes of the outermost rings of 35nm and 10nm and the aspect ratio close to 250 is manufactured on the surface of a glass fiber filament by German Mapu intelligent research institute in 2013 for the first time by adopting a technology of combining atomic layer deposition and focused ion beams. However, since the central filament is a glass fiber filament, it has a large transmittance for X-rays, resulting in very strong zero-order light, which affects the diffraction efficiency and imaging resolution of the optical focusing element. If a metal wire is used, the bonding between the metal wire and the thin film is not firm due to stress and other unknown factors when the thin film is deposited on the surface of the metal wire, so that the technology of combining the atomic layer deposition and the focused ion beam has a plurality of problems to be overcome.
According to the search, Chinese patents 201510325463, X "preparation method of self-aligned double-layer X-ray diffraction optical focusing element" and 201110150368.2 "a method for preparing phase type X-ray diffraction optical focusing element" both disclose a preparation method of X-ray diffraction optical focusing element, but both adopt electron beam exposure process, the collapse of the photoresist structure is easily caused when the X-ray diffraction optical focusing element with large depth-width ratio is prepared, the X-ray diffraction optical focusing element with large depth-width ratio is difficult to prepare, the technology of combining atomic layer deposition and focused ion beam in the prior art does not disclose the parameters of the atomic layer deposition in detail, has no operability, these parameters have direct effects on the efficiency and effect of atomic layer deposition, and no method for solving the problems of bonding and weakness between the metal wire and the thin film is proposed.
Disclosure of Invention
In view of the above problems in the prior art, the present invention provides a method for manufacturing an X-ray diffraction optical focusing element having high diffraction efficiency and imaging resolution, which solves at least one of the problems known in the above prior art manufacturing methods.
In order to achieve the above object, the present invention provides a method for manufacturing an X-ray diffraction optical focusing element, which comprises the following steps:
a method of manufacturing an X-ray diffraction optical focusing element having high diffraction efficiency and imaging resolution, comprising the steps of:
step 1, etching a groove with the width and the depth of 5-25 micrometers and the length of 220 millimeters on the surface of a 12-inch monocrystalline silicon wafer in a chemical etching mode;
step 2, selecting a tungsten wire with the diameter of 3-20 mu m and the length of 200mm as a central filament;
fixing a tungsten filament in a groove etched on the surface of the wafer, and performing ion bombardment on the wafer fixed with the tungsten filament in a high-energy ion implanter, wherein the ion implanter has the following parameters during ion bombardment: the energy range is 1-1.8MeV, the ion source is phosphorus ions, and the bombardment time is 2-4 hours;
step 4, after the bombardment in the step 3 is finished, taking out the wafer from the ion implanter, rotating the tungsten filament by 180 degrees along the axial direction, fixing the tungsten filament in the groove etched on the surface of the wafer, and repeating the bombardment process in the step 3;
step 5, within one hour after the bombardment is finished, taking the tungsten wire prepared in the step 4 as a central substrate for atomic layer deposition and placing the central substrate in an atomic layer deposition system;
step 6, obtaining the corresponding number of layers according to the thickness and calculation of the outermost layer of the given X-ray diffraction optical focusing element, and alternately depositing aluminum oxide and hafnium oxide on the surface of the metal wire by utilizing an atomic layer deposition system to form a series of concentric ring structures;
and 7, after the film coating is finished, cutting the metal wire sample after the film coating into slices with proper thickness by using a focused ion beam technology, and polishing to prepare the X-ray diffraction optical focusing element meeting the requirements.
The specific deposition parameters are that a first precursor for depositing the aluminum oxide atomic layer is room-temperature Trimethylaluminum (TMA), a second precursor is room-temperature hydrogen peroxide, purging is carried out for 30s after the first precursor is introduced for 50ms, then purging is carried out for 20s after the second precursor is introduced for 40ms, the vacuum degree is kept below 0.1torr, and the temperature of the central substrate of the metal wire is kept at 120-150 ℃; the first precursor of the hafnium oxide atomic layer deposition is tetra (dimethylamino) hafnium (TDMAHf) with the temperature of 80 ℃, the second precursor is room-temperature hydrogen peroxide, purging is carried out for 50s after the first precursor is introduced for 125ms, then purging is carried out for 20s after the second precursor is introduced for 40ms, the vacuum degree is kept below 0.1torr, and the temperature of the metal wire central substrate is kept at 150-180 ℃.
Wherein, when the focused ion beam is used for cutting, gallium ions with the energy of 30kV and the ion beam current of more than 1000pA are adopted; and gallium ions with the energy of 30kV and the ion beam current of less than 1000pA are adopted during polishing. And after polishing, obtaining the X-ray diffraction optical focusing element with required precision and thickness.
Compared with the prior art, the invention has the advantages that:
the metal tungsten filament is selected as the central substrate filament of the X-ray diffraction optical focusing element, the metal tungsten filament has high density and can play a role in blocking zero-order light, the metal tungsten filament is subjected to surface modification by using a high-energy ion implanter before atomic deposition, the bonding firmness of the metal tungsten filament and an atomic deposition film is enhanced, the optimized parameters of the atomic deposition are given, and the parameter combination can obtain higher deposition rate and reliable film thickness controllability through multiple tests.
Detailed Description
It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
The specific implementation steps of the manufacturing method for preparing the X-ray diffraction optical focusing element with high diffraction efficiency and imaging resolution of the invention are as follows:
step 1, etching a groove with the width and the depth of 10 microns and the length of 220 millimeters on the surface of a 12-inch monocrystalline silicon wafer in a chemical etching mode;
step 2, selecting a tungsten wire with the diameter of 8 mu m and the length of 200mm as a central filament;
step 3, fixing a tungsten filament in a groove etched on the surface of the wafer, and performing ion bombardment on the wafer fixed with the tungsten filament in a high-energy ion implanter, wherein the high-energy ion implanter belongs to known equipment in the semiconductor industry, and the ion implanter with the energy upper limit of more than 1MeV can be called as a high-energy ion implanter, and the parameters during the ion bombardment are as follows: the energy range is 1-1.8MeV, the ion source is phosphorus ions, the bombardment time is 2-4 hours, the ion implanter can carry out four-quadrant implantation generally, the bombardment process preferably adopts a four-quadrant implantation program, and meanwhile, the energy is found to have direct influence on the surface modification degree in the experiment, the influence of the dose is not obvious, so the bombardment dose is not limited;
step 4, after the bombardment in the step 3 is finished, taking out the wafer from the ion implanter, rotating the tungsten filament by 180 degrees along the axial direction, fixing the tungsten filament in the groove etched on the surface of the wafer, and repeating the bombardment process in the step 3 to fully bombard the surface of the tungsten filament;
step 5, within one hour after the bombardment is finished, taking the tungsten wire prepared in the step 4 as a central substrate for atomic layer deposition and placing the central substrate in an atomic layer deposition system, wherein the time cannot be too long and cannot exceed two hours at most, the atomic layer deposition system can adopt known equipment, and is not particularly limited, and for example, a Beneq TFS-200 ALD deposition system can be adopted;
step 6, obtaining the corresponding layer number according to the thickness and calculation of the outermost layer of the given X-ray diffraction optical focusing element, wherein the calculation mode belongs to the common knowledge in the field and is not repeated, aluminum oxide and hafnium oxide are alternately deposited on the surface of the metal wire by utilizing an atomic layer deposition system to form a series of concentric ring structures, the specific deposition parameters are that a first precursor for aluminum oxide atomic layer deposition is room-temperature Trimethylaluminum (TMA), a second precursor is room-temperature hydrogen peroxide, purging is performed for 30s after the first precursor is introduced for 50ms, purging is performed for 20s after the second precursor is introduced for 40ms, the vacuum degree is kept below 0.1torr, and the temperature of the metal wire central substrate is kept at 140 ℃; the first precursor of the hafnium oxide atomic layer deposition is tetra (dimethylamino) hafnium (TDMAHf) with the temperature of 80 ℃, the second precursor is hydrogen peroxide with the temperature of room temperature, purging is carried out for 50s after the first precursor is introduced for 125ms, then purging is carried out for 20s after the second precursor is introduced for 40ms, the vacuum degree is kept below 0.1torr, and the temperature of the metal wire central substrate is kept at 160 ℃.
Step 7, after the film coating is finished, cutting the metal wire sample after the film coating into slices with proper thickness by utilizing a focused ion beam technology, polishing, and preparing an X-ray diffraction optical focusing element meeting the requirements, wherein gallium ions with the energy of 30kV and the ion beam current of more than 1000pA are adopted during the cutting by utilizing the focused ion beam; and gallium ions with the energy of 30kV and the ion beam current of less than 1000pA are adopted during polishing. And after polishing, obtaining the X-ray diffraction optical focusing element with required precision and thickness.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (2)
1. A method of manufacturing an X-ray diffraction optical focusing element having high diffraction efficiency and imaging resolution, comprising the steps of:
step 1, etching a groove with the width and the depth of 5-25 micrometers and the length of 220 millimeters on the surface of a 12-inch monocrystalline silicon wafer in a chemical etching mode;
step 2, selecting a tungsten wire with the diameter of 3-20 mu m and the length of 200mm as a central filament;
fixing a tungsten filament in a groove etched on the surface of the wafer, and performing ion bombardment on the wafer fixed with the tungsten filament in a high-energy ion implanter, wherein the ion implanter has the following parameters during ion bombardment: the energy range is 1-1.8MeV, the ion source is phosphorus ions, and the bombardment time is 2-4 hours;
step 4, after the bombardment in the step 3 is finished, taking out the wafer from the ion implanter, rotating the tungsten filament by 180 degrees along the axial direction, fixing the tungsten filament in the groove etched on the surface of the wafer, and repeating the bombardment process in the step 3;
step 5, within one hour after the bombardment is finished, placing the tungsten wire prepared in the step 4 in an atomic layer deposition system as a central substrate for atomic layer deposition;
step 6, according to the thickness of the outermost layer of the given X-ray diffraction optical focusing element and the corresponding calculated number of layers, alternately depositing aluminum oxide and hafnium oxide on the surface of the metal wire by utilizing an atomic layer deposition system to form a series of concentric ring structures;
and 7, after the film coating is finished, cutting the metal wire sample after the film coating into slices with proper thickness by utilizing a focused ion beam technology, adopting gallium ions with the energy of 30kV and the ion beam current of more than 1000pA during cutting, adopting gallium ions with the energy of 30kV and the ion beam current of less than 1000pA for polishing, and obtaining the X-ray diffraction optical focusing element with required precision and thickness after polishing.
2. The method of manufacturing an X-ray diffraction optical focusing element according to claim 1, wherein: the specific deposition parameters in the step 6 are that a first precursor for depositing the aluminum oxide atomic layer is room-temperature trimethylaluminum, a second precursor is room-temperature hydrogen peroxide, purging is carried out for 30s after the first precursor is introduced for 50ms, then purging is carried out for 20s after the second precursor is introduced for 40ms, the vacuum degree is kept below 0.1torr, and the temperature of the central substrate of the metal wire is kept at 120-150 ℃; the first precursor of the hafnium oxide atomic layer deposition is tetra (dimethylamino) hafnium at the temperature of 80 ℃, the second precursor is room-temperature hydrogen peroxide, the purging is carried out for 50s after the first precursor is introduced for 125ms, then the purging is carried out for 20s after the second precursor is introduced for 40ms, the vacuum degree is kept below 0.1torr, and the temperature of the metal wire central substrate is kept at the temperature of 150-180 ℃.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3867637A (en) * | 1973-09-04 | 1975-02-18 | Raytheon Co | Extended monochromatic x-ray source |
| CN102168294A (en) * | 2011-05-19 | 2011-08-31 | 北京工业大学 | Method for improving tungsten-base gold-plating bond strength |
| CN102585330A (en) * | 2012-01-18 | 2012-07-18 | 厦门虹鹭钨钼工业有限公司 | Tungsten-polymer composite material and preparation method thereof |
| WO2013191743A1 (en) * | 2012-02-17 | 2013-12-27 | The Massachusetts Institute Of Technology | Surface modification of cladding material |
| CN103924202A (en) * | 2014-04-03 | 2014-07-16 | 西南交通大学 | Metal support surface modification method |
| CN107833649A (en) * | 2017-10-16 | 2018-03-23 | 中国科学院电工研究所 | A kind of preparation method of X ray zone plate |
-
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- 2019-03-26 CN CN201910234877.XA patent/CN109903877B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3867637A (en) * | 1973-09-04 | 1975-02-18 | Raytheon Co | Extended monochromatic x-ray source |
| CN102168294A (en) * | 2011-05-19 | 2011-08-31 | 北京工业大学 | Method for improving tungsten-base gold-plating bond strength |
| CN102585330A (en) * | 2012-01-18 | 2012-07-18 | 厦门虹鹭钨钼工业有限公司 | Tungsten-polymer composite material and preparation method thereof |
| WO2013191743A1 (en) * | 2012-02-17 | 2013-12-27 | The Massachusetts Institute Of Technology | Surface modification of cladding material |
| CN103924202A (en) * | 2014-04-03 | 2014-07-16 | 西南交通大学 | Metal support surface modification method |
| CN107833649A (en) * | 2017-10-16 | 2018-03-23 | 中国科学院电工研究所 | A kind of preparation method of X ray zone plate |
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