CN115015995A - Method for preparing neutron sensitive film layer on inner wall of microchannel plate channel - Google Patents
Method for preparing neutron sensitive film layer on inner wall of microchannel plate channel Download PDFInfo
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- CN115015995A CN115015995A CN202210508937.4A CN202210508937A CN115015995A CN 115015995 A CN115015995 A CN 115015995A CN 202210508937 A CN202210508937 A CN 202210508937A CN 115015995 A CN115015995 A CN 115015995A
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052796 boron Inorganic materials 0.000 claims abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000376 reactant Substances 0.000 claims abstract description 8
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 65
- 239000010410 layer Substances 0.000 claims description 65
- 238000000151 deposition Methods 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 8
- 150000004820 halides Chemical class 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 6
- 239000011241 protective layer Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- -1 tris (dimethylamine) boron Chemical compound 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 239000007789 gas Substances 0.000 abstract description 13
- 239000007795 chemical reaction product Substances 0.000 abstract description 9
- 239000011521 glass Substances 0.000 abstract description 6
- 239000012433 hydrogen halide Substances 0.000 abstract description 5
- 229910000039 hydrogen halide Inorganic materials 0.000 abstract description 5
- 150000001412 amines Chemical class 0.000 abstract description 4
- 101710121996 Hexon protein p72 Proteins 0.000 description 4
- 101710125418 Major capsid protein Proteins 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052810 boron oxide Inorganic materials 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T3/00—Measuring neutron radiation
- G01T3/006—Measuring neutron radiation using self-powered detectors (for neutrons as well as for Y- or X-rays), e.g. using Compton-effect (Compton diodes) or photo-emission or a (n,B) nuclear reaction
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T7/00—Details of radiation-measuring instruments
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J43/00—Secondary-emission tubes; Electron-multiplier tubes
- H01J43/04—Electron multipliers
- H01J43/06—Electrode arrangements
- H01J43/18—Electrode arrangements using essentially more than one dynode
- H01J43/24—Dynodes having potential gradient along their surfaces
- H01J43/246—Microchannel plates [MCP]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/12—Manufacture of electrodes or electrode systems of photo-emissive cathodes; of secondary-emission electrodes
- H01J9/125—Manufacture of electrodes or electrode systems of photo-emissive cathodes; of secondary-emission electrodes of secondary emission electrodes
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Molecular Biology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Measurement Of Radiation (AREA)
Abstract
The invention provides a method for preparing a neutron sensitive film layer on the inner wall of a microchannel plate channel, which comprises the following steps: the organic boron precursor and the ozone or the oxygen plasma are used as two reactants to generate the organic boron/ozone/oxygen plasma through chemical reaction by adopting the atomic layer deposition technology 10 B 2 O 3 A film layer; the reaction products being deposited on the inner walls of the channels in addition to 10 B 2 O 3 Besides the film layer, amine and organic gases exist, and hydrogen halide gas harmful to the MCP substrate does not exist, so that the overall quality of the deposited film layer is high; by preparing the neutron sensitive film layer, the detection efficiency can reach a higher level than by uniformly doping the neutron sensitive film layer in the MCP substrate glass.
Description
Technical Field
The invention relates to the technical field of vacuum photoelectric detection, in particular to a method for preparing a neutron sensitive film layer on the inner wall of a microchannel plate channel.
Background
A Microchannel Plate (MCP) is a two-dimensional electron multiplier device with a compact structure, which has been successfully developed in the end of the 60 s of the 20 th century, can detect particles such as ions and electrons, and radiation such as X rays and UV light, has the advantages of high position resolution, high gain, low power consumption, self-saturation, high-speed detection, low noise and the like, and is applied to various detectors in various forms. Neutron sensitive nuclide is doped into the MCP in a certain mode, so that incident neutrons can be absorbed and nuclear reaction can occur, high-energy particles are generated to impact the inner wall of the channel to realize detection and multiplication of signals, imaging detection of neutrons is realized, and the MCP is a neutron detector core element with wide application prospect.
The methods for incorporating neutron-sensitive nuclides into MCPs are mainly divided into two main categories, one is to directly incorporate the neutron-sensitive nuclides into the glass material, such as 10 B、 155 Gd、 157 Gd, the other is prepared into a neutron sensitive film layer on the MCP in a film coating mode, and the prepared neutron sensitive film layer can be 155、157 Gd 2 O 3 、 10 B 2 O 3 、 10 BN, etc. of nuclides therein 155、157 The capture cross section of Gd is larger, the detection efficiency is higher, but the energy of reaction product particles is higher, and the position resolution can be influenced; while the nuclide 10 The neutron capture area of B is smaller, the detection efficiency is slightly lower, but the energy of nuclear reaction product particles is lower, which is beneficial to position resolution, and meanwhile, in the aspect of white light neutron resonance imaging application, 10 b has no obvious characteristic peak for the detection efficiency of neutrons with different energies, and Gd can not meet the requirement.
Preparation of neutron-sensitive films, especially of membranes containing 10 In the method for preparing neutron sensitive film layer of B nuclide, the adopted mode is atomic layer deposition technology, and the used boron precursors are all halides, such as BBr 3 、BCl 3 The reactant product, including the acidic gas HBr, has the following serious effects on the fabrication of boron-containing films on MCPs: (1) the microchannel plate substrate material contains alkali metal oxide and alkaline earth metal oxide, and reaction products HBr or HCl react with the surface of the MCP substrate to cause the problems of high noise and the like; (2) the chemical source has high danger, and the tail gas processor which has strong corrosion resistance and is used for processing the hydrogen halide gas is required, so that the application range is limited.
Disclosure of Invention
The invention aims to provide a method for preparing a neutron sensitive film layer on the inner wall of a microchannel plate channel, which adopts an atomic layer deposition technology, uses a non-halide organic boron source as a precursor, adopts ozone or oxygen plasma as an oxygen source, and generates two reactants through a chemical reaction 10 B 2 O 3 And a film layer, namely a neutron sensitive film layer.
Whereby reaction products are deposited on the inner walls of the channels in addition to 10 B 2 O 3 Besides the film layer, amine and organic gases exist, and hydrogen halide gas harmful to the MCP substrate is not contained, so that the overall quality of the deposited film layer is high; the boron atoms doped with the same amount are higher in detection efficiency in the form of a film layer than in the MCP substrate glass by uniformly doping.
Preferably, the length-to-diameter ratio of the MCP substrate is 30:1 to 80:1, the pore diameter is 5 μm to 12um,prepared 10 B 2 O 3 The thickness of the film layer is 100nm-1000 nm.
Preferably, the organic boron source employs tris (dimethylamine) boron.
Preferably, the process of chemical reaction comprises preparation of deposition conditions and deposition of a film layer, wherein:
the deposition condition preparation includes:
the MCP substrate is arranged in the tool clamp and placed in the reaction cavity, so that the MCP substrate is horizontally placed in the middle of the reaction cavity, and precursor gas can be favorably diffused into the channels from two ends;
vacuumizing until the vacuum degree is better than 3 mbar;
heating the reaction cavity to the reaction temperature of 100-200 ℃, and preserving the heat for 30min-3 h;
the film deposition comprises:
firstly, organic boron precursor is introduced: the boron source is a liquid source and is controlled by controlling a pulse valve, the pulse time is 0.5s-4s, and after the boron source is pulsed, nitrogen purging is continuously carried out for 30s-5min, so that a reaction product and an unreacted boron source are removed from the reaction cavity;
then, ozone or plasma is introduced: the time of passage was 0.2s-2s, followed by a nitrogen purge for 30s-5min, where: the mass concentration of the ozone is 10-15%; the power of the oxygen plasma generator is 20W-150W;
the two-step reactant introduction process of the film deposition is operated, the circulation is 2000 times and 20000 times, and the thickness of the prepared film is 100nm-1000 nm.
Preferably, in deposition 10 B 2 O 3 And depositing an alumina protective layer after the film layer.
It should be understood that all combinations of the foregoing concepts and additional concepts described in greater detail below can be considered as part of the inventive subject matter of this disclosure unless such concepts are mutually inconsistent. In addition, all combinations of claimed subject matter are considered a part of the presently disclosed subject matter.
The foregoing and other aspects, embodiments and features of the present teachings will be more fully understood from the following description taken in conjunction with the accompanying drawings. Additional aspects of the present invention, such as features and/or advantages of exemplary embodiments, will be apparent from the description which follows, or may be learned by practice of specific embodiments in accordance with the teachings of the present invention.
Drawings
The drawings are not intended to be drawn to scale. In the drawings, each identical or nearly identical component that is illustrated in various figures may be represented by a like numeral. For purposes of clarity, not every component may be labeled in every drawing. Embodiments of various aspects of the present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
fig. 1 is a schematic response diagram of a scheme for doping a neutron-sensitive species in a substrate glass.
Fig. 2 is a response diagram of the preparation of the neutron sensitive film layer MCP according to the exemplary embodiment of the invention.
Fig. 3 is a schematic structural diagram of preparation of a neutron-sensitive film layer MCP according to an exemplary embodiment of the present invention.
FIG. 4 is a schematic view of the positions of the constituents of MCP prepared by the exemplary embodiment of the present invention detected by SEM.
FIG. 5 is a schematic diagram of the components and amounts of MCP prepared by the exemplary embodiment of the present invention, which is detected by SEM, and corresponds to spectrum 12-spectrum 12 in FIG. 4.
Fig. 6 shows the results of testing the detection efficiency of MCPs prepared according to the present invention versus conventional MCPs at a neutron beam streamline station.
Description of the reference numerals:
1-a channel of an MCP substrate; 3-incident neutron signal; 4-MCP glass substrate doped with neutron-sensitive nuclides; 5-a neutron sensitive membrane layer; 6-MCP substrate without neutron-sensitive nuclides; 7-protective layer.
Detailed Description
In order to better understand the technical content of the present invention, specific embodiments are described below with reference to the accompanying drawings.
In this disclosure, aspects of the present invention are described with reference to the accompanying drawings, in which a number of illustrative embodiments are shown. Embodiments of the present disclosure are not necessarily intended to include all aspects of the invention. It should be appreciated that the various concepts and embodiments described above, as well as those described in greater detail below, may be implemented in any of numerous ways, as the disclosed concepts and embodiments are not limited to any one implementation. In addition, some aspects of the present disclosure may be used alone, or in any suitable combination with other aspects of the present disclosure.
The invention aims to provide a method for preparing a neutron sensitive film layer on the inner wall of an MCP channel, which adopts an atomic layer deposition technology, uses a non-halide organic boron source as a precursor, adopts ozone or oxygen plasma as an oxygen source, and generates two reactants through a chemical reaction 10 B 2 O 3 And the film layer is a neutron sensitive film layer. The reaction products being deposited on the inner walls of the channels in addition to 10 B 2 O 3 Besides, the film layer also comprises amine and organic gas, and no hydrogen halide gas harmful to the MCP substrate exists, so that the overall quality of the deposited film layer is high.
Preferably, the process of the chemical reaction comprises preparation of deposition conditions and deposition of a film layer, wherein:
the deposition condition preparation includes:
the MCP substrate is arranged in the tool clamp and placed in the reaction cavity, so that the MCP substrate is horizontally placed in the middle of the reaction cavity, and precursor gas can be favorably diffused into the channels from two ends;
vacuumizing until the vacuum degree is better than 3 mbar;
heating the reaction cavity to the reaction temperature of 100-200 ℃, and preserving the heat for 30min-3 h;
the film deposition comprises:
firstly, organic boron precursor is introduced: the boron source is a liquid source and is controlled by controlling a pulse valve, the pulse time is 0.5s-4s, and after the boron source is pulsed, nitrogen purging is continuously carried out for 30s-5min, so that a reaction product and an unreacted boron source are removed from the reaction cavity;
then, ozone or plasma is introduced: the time was 0.2s-2s, followed by a nitrogen purge of 30s-5min, where: the mass concentration of the ozone is 10-15%; the power of the oxygen plasma generator is 20W-150W;
the two-step reactant introduction process of the film deposition is operated, the circulation is 2000 times and 20000 times, and the thickness of the prepared film is 100nm-1000 nm.
Preferably, in the deposition 10 B 2 O 3 And depositing an alumina protective layer after the film layer. Thus, the prepared B can be avoided 2 O 3 The film layer is contacted with water vapor before preparing the functional film layer of the resistance layer and the emission layer and in the subsequent use process to maintain B 2 O 3 Stability of the film layer over long-term use.
According to an embodiment of the disclosure, there is also provided a neutron sensitive membrane microchannel plate, including: microchannel plate substrate prepared according to the method on the channel walls 10 B 2 O 3 A film layer; on the base of microchannel plates 10 B 2 O 3 A resistance layer and an emission layer prepared on the basis of the film layer; and metal electrode thin film layers prepared on two end faces of the substrate of the microchannel plate.
Wherein, as neutron sensitive film layer 10 B 2 O 3 The thickness of the film layer is 100-1000 nm.
In this embodiment, after depositing boron oxide and a protective film layer by MCP, a resistive layer and an emitting layer are prepared on the basis of the boron oxide and the protective film layer, and then an electrode film is prepared on an end surface, so as to prepare a neutron-sensitive MCP for performance testing on a neutron beam streamline station, and compare the performance testing result with an MCP prepared by doping a neutron-sensitive nuclide and a neutron-sensitive film MCP prepared by using a halide boron precursor source, as follows:
| serial number | Neutron MCP species | 0.1eV neutron detection efficiency | Dark count rate |
| 1 | 10B doped MCP | 20.5％ | 2.9s -1 · |
| 2 | Halide boron source ALD-MCP | 25.3％ | 8.7s -1 · |
| 3 | ALD-MCP of organoboron source | 25.8％ | 1.1s -1 ·cm -2 |
As can be seen from the above test results, and by comparing the detection efficiency results shown in FIG. 6, the present invention employs an atomic layer deposition technique, and uses an organoboron precursor and ozone or oxygen plasma as two reactants to generate the organoboron precursor and the ozone or oxygen plasma by chemical reaction 10 B 2 O 3 A film layer; the reaction products being deposited on the inner walls of the channels in addition to 10 B 2 O 3 Besides the film layer, the film layer contains amine and organic gas, and has no hydrogen halide gas harmful to the MCP substrate, so that the overall quality of the deposited film layer is higher, and the detection efficiency can reach a higher level by preparing the neutron sensitive film layer than by uniformly doping the neutron sensitive film layer in the MCP substrate glass.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.
Claims (8)
1. A method for preparing a neutron sensitive film layer on the inner wall of a micro-channel plate channel is characterized in that an atomic layer deposition technology is adopted, a non-halide organic boron source is used as a precursor, ozone or oxygen plasma is used as an oxygen source, and the oxygen source and the precursor are chemically reacted to generate the neutron sensitive film layer on the inner wall of the channel of an MCP substrate 10 B 2 O 3 And a film layer, namely a neutron sensitive film layer.
2. The method for preparing the neutron sensitive film layer on the inner wall of the microchannel plate channel as claimed in claim 1, wherein the length-diameter ratio of the MCP substrate is 30:1 to 80:1, the pore diameter is 5 μm to 12um, and the prepared MCP substrate has the advantages of high aspect ratio, high resolution, high sensitivity and good stability 10 B 2 O 3 The thickness of the film layer is 100nm-1000 nm.
3. The method of fabricating a neutron sensitive membrane layer within MCP channels of claim 1, wherein the organoboron source employs tris (dimethylamine) boron.
4. The method for preparing the neutron sensitive film layer on the inner wall of the microchannel plate channel as recited in any one of claims 1 to 3, wherein the chemical reaction process comprises preparation of deposition conditions and film layer deposition, wherein:
the deposition condition preparation includes:
the MCP substrate is arranged in a tool clamp and placed in a reaction cavity, so that the MCP substrate is horizontally placed in the middle of the reaction cavity;
vacuumizing to a preset vacuum degree;
heating the reaction cavity to the reaction temperature of 100-200 ℃, and keeping the temperature for 30min-3 h;
the film deposition comprises:
firstly, organic boron precursor is introduced: the boron source is a liquid source, is controlled by controlling a pulse valve, the pulse time is 0.5s-4s, and then nitrogen purging is continuously carried out for 30s-5 min;
then, ozone or plasma is introduced: the time of passage was 0.2s-2s, followed by a nitrogen purge for 30s-5min, where: the mass concentration of the ozone is 10-15%; the power of the oxygen plasma generator is 20W-150W;
the two-step reactant introduction process of the film deposition is operated, the circulation is 2000 times and 20000 times, and the thickness of the prepared film is 100nm-1000 nm.
5. The method for preparing the neutron sensitive film layer on the inner wall of the microchannel plate channel of claim 4, wherein the neutron sensitive film layer is deposited on the inner wall 10 B 2 O 3 And depositing an alumina protective layer after the film layer.
6. A neutron sensitive membrane layer prepared on the inner wall of MCP channel according to the method of any one of claims 1 to 5.
7. A neutron sensitive membrane microchannel plate, comprising:
microchannel plate substrate, the channel walls of which are prepared according to the method of any of the preceding claims 1 to 5 10 B 2 O 3 A film layer;
on the base of microchannel plates 10 B 2 O 3 A resistance layer and an emission layer prepared on the basis of the film layer; and
and the metal electrode thin film layers are prepared on two end faces of the substrate of the microchannel plate.
8. The neutron sensitive membrane microchannel plate of claim 7, wherein the neutron sensitive membrane microchannel plate 10 B 2 O 3 The thickness of the film layer is 100-1000 nm.
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Citations (8)
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| US20160355729A1 (en) * | 2013-08-05 | 2016-12-08 | Colorado School Of Mines | Boron compounds for use in scintillators and admixture to scintillators |
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| CN110467865A (en) * | 2018-05-09 | 2019-11-19 | 同方威视技术股份有限公司 | A kind of painting boron method |
| CN112725764A (en) * | 2020-12-18 | 2021-04-30 | 松山湖材料实验室 | Neutron absorption material and preparation method and application thereof |
| CN114203515A (en) * | 2021-12-14 | 2022-03-18 | 中国科学院高能物理研究所 | Neutron sensitive microchannel plate with high gamma suppression ratio and manufacturing method thereof |
| US20220140244A1 (en) * | 2020-11-05 | 2022-05-05 | Kabushiki Kaisha Toshiba | Radiation detector |
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2022
- 2022-05-10 CN CN202210508937.4A patent/CN115015995A/en active Pending
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