CN103995280A - Boron film cathode of neutron detector and preparing method thereof - Google Patents

Boron film cathode of neutron detector and preparing method thereof Download PDF

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Publication number
CN103995280A
CN103995280A CN201410197126.2A CN201410197126A CN103995280A CN 103995280 A CN103995280 A CN 103995280A CN 201410197126 A CN201410197126 A CN 201410197126A CN 103995280 A CN103995280 A CN 103995280A
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negative electrode
boron
neutron detector
neutron
boron film
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CN103995280B (en
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魏志勇
陈国云
朱立
方美华
张紫霞
雷胜杰
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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Abstract

The invention discloses a boron film cathode of a neutron detector and a preparing method of the boron film cathode of the neutron detector. The boron film cathode of the neutron detector is detector cathode with good electrical properties and neutron sensitive performance. Conductive metal Al matrix is adopted for the cathode, and the surface of the cathode is coated with a neutron sensitive film. The neutron sensitive film comprises, by mass, 100 parts of boron powder, 15 parts to 25 parts of substance (the molecular formula of the substance is described in the instruction), 7 parts to 12 parts of curing agents and 30 parts to 40 parts of organic solvent. The boron film cathode of the neutron detector is simple in preparation, low in cost, high in adhesive force and good in uniformity, and the obtained detector is high in detection efficiency.

Description

A kind of neutron detector boron film negative electrode and preparation method thereof
Technical field
The present invention relates to a kind of neutron detector boron film negative electrode and preparation method thereof.
Background technology
The detection of neutron with Detection Techniques in occupy special status, it is more much more difficult than charged particle or gamma-ray detection, is mainly interacted and is produced charged particle or γ photon is realized by it and atomic nucleus.Be coated with in recent years boron gas detector and compare and fill 3He or BF3 detector advantage shows especially, become gradually a kind of main neutron detection instrument.Quantitatively being coated with boron cathode technique is to make the most important thing that is coated with boron gas detector, is related to the selection of the definite and environment for use of detector performance parameters.
Start late because being coated with the development of boron detector, the report of relevant quantitatively painting boron cathode technique is very few both at home and abroad, and negative electrode boron film of the prior art exists poor adhesive force, lack of homogeneity, thereby affects the detection efficiency of detector.
Summary of the invention
The present invention newly provides a kind of neutron detector boron film negative electrode and preparation method thereof.
For solving the problems of the technologies described above, the invention of this reality adopts following technical scheme:
A kind of neutron detector boron film negative electrode, cathode surface is covered with neutron sensitive film, and the feed composition of neutron sensitive film comprises: 100 parts of boron powder, 15-25 part 7-12 part hardening agent and 30-40 part organic solvent, described umber is mass fraction.
Above-mentioned negative electrode is conductive cathode, preferably adopts conducting metal Al matrix, first pre-service before film, and above-mentioned neutron detector boron film negative electrode, for neutron detection, have the detector negative electrode of good electrical performance and the sensitive performance of neutron.
Applicant finds after deliberation: negative electrode, after the process such as polishing, cleaning, oven dry is processed, adopts above-mentioned raw materials component, is modulated, after coupling agent modulation, coating, cold treatment and drying course, can obtain uniform and stable boron film, and thickness is controlled by solvent; Boron is crossed boron layer at least cannot firmly be coated in region to be coated with, and boron too much can cause the in uneven thickness of boron film; Before being coated with boron, solution must be adjusted evenly, if there is graininess boron powder, easily makes the boron film being shaped produce protruding boron powder particles, and the place of projection may cause spike electric discharge phenomena add high voltage in detector test after; consumption too much can increase the loss of outgoing particle energy, reduces detection efficiency, and very few adhesion is inadequate.
The material component of above-mentioned neutron detector boron film negative electrode also comprises 3-5 part toughner, and described umber is mass fraction.Adhesion, the homogeneity that can further strengthen like this gained film ensure detection efficiency simultaneously.
The feed composition of above-mentioned neutron detector boron film negative electrode also comprises 6-8 part HO-[-CH 2-NH-CO-NH-CH 2-O] n-H, 1-2 part (COOH) 2 and 0.8-1 part C6H6O, described umber is mass fraction, the preferred 70-120 of said n.Can further strengthen like this adhesion, the homogeneity of gained film, improve the detection efficiency of detector simultaneously.
The raw material group feed composition of above-mentioned neutron detector boron film negative electrode also comprises 3-4 part with 0.5-0.8 part C 36h 70caO, wherein R1 is described umber is mass fraction.Can, in ensureing boron film homogeneity, adhesion, ensure the sensitivity of detector like this.
Above-mentioned middle n value is 1-3.
Boron powder needs chemical purity and two aspects of isotopic purity, and wherein chemical purity is better than more than 95%, and B10 abundance is not less than 90%.Can further ensure like this detection efficiency of detector.
Above-mentioned hardening agent is preferably the potpourri that polyetheramine hardening agent and phenolic aldehyde amine curing agent mass ratio are 1.1-1.3.Can further ensure like this adhesion and the drying efficiency of boron film.
Above-mentioned organic solvent is preferably tetrahydrofuran, dimethyl fumarate, dimethyl sulfoxide (DMSO) or acetone.
The thickness of above-mentioned boron film is preferably 2.5-3.5um, is 0.62-0.82mg/cm 2.Can make like this detection efficiency of detector reach optimum value.
The preparation method of above-mentioned neutron detector boron film negative electrode, comprises the following steps that order is joined:
A, cathode treatment: by negative electrode polishing, polishing, cleaning, oven dry;
B, the feed composition except boron powder is mixed, obtain coating fluid;
C, by negative electrode evenly after coating one deck coating fluid, evenly spray boron powder, and then last layer coating fluid;
D, by step C gained 92-96 DEG C insulation 2-2.5 hour, to obtain final product.
Applicant finds after deliberation: adopting said method with respect to methods such as submergence coatings, can significantly save the consumption of various resins, organic solvent etc., and gained boron film is even, detection efficiency is high, is not only cost-saving but also can improve the best approach of detection efficiency.
The neutron detector that comprises above-mentioned neutron detector boron film negative electrode, working gas is 90%Ar and 10%CH 4potpourri.
Above-mentioned gas ionization potential is low, and the drift velocity of electronics is large, and electronics adsorption effect is little, is convenient to improve the collection efficiency of electronics; And conveniently store, transport, do not impair one's health.
The NM technology of the present invention is prior art.
A kind of neutron detector boron film of the present invention negative electrode, prepares simple, with low costly, and adhesion is high, good uniformity, and the detection efficiency of gained detector is high.
Figure of description
Fig. 1 is the graph of a relation of ionization chamber detection efficiency and boron film linear thickness.
Fig. 2 is the schematic diagram of gained boron film on stainless steel substrates in embodiment 1.
Fig. 3 is the detection efficiency that embodiment 1 makes boron film negative electrode proportional counter by oneself.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
On stainless steel substrates, be coated with as follows boron film, following steps order is joined:
A, cathode treatment: by negative electrode polishing, polishing, cleaning, oven dry;
B, the feed composition except boron powder is mixed, obtain coating fluid;
C, by negative electrode evenly after coating one deck coating fluid, evenly spray boron powder, and then last layer coating fluid;
D, by step C gained 92-96 DEG C insulation 2-2.5 hour, to obtain final product.
The feed composition of neutron detector boron film negative electrode comprises: 100 parts of boron powder (the amorphous enrichment 10B boron powder (10B abundance 90%, B content 95%) of Dalian Boronten Sci & Tech Co., Ltd., 20 parts (mean value of n is 2.3), 10 parts of hardening agent (potpourri that polyetheramine hardening agent D400 and phenolic aldehyde amine curing agent TZ500 mass ratio are 1.2), 35 parts of organic solvents, 4 parts of toughner (QS-BE), 7 parts of part structural formulas are HO-[-CH 2-NH-CO-NH-CH 2-O] resin (powdery, n is 80-100, Zha Xi Jebb chemical industry), 1.5 parts (COOH) 2,0.9 parts of C6H6O, 3.5 parts of n-H with 0.6 part of C 36h 70caO, wherein R1 is described umber is mass fraction.
Organic solvent is dimethyl sulfoxide (DMSO); The thickness of boron film is 3um.
Said method gained boron film adhesion is high, good uniformity, and the detection efficiency of gained neutron detector is high, and the working gas of neutron detector is 90%Ar and 10%CH 4potpourri.
Use said method, made one by oneself and adhered to last layer B10 film at proportional counter counter inwall (proportional counter negative electrode), as thermal neutron sensitive layer.Meanwhile, the sensitive proportional counter of homemade painting boron thermal neutron is placed into standard 241in Am-Be neutron source, carry out experiment measuring.Under 800V high pressure, use respectively the cylindrical high density polyethylene that 7mm and 20mm are thick (HDPE winding pipe A type, Hangzhou Liantong Tube Co., Ltd.) sleeve pipe parcel proportional counter, in 1000 seconds, record two groups of neutron spectra of proportional counter; Remove again the neutron spectra that records naked proportional counter tube after high density polyethylene sleeve pipe under the same terms.Analyzing three groups of spectrums with multiple tracks software ums draws the area under spectrum of each spectrum, entirely composes counting, average energy and counting rate data and be listed in the table below 1.
The detection efficiency of self-control boron film negative electrode proportional counter corresponding standard A m-Be neutron source is 0.24%.The average neutron energy of Am-Be neutron source is 4MeV, is fast neutron source.Boron film negative electrode is thermal neutron (0.025eV) sensitivity.Calculate the detection efficiency of the self-control boron film negative electrode proportional counter that the different single-end neutron of acquisition are corresponding and see Fig. 3.
Neutron spectra parameter after table 1 polyethylene pipe parcel proportional counter tube
Measuring condition Area under spectrum (S) Full spectrum counting (C) Average energy (S/C) Counting rate (C/T)/cps
Naked proportional counter 6219 7394 0.841 7.39
The thick HDPE of parcel 7mm 5750 7635 0.753 7.64
The thick HDPE of parcel 20mm 6745 9283 0.727 9.28
Note: the data in form are except full spectrum counting and counting rate, and unit is relative unit.
Concerning neutron field, because the neutron energy of Am-Be neutron source transmitting is mostly up to MeV magnitude, originally just little with boron film action section in proportional counter, in proportional counter tube naked pipe situation, counting rate is just relatively low.Proportional counter outer wrapping high-density polyethylene layer is thicker, and the energy that neutron loses is therein just more, enters neutron energy in proportional counter just lower, and the probability being detected is also just higher, thereby counting rate is relatively high.And for γ field, the counting rate of γ photon is to present such trend.This is also just with experiment showed, that the signal that proportional counter is recorded to is the signal of neutron really.

Claims (10)

1. a neutron detector boron film negative electrode, is characterized in that: cathode surface is covered with neutron sensitive film, and the feed composition of neutron sensitive film comprises: 100 parts of boron powder, 15-25 part 7-12 part hardening agent and 30-40 part organic solvent, described umber is mass fraction.
2. neutron detector boron film negative electrode as claimed in claim 1, is characterized in that: feed composition also comprises 3-5 part toughner, described umber is mass fraction.
3. neutron detector boron film negative electrode as claimed in claim 1 or 2, is characterized in that: feed composition also comprises 6-8 part HO-[-CH 2-NH-CO-NH-CH 2-O] n-H, 1-2 part (COOH) 2with 8-1 part C 6h 6o, described umber is mass fraction.
4. neutron detector boron film negative electrode as claimed in claim 1 or 2, is characterized in that: feed composition also comprises 3-4 part with 0.5-0.8 part C 36h 70caO, wherein R1 is described umber is mass fraction.
5. neutron detector boron film negative electrode as claimed in claim 1 or 2, is characterized in that: middle n value is 1-3.
6. neutron detector boron film negative electrode as claimed in claim 1 or 2, is characterized in that: in boron powder, B10 abundance is not less than 90%.
7. neutron detector boron film negative electrode as claimed in claim 1 or 2, is characterized in that: hardening agent is the potpourri that polyetheramine hardening agent and phenolic aldehyde amine curing agent mass ratio are 1.1-1.3.
8. neutron detector boron film negative electrode as claimed in claim 1 or 2, is characterized in that: organic solvent is tetrahydrofuran, dimethyl fumarate, dimethyl sulfoxide (DMSO) or acetone; The thickness of boron film is 2.5-3.5um.
9. the preparation method of the neutron detector boron film negative electrode described in claim 1-8 any one, is characterized in that: comprise the following steps that order is joined:
A, cathode treatment: by negative electrode polishing, polishing, cleaning, oven dry;
B, the feed composition except boron powder is mixed, obtain coating fluid;
C, by negative electrode evenly after coating one deck coating fluid, evenly spray boron powder, and then last layer coating fluid;
D, by step C gained 92-96 DEG C insulation 2-2.5 hour, to obtain final product.
10. the neutron detector that comprises the neutron detector boron film negative electrode described in claim 1-8 any one, is characterized in that: working gas is 90%Ar and 10%CH 4potpourri.
CN201410197126.2A 2014-05-09 2014-05-09 A kind of neutron detector boron film negative electrode and preparation method thereof Expired - Fee Related CN103995280B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105137473A (en) * 2015-07-21 2015-12-09 时天成 Production method for boron-10 element used for neutron detector
CN106199681A (en) * 2016-06-24 2016-12-07 西北核技术研究所 A kind of nuclear reaction radiation conversion target and preparation method thereof and a kind of offset-type neutron detector
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
CN112859142A (en) * 2021-01-25 2021-05-28 核工业西南物理研究院 Preparation method of tube wall neutron sensitive layer and proportional counter tube

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CN103048677A (en) * 2011-09-09 2013-04-17 通用电气公司 Boron containing coating for neutron detection
EP2700980A1 (en) * 2011-04-18 2014-02-26 Nuctech Company Limited Neutron detector coated with boron and method for manufacture thereof
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EP2700980A1 (en) * 2011-04-18 2014-02-26 Nuctech Company Limited Neutron detector coated with boron and method for manufacture thereof
US20140103221A1 (en) * 2011-05-12 2014-04-17 Otnd Onet Technologies Nuclear Decommissioning Method of depositing boron on sheet metal for neutron detection apparatus or ionization chamber
CN103048677A (en) * 2011-09-09 2013-04-17 通用电气公司 Boron containing coating for neutron detection

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105137473A (en) * 2015-07-21 2015-12-09 时天成 Production method for boron-10 element used for neutron detector
CN106199681A (en) * 2016-06-24 2016-12-07 西北核技术研究所 A kind of nuclear reaction radiation conversion target and preparation method thereof and a kind of offset-type neutron detector
CN106199681B (en) * 2016-06-24 2018-11-02 西北核技术研究所 A kind of nuclear reaction radiation conversion target and preparation method thereof and a kind of offset-type neutron detector
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
US11090686B2 (en) 2018-05-09 2021-08-17 Nuctech Company Limited Method for coating boron
CN112859142A (en) * 2021-01-25 2021-05-28 核工业西南物理研究院 Preparation method of tube wall neutron sensitive layer and proportional counter tube
CN112859142B (en) * 2021-01-25 2023-01-24 核工业西南物理研究院 Preparation method of tube wall neutron sensitive layer and proportional counter tube

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