CN106868480B - A kind of preparation method of the compound target membrane of 6Li-D - Google Patents

A kind of preparation method of the compound target membrane of 6Li-D Download PDF

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Publication number
CN106868480B
CN106868480B CN201710001095.2A CN201710001095A CN106868480B CN 106868480 B CN106868480 B CN 106868480B CN 201710001095 A CN201710001095 A CN 201710001095A CN 106868480 B CN106868480 B CN 106868480B
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China
Prior art keywords
target membrane
compound target
quartz glass
preparation
glass ware
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CN106868480A (en
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樊启文
胡跃明
张榕
王�华
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C20/00Chemical coating by decomposition of either solid compounds or suspensions of the coating forming compounds, without leaving reaction products of surface material in the coating
    • C23C20/06Coating with inorganic material, other than metallic material
    • C23C20/08Coating with inorganic material, other than metallic material with compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/04Hydrides of alkali metals, alkaline earth metals, beryllium or magnesium; Addition complexes thereof

Abstract

The invention belongs to target piece preparation technical fields, disclose one kind6The preparation method of the compound target membrane of Li-D.This approach includes the following steps:(1) will6LiF and (CD2)nTwo kinds of dusty materials with6The atomic ratio of Li and D is 1:3~1:5 ratio uniform mixing;(2) diformazan benzo is added into said mixture and stirs to get uniformly gluey suspension under heating;(3) suspension is poured into the quartz glass ware leveled;(4) be buckled to above quartz glass ware one can thermal conductive container, to this can thermal conductive container to be heated uniformly to the temperature of the gluey suspension be 90~120 DEG C.(5) it after being heated to dimethylbenzene volatilization, is formed uniform6The compound target membrane of Li-D removes it from quartz glass ware bottom;(6) step (5) is obtained6The compound target membrane of Li-D is put into stainless steel intermediate plate, obtains required thickness by cold rolling mill6The compound target membrane of Li-D.It is 0.5~6mg/cm that mass thickness, which can be prepared, using this method2Compound target membrane and thickness is uniform, stability is good.

Description

It is a kind of6The preparation method of the compound target membrane of Li-D
Technical field
The invention belongs to target piece preparation technical fields, and in particular to a kind of6The preparation method of the compound target membrane of Li-D.
Background technique
Lithium hydride class material (LiH, LiD, LiDT etc.) has the peculiar properties such as low-density, low atomic number, can be used as low The scattering of energy X-ray and conveying material, lightweight neutron moderator etc. have important in the fields such as astronomy research and nuclear effect test Research and application value.Especially lithium deuteride, it is the main stuffing of hydrogen bomb and the primary raw material of nuclear fusion, product It can be used as the supplement of tritium particle in hot spot, to make up deuterium tritium raito (T.R) example mismatch caused by a small amount of loss of tritium decay.Deuterate at present The preparation of lithium is usually to utilize sintering process, but the lithium deuteride thickness of sintering process preparation is larger, and it is real not to be able to satisfy some nuclear physics The demand tested.
Summary of the invention
(1) goal of the invention
According to the problems of prior art, the present invention provides a kind of preparation process is simple, quality is thick
Degree is 0.5~6mg/cm2's6The preparation method of the compound target membrane of Li-D.
(2) technical solution
It is a kind of6The preparation method of the compound target membrane of Li-D, this approach includes the following steps:
(1) will6LiF and (CD2)nTwo kinds of dusty materials with6The atomic ratio of Li and D is 1:3~1:5 ratio uniform mixing; Wherein6The partial size of LiF is 5~10 μm, (CD2)nPartial size be 50~100 μm;
(2) solvent xylene is added into mixture obtained in step (1) and stirs to get uniform glue under heating Suspension;Wherein the volume mass of dimethylbenzene and mixture ratio is 1ml:4mg~1ml:12mg;
(3) the uniform gluey suspension for obtaining step (2) pours into the quartz glass ware that bottom surface is plane;The quartz Glassware is placed on the platform calibrated with level meter;
(4) above the quartz glass ware described in step (3) be buckled to one can thermal conductive container, to this can thermal conductive container it is equal The even temperature for being heated to the gluey suspension is 90~120 DEG C, so that (CD2)nIt is sufficiently poly- in the saturation atmosphere of dimethylbenzene It closes, simultaneously6LiF equably penetrates into (CD2)nIn;There are an outside flow-guiding mouths on the back-off container, so that dimethylbenzene is waved Hair overflows.
(5) it after being heated to dimethylbenzene volatilization, is formed uniformly in quartz glass ware bottom surface6Li-D is compound Target membrane, will6The compound target membrane of Li-D is removed from quartz glass ware bottom;
(6) step (5) is obtained6The compound target membrane of Li-D is put into stainless steel intermediate plate, obtains institute by cold rolling mill Need thickness6The compound target membrane of Li-D.
(CD described in step (1)2) n be deuterated polyethylene;
Preferably, the mode of stirring described in step (2) is magnetic agitation, and it is slightly boiled to be heated to solution.
Preferably, removing described in step (5) is to utilize sharp cutter will from quartz glass ware bottom surrounding6Li-D is multiple It closes target membrane to cut, then take out.
Preferably, described in step (4) can thermal conductive container be glass container.
Preferably, heating method described in step (4) is uniformly to be toasted using infrared lamp.
(3) beneficial effect
It is provided by the invention6The preparation method of the compound target membrane of Li-D, this method are to use6LiF and (CD2)nTwo kinds of powder materials Material and xylene solvent prepare compound target membrane, and this method is at home and abroad not reported in open source literature.It can using this method Preparing mass thickness is 0.5~6mg/cm2Compound target membrane and thickness is uniform, stability is good.Wherein, in order to guarantee the flat of target membrane Whole property, the present invention are placed in uniform gluey suspension in the quartz container that special bottom surface is plane, and the quartz Glass container is placed on the platform leveled.Meanwhile uniformly for homogeneous heating and film forming, the application is not directly in suspension Bottom-heated but heated on the thermal conductive container of back-off, also on the thermal conductive container be provided with one convenient for dimethylbenzene volatilization Flow-guiding mouth.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment 1
It is a kind of6The preparation method of the compound target membrane of Li-D, this approach includes the following steps:
(1) will6LiF and (CD2)nTwo kinds of dusty materials with6The atomic ratio of Li and D is 1:4 ratio uniform mixing;Wherein6The partial size of LiF is 5~10 μm, (CD2)nPartial size be 50~100 μm;
(2) solvent xylene is added into mixture obtained in step (1) and magnetic agitation obtains uniformly under heating Gluey suspension;Wherein the volume mass of dimethylbenzene and mixture ratio is 1ml:12mg, agitating mode are magnetic agitation, are heated to Solution is slightly boiled.
(3) the uniform gluey suspension for obtaining step (2) pours into the quartz glass ware that bottom surface is plane;The quartz Glassware is placed on the platform calibrated with level meter;
(4) glass container is buckled to above the quartz glass ware described in step (3), it is equably right using infrared lamp The temperature that the glass container is heated to the gluey suspension is 100 DEG C, so that (CD2)nIn the saturation atmosphere of dimethylbenzene sufficiently Polymerization, simultaneously6LiF equably penetrates into (CD2)nIn;There are an outside flow-guiding mouths on the glass, so as to dimethylbenzene volatilization It overflows.
(5) it after being heated to dimethylbenzene volatilization, is formed uniformly in quartz glass ware bottom surface6Li-D is compound Target membrane, will from quartz glass ware bottom surrounding using sharp cutter6Li-D composition target film stripping, then takes out.
(6) step (5) is obtained6The compound target membrane of Li-D is put into stainless steel intermediate plate, obtains institute by cold rolling mill Need thickness6The compound target membrane of Li-D.
(CD described in step (1)2) n be deuterated polyethylene;
Embodiment 2
Unlike the first embodiment, in step (1)6The atomic ratio of Li and D is 1:3, dimethylbenzene and mixing in step (2) The volume mass ratio of object is 1ml:4mg, the temperature that the gluey suspension is heated in step (4) is 90 DEG C.
Embodiment 3
Unlike the first embodiment, in step (1)6The atomic ratio of Li and D is 1:5, dimethylbenzene and mixing in step (2) The volume mass ratio of object is 1ml:8mg, the temperature that the gluey suspension is heated in step (4) is 120 DEG C.

Claims (5)

1. a kind of6The preparation method of the compound target membrane of Li-D, which is characterized in that this approach includes the following steps:
(1) will6LiF and (CD2) two kinds of dusty materials of n with6The atomic ratio of Li and D is 1:3~1:5 ratio uniform mixing;Wherein6The partial size of LiF is 5~10 μm, (CD2) n partial size be 50~100 μm;
(2) solvent xylene is added into mixture obtained in step (1) and stirs to get under heating uniformly gluey suspended Liquid;Wherein the volume mass of dimethylbenzene and mixture ratio is 1ml:4mg~1ml:12mg;
(3) the uniform gluey suspension for obtaining step (2) pours into the quartz glass ware that bottom surface is plane;The quartz glass Vessel are placed on the platform calibrated with level meter;
(4) above the quartz glass ware described in step (3) be buckled to one can thermal conductive container, to this can thermal conductive container uniformly add The temperature of heat to the gluey suspension is 90~120 DEG C, so that (CD2)nSufficiently it polymerize in the saturation atmosphere of dimethylbenzene, together When6LiF equably penetrates into (CD2)nIn;There are an outside flow-guiding mouths on the back-off container, so that dimethylbenzene volatilization is overflow Out;
(5) it after being heated to dimethylbenzene volatilization, is formed uniformly in quartz glass ware bottom surface6The compound target membrane of Li-D, It will6The compound target membrane of Li-D is removed from quartz glass ware bottom;
(6) step (5) is obtained6The compound target membrane of Li-D is put into stainless steel intermediate plate, obtains required thickness by cold rolling mill 's6The compound target membrane of Li-D;
(CD described in step (1)2) n be deuterated polyethylene.
2. one kind according to claim 16The preparation method of the compound target membrane of Li-D, which is characterized in that described in step (2) The mode of stirring is magnetic agitation, and it is slightly boiled to be heated to solution.
3. one kind according to claim 16The preparation method of the compound target membrane of Li-D, which is characterized in that described in step (5) Removing is to utilize sharp cutter will from quartz glass ware bottom surrounding6The compound target membrane of Li-D is cut, and is then taken out.
4. one kind according to claim 16The preparation method of the compound target membrane of Li-D, which is characterized in that described in step (4) Can thermal conductive container be glass container.
5. one kind according to claim 16The preparation method of the compound target membrane of Li-D, which is characterized in that described in step (4) The mode of heating is uniformly to be toasted using infrared lamp.
CN201710001095.2A 2017-01-03 2017-01-03 A kind of preparation method of the compound target membrane of 6Li-D Active CN106868480B (en)

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Publication number Priority date Publication date Assignee Title
CN108342698B (en) * 2018-02-07 2019-10-15 中国原子能科学研究院 It is a kind of6The preparation process of LiF target membrane
CN112030118A (en) * 2020-07-31 2020-12-04 中国原子能科学研究院 Preparation method of deuterated polyethylene nanowire array target

Citations (4)

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CN104176749A (en) * 2014-07-02 2014-12-03 北京理工大学 Method for preparing lithium deuteride by using high-temperature direct manner
CN104241614A (en) * 2013-06-19 2014-12-24 量子世界公司 Protective coatings for conversion material cathodes
CN104602438A (en) * 2014-12-29 2015-05-06 中国原子能科学研究院 Preparation method of tritium impregnated target slice
CN205793592U (en) * 2016-05-24 2016-12-07 西安冠能中子探测技术有限公司 The drive-in target manufactured for neutron tube

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Publication number Priority date Publication date Assignee Title
US20160164135A1 (en) * 2014-12-05 2016-06-09 Quantumscape Corporation Nanocomposite particles of conversion chemistry and mixed electronic ionic conductor materials

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN104241614A (en) * 2013-06-19 2014-12-24 量子世界公司 Protective coatings for conversion material cathodes
CN104176749A (en) * 2014-07-02 2014-12-03 北京理工大学 Method for preparing lithium deuteride by using high-temperature direct manner
CN104602438A (en) * 2014-12-29 2015-05-06 中国原子能科学研究院 Preparation method of tritium impregnated target slice
CN205793592U (en) * 2016-05-24 2016-12-07 西安冠能中子探测技术有限公司 The drive-in target manufactured for neutron tube

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