CN108342698B - It is a kind of6The preparation process of LiF target membrane - Google Patents
It is a kind of6The preparation process of LiF target membrane Download PDFInfo
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- CN108342698B CN108342698B CN201810120468.2A CN201810120468A CN108342698B CN 108342698 B CN108342698 B CN 108342698B CN 201810120468 A CN201810120468 A CN 201810120468A CN 108342698 B CN108342698 B CN 108342698B
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- target membrane
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/04—Halides
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
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Abstract
The invention belongs to isotope target preparation technical fields, disclose one kind6The preparation process of LiF target membrane.The technique be by6After LiF is prepared into reunion shape, it is deposited on bottom liner using electron bombardment equipment, technique preparation6LiF target membrane and the binding force of bottom liner are good, not easily to fall off.This method can farthest save material simultaneously, improve the utilization rate of material.
Description
Technical field
The invention belongs to isotope target preparation technical fields, and in particular to a kind of6The preparation process of LiF target membrane.
Background technique
6Li is the most light solid isotope of atomic weight, is the important materials and fuel of fusion reactor and thermonuclear device, can also be with
Used as neutron measurement and neutron shielding material, wherein neutron is measured using the isotope and monitoring be with6LiF this
What one stable form carried out, to estimate the energy and power spectrum of neutron field.
In order to utilize6LiF measures neutron, needs for it to be plated on bottom liner by certain technique, be made6LiF target membrane, the thickness of the target membrane is usually all at 10 μm or more.Existing technology is banged using thermal evaporation and common big electron gun
Evaporation is hit to obtain6LiF target membrane, but the method has film and bottom liner binding force poor, the easy peeling of film layer falls off, when evaporation due to6The splashing of LiF drop be easy to cause film surface coarse and forms a large amount of macroscopic particles on surface.In order to obtain6LiF film theory
On can also use magnetically controlled sputter method, but since material is very expensive, need bulk6LiF as sputtering source, therefore
It is not applicable.Be badly in need of at present it is a kind of can reasonable control cost, with bottom liner binding force is good, the thickness uniformity is good6The system of LiF target membrane
Standby technology.
Summary of the invention
(1) goal of the invention
According to problem of the existing technology, the present invention provides a kind of good with bottom liner binding force, thickness uniformly, surface light
Cleanliness is good6The preparation process of LiF target membrane.
(2) technical solution
In order to solve the problems of prior art, technical solution provided by the invention is as follows:
It is a kind of6The preparation process of LiF target membrane, the technique the following steps are included:
1) pretreatment of bottom liner
The pretreatment includes two steps:
(a) cleaning of deoiling successively is carried out to bottom liner with alcohol, acetone；
(b) bottom liner for obtaining step (a) is put into progress Glow Discharge Cleaning in vacuum and is inhaled on bottom liner with further removing
Attached or contamination impurity；
The bottom liner is aluminium flake, stainless steel substrates or titanium sheet；
2) pre-treatment of raw material
It will be powdered6LiF raw material are prepared into reunion shape；Then by shape of reuniting6LiF is removed in a manner of electron bombardment
2~4h of gas；
The electron bombardment device therefor mainly includes vacuum chamber, graphite crucible, stainless steel shielding cylinder, the first tungsten wire, second
Tungsten wire and power supply, wherein graphite crucible, stainless steel shielding cylinder, the first tungsten wire, the second tungsten wire are respectively positioned on internal vacuum chamber；Described
One tungsten wire disk is circle, is located above graphite crucible, which is less than the diameter and first tungsten wire of stainless steel shielding cylinder
Height is concordant with stainless steel shielding cylinder upper end；The power supply is integrated power supply, including exchange pole and high-pressure stage, can provide friendship respectively
Galvanic electricity and high voltage direct current, the first tungsten wire exchange pole connection with power supply；Voltage, electric current and the power parameter of the power supply high-pressure stage
It can be continuously adjusted since 0；
The graphite crucible stretches in stainless steel shielding cylinder from stainless steel shielding cylinder bottom, and the graphite crucible is for putting
It sets6LiF is provided with an insulator below, is equipped between the insulator and graphite crucible and is capable of providing high pressure and is adjustable
Second tungsten wire of graphite crucible height, the diameter of second tungsten wire are 0.9~1.2mm, the bottom company of one end and graphite crucible
It connects, the other end passes through insulator and the high-pressure stage of power supply connects；
Reunion shape6LiF degasification operation need to only open capable AC pole switch, and electric current is set as 5~8A, and the time is 2~
4h may make vacuum to stablize, and degasification terminates after vacuum is stablized；
3) prepared by electron bombardment6LiF target membrane
After degasification6LiF continues to be deposited in a manner of electron bombardment in the electron bombardment equipment described in step 2)
On bottom liner, the time of electron bombardment depends on required in the step6The thickness of LiF target membrane；
The parameter for wherein exchanging pole is that voltage is fixed as 12V, and electric current is 8~10A；The parameter of high-pressure stage is that voltage is opened from 0
Begun to adjust, every 10min increases 25V, according to graphite crucible size and6The amount of LiF adjusts voltage to peak, and the peak is not with
So that6LiF is molten into liquid and is limited.
Preferably, the main operating parameters of Glow Discharge Cleaning described in step 1) include, and scavenging period is 3~
5min, vacuum degree are 1~10Pa, and voltage is 400~500V.
Preferably, insulator described in step 2) is discoid boron nitride.
Preferably, the vacuum degree of vacuum chamber described in step 2) is better than 10-3Pa。
Preferably, reunion shape described in step (2)6LiF is prepared by die pressing.
Preferably, reunion shape described in step (2)6LiF is cylindrical shape and cylinder dimensions are as follows: diameter 6~
9mm, with a thickness of 5-8mm.
Preferably, the bottom liner is connect with quartz crystal film thickness monitor.
Preferably, the bottom liner is in graphite crucible6The distance of LiF material upper end is 10~15cm.
(3) beneficial effect
Using provided by the invention6The preparation process of LiF target membrane, preparation6LiF target membrane and the binding force of bottom liner are good, are not easy
It falls off.Simultaneously because6LiF material is not easy to buy, and can be saved material as far as possible using the method, improve the utilization of material
Rate.
Detailed description of the invention
Fig. 1 is the schematic diagram for the electron bombardment equipment that specific embodiment experimental example 1 provides；Wherein 1 is vacuum chamber；2 are
Second tungsten wire；3 be the first tungsten wire；4 be stainless steel shielding cylinder；5 be graphite crucible；6 be boron carbide；7 be power supply.
Specific embodiment
The present invention is further elaborated below in conjunction with specific experiment example and Figure of description.
Method preparation provided by the invention6The basic principle of LiF is: passing to alternating current to the first tungsten wire, and passes through
Second tungsten wire adds high pressure to crucible, and the first tungsten wire generates heat and a large amount of electronics for emitting are under electrostatic field, bombards on crucible, makes
Temperature rise, in crucible6LiF target material, which is just evaporated, is deposited on base lining.
Experimental example 1
It is a kind of6The preparation process of LiF target membrane, the technique the following steps are included:
1) pretreatment of bottom liner
The pretreatment includes two steps:
(a) cleaning of deoiling successively carried out to bottom liner with alcohol, acetone, removes the grease stain on bottom liner and dirty；
(b) bottom liner for obtaining step (a) is put into progress Glow Discharge Cleaning in vacuum and is inhaled on bottom liner with further removing
Attached or contamination impurity, this step is more important, and it is indetectable miscellaneous to can remove the naked eyes adsorbed on bottom liner by this step
Matter, to ensure6LiF and the more firm combination of bottom liner；The operation major parameter of Glow Discharge Cleaning be scavenging period be 3~
5min, vacuum degree are 1~10Pa, and voltage is 400~500V.
The bottom liner is aluminium flake, with a thickness of 100 μm.
2) pre-treatment of raw material
It will be powdered6LiF raw material are prepared into reunion shape；Then by shape of reuniting6LiF passes through electronics in high vacuum
2~4h of mode degasification of bombardment；The electron bombardment device therefor is as shown in Figure 1, mainly include vacuum chamber 1, graphite crucible 5, no
Become rusty steel shielding cylinder 4, the first tungsten wire 3, the second tungsten wire 2 and power supply 7, wherein graphite crucible 5, stainless steel shielding cylinder 4, the first tungsten wire 3,
Second tungsten wire 2 is respectively positioned on internal vacuum chamber；The power supply 7 is integrated power supply, including exchange pole and high-pressure stage, can provide friendship respectively
Galvanic electricity and high voltage direct current, it is critical that the voltage of its high-pressure stage, electric current and power parameter can be continuously adjusted since 0；
The effect that stainless steel shielding cylinder 4 is arranged is can to reduce electrical losses, bombards electronics all on graphite crucible 5, vacuum
Vacuum degree in room 1 is 10-4Pa.First tungsten wire, 3 disk is circle, is located above graphite crucible, and round diameter is slightly less than not
Become rusty steel shielding cylinder diameter and the first tungsten wire height it is concordant with stainless steel shielding cylinder upper end；First tungsten wire 3 is exchanged with power supply 7
Pole connection.The graphite crucible 5 stretches in stainless steel shielding cylinder 4 from 4 bottom of stainless steel shielding cylinder, which is used for
It places6LiF is provided with an insulator below, is equipped between the insulator and graphite crucible and is capable of providing high pressure and can adjust
The second tungsten wire of graphite crucible height is saved, the diameter of second tungsten wire is 0.9~1.2mm, the bottom of one end and graphite crucible
Connection, the other end pass through insulator and the high-pressure stage of power supply connects；
Reunion shape6LiF degasification need to only open capable AC pole switch, and electric current is set as 5~8A, and the time is that 2~4h is
Vacuum may make to stablize, degasification terminates；
Deaeration step is remarkably improved target membrane purity and vacuum degree is made to keep stablizing as much as possible, and this is mainly due to powder
Shape material inevitably adsorbs moisture, air and other impurities in air, therefore is first removed before electron bombardment
Otherwise gas can be such that the vacuum regulated steeply rises and can bring the impurity such as O, H, N to target membrane.
3) prepared by electron bombardment6LiF target membrane
Step 2) is obtained6It is deposited on bottom liner in a manner of electron bombardment in LiF merging electron bombardment equipment, the step
The time of electron bombardment depends on required in rapid6The thickness of LiF target membrane；Bottom liner distance6The distance of LiF material upper end be 10~
15cm。
Preparation6During LiF target membrane, the parameter for exchanging pole is that voltage is fixed as 12V, and electric current is 8~10A, high-pressure stage
Parameter is that voltage is adjusted from 0, and every 10min increases 25V, according to graphite crucible size with6The amount of LiF adjusts voltage to highest
Value, the peak is not to make6LiF is molten into liquid and is limited.
6LiF target membrane it is non-fusible at liquid in the case where be deposited on bottom liner, avoid liquid6It is a large amount of caused by LiF
Fluid spills, and ultimately form coarse non-uniform target membrane.
In this experimental example, in one insulator of graphite crucible following settings and non-conductor, be that applicant is dexterously utilized
The principle of electric field, bring act on clearly.Because graphite crucible is connect with high pressure, if below high pressure being conductor, that
The current potential of conductor is identical as graphite crucible, and the electronics of the first tungsten wire transmitting will be moved to high pressure direction in parallel from top to down
It is dynamic, and in this experimental example, below graphite crucible it is insulator, electric field is then focused on graphite crucible with similar tapered form,
Heat is more concentrated.Meanwhile second tungsten wire be relatively large in diameter, can effectively support graphite crucible.
The reunion shape6LiF is prepared by die pressing.The reunion shape6LiF is cylindrical shape and cylinder
Body size are as follows: diameter 8mm, with a thickness of 7mm.
The parameter setting when electron bombardment are as follows: high pressure is adjusted from 0, and every 10min increases 25V, according to graphite earthenware
Crucible size and6The amount of LiF adjusts voltage to peak, and the peak is not to make6LiF is molten into liquid and is limited, this experimental example
In, high pressure 300V.In addition, can also pass through adjusting6The distance of the first tungsten wire of LiF distance is comprehensive to be realized6The successful preparation of LiF, keeps away
Exempt from6LiF is molten into liquid bring fluid spills and bring target membrane rough surface is uneven.
Experimental result: it is Ф 50mm, with a thickness of 22 μm that diameter is 1. prepared on the Al substrate with a thickness of 100 μm6LiF target membrane, the target membrane any surface finish are not fallen off, and binding force is good.
2. being placed 6 months under atmospheric environment, almost it is not any change, surface is not fallen off, and is not relaxed, and is wiped with gauze etc.
After tool wiping, target membrane surface is unchanged；
3. 5 × 10-4Sample is heated in the vacuum of Pa, heating temperature is 300 DEG C, and the heating and thermal insulation time is equal
For 6h, surface is not almost any change as the result is shown, and surface is not fallen off, with hundred a ten thousandth microbalances to heat treatment front and back into
Row weighing, quality is almost unchanged as the result is shown.
Experimental example 2
Unlike experimental example 1, the bottom liner is connect with quartz crystal film thickness monitor, can monitor target membrane thickness on-line
Degree；The bottom liner is stainless steel substrates.
Claims (8)
1. a kind of6The preparation process of LiF target membrane, which is characterized in that the technique the following steps are included:
1) pretreatment of bottom liner
The pretreatment includes two steps:
(a) cleaning of deoiling successively is carried out to bottom liner with alcohol, acetone；
(b) bottom liner for obtaining step (a) be put into vacuum carry out Glow Discharge Cleaning with further remove on bottom liner absorption or
The impurity of contamination；
The bottom liner is aluminium flake, stainless steel substrates or titanium sheet；
2) pre-treatment of raw material
It will be powdered6LiF raw material are prepared into reunion shape；Then by shape of reuniting6Degasification 2 in a manner of electron bombardment LiF
~4h；
The electron bombardment device therefor includes vacuum chamber, graphite crucible, stainless steel shielding cylinder, the first tungsten wire, the second tungsten wire and electricity
Source, wherein graphite crucible, stainless steel shielding cylinder, the first tungsten wire, the second tungsten wire are respectively positioned on internal vacuum chamber；The first tungsten wire disk
For circle, be located above graphite crucible, the round diameter be less than the diameter of stainless steel shielding cylinder and the first tungsten wire height with not
Rust steel shielding cylinder upper end is concordant；The power supply is integrated power supply, including exchange pole and high-pressure stage, can provide alternating current and height respectively
Straightening galvanic electricity, the first tungsten wire exchange pole connection with power supply；Voltage, electric current and the power parameter of the power supply high-pressure stage can be from
0 starts to be continuously adjusted；
The graphite crucible stretches in stainless steel shielding cylinder from stainless steel shielding cylinder bottom, and the graphite crucible is for placing6LiF,
It is provided with an insulator below, is equipped between the insulator and graphite crucible and is capable of providing high pressure and is adjustable graphite crucible
Second tungsten wire of height, the diameter of second tungsten wire are 0.9~1.2mm, one end and the bottom connection of graphite crucible, the other end
It is connected across the high-pressure stage of insulator and power supply；
Reunion shape6LiF degasification operation need to only open capable AC pole switch, and electric current is set as 5~8A, and the time is 2~4h
So that vacuum is stablized, degasification terminates after vacuum is stablized；
3) prepared by electron bombardment6LiF target membrane
After degasification6LiF continues to be deposited on bottom liner in a manner of electron bombardment in the electron bombardment equipment described in step 2)
On, the time of electron bombardment depends on required in the step6The thickness of LiF target membrane；
The parameter for wherein exchanging pole is that voltage is fixed as 12V, and electric current is 8~10A；The parameter of high-pressure stage is voltage from 0
Adjust, every 10min increases 25V, according to graphite crucible size and6The amount of LiF adjusts voltage to peak, and the peak is not to make6LiF is molten into liquid and is limited.
2. one kind according to claim 16The preparation process of LiF target membrane, which is characterized in that aura described in step 1)
The operating parameter of Discharge Cleaning includes that scavenging period is 3~5min, and vacuum degree is 1~10Pa, and voltage is 400~500V.
3. one kind according to claim 16The preparation process of LiF target membrane, which is characterized in that insulator described in step 2)
For discoid boron nitride.
4. one kind according to claim 16The preparation process of LiF target membrane, which is characterized in that vacuum chamber described in step 2)
Vacuum degree be higher than 10-3Pa。
5. one kind according to claim 16The preparation process of LiF target membrane, which is characterized in that shape of reuniting described in step (2)
's6LiF is prepared by die pressing.
6. one kind according to claim 16The preparation process of LiF target membrane, which is characterized in that shape of reuniting described in step (2)
's6LiF is cylindrical shape and cylinder dimensions are as follows: 6~9mm of diameter, with a thickness of 5-8mm.
7. one kind according to claim 16The preparation process of LiF target membrane, which is characterized in that the bottom liner and quartz crystal
Film thickness monitor connection.
8. a kind of preparation process of 6LiF target membrane according to claim 1, which is characterized in that the bottom liner is apart from graphite earthenware
In crucible6The distance of LiF material upper end is 10~15cm.
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| CN201810120468.2A CN108342698B (en) | 2018-02-07 | 2018-02-07 | It is a kind of6The preparation process of LiF target membrane |
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| CN201810120468.2A CN108342698B (en) | 2018-02-07 | 2018-02-07 | It is a kind of6The preparation process of LiF target membrane |
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