CN108342698A - It is a kind of6The preparation process of LiF target membranes - Google Patents
It is a kind of6The preparation process of LiF target membranes Download PDFInfo
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- CN108342698A CN108342698A CN201810120468.2A CN201810120468A CN108342698A CN 108342698 A CN108342698 A CN 108342698A CN 201810120468 A CN201810120468 A CN 201810120468A CN 108342698 A CN108342698 A CN 108342698A
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- lif
- graphite crucible
- preparation process
- tungsten filament
- bottom liner
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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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention belongs to isotope target preparing technical fields, disclose one kind6The preparation process of LiF target membranes.The technique be by6After LiF is prepared into reunion shape, it is deposited onto on bottom liner using electron bombardment equipment, what which prepared6LiF target membranes 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 preparing technical fields, and in particular to a kind of6The preparation process of LiF target membranes.
Background technology
6Li is the most light solid isotope of atomic weight, is the important materials and fuel of fusion reactor and thermonuclear device, can also
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 its being plated on bottom liner by certain technique, be made6LiF target membranes, 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 membranes, but there is the method film and bottom liner combination force difference, the easy peeling of film layer to fall off, when evaporation due to6It is coarse and form a large amount of macroscopic particles on surface that the splashing of LiF drops be easy to cause film surface.In order to obtain6LiF film theories
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, thickness evenness is good6The system of LiF target membranes
Standby technology.
Invention content
(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 membranes.
(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 membranes, the technique include the following steps：
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 that step (a) obtains progress Glow Discharge Cleaning in vacuum is put into inhale on bottom liner further to remove
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 includes mainly vacuum chamber, graphite crucible, stainless steel shielding cylinder, the first tungsten filament, second
Tungsten filament and power supply, wherein graphite crucible, stainless steel shielding cylinder, the first tungsten filament, the second tungsten filament are respectively positioned on internal vacuum chamber；Described
One tungsten filament disk is circle, is located above graphite crucible, which is less than the diameter and first tungsten filament 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 filament 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 is stretched to from stainless steel shielding cylinder bottom in stainless steel shielding cylinder, and the graphite crucible is for putting
It sets6LiF, there are one insulators for setting below, are equipped between the insulator and graphite crucible and are capable of providing high pressure and can adjust
The bottom of second tungsten filament of graphite crucible height, a diameter of 0.9~1.2mm of second tungsten filament, one end and graphite crucible connects
It connects, the other end passes through the high-pressure stage of insulator and power supply to connect；
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 i.e. may make vacuum to stablize, vacuum stablize after degasification terminate；
3) prepared by electron bombardment6LiF target membranes
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 is depending on required in the step6The thickness of LiF target membranes；
The parameter of wherein exchange 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, 25V increased per 10min, 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 the 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：Diameter 6~
9mm, thickness 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 materials upper end is 10~15cm.
(3) advantageous effect
Using provided by the invention6The preparation process of LiF target membranes, preparation6LiF target membranes and the binding force of bottom liner are good, are not easy
It falls off.Simultaneously because6LiF materials are not easy to buy, and can be saved material as far as possible using the method, improve the utilization of material
Rate.
Description of the drawings
Fig. 1 is the schematic diagram for the electron bombardment equipment that specific implementation mode experimental example 1 provides；Wherein 1 is vacuum chamber；2 are
Second tungsten filament；3 be the first tungsten filament；4 be stainless steel shielding cylinder；5 be graphite crucible；6 be boron carbide；7 be power supply.
Specific implementation mode
The present invention is further elaborated below in conjunction with specific experiment example and Figure of description.
It is prepared by method provided by the invention6The basic principle of LiF is：Alternating current is passed to the first tungsten filament, and is passed through
Second tungsten filament adds high pressure to crucible, and the first tungsten filament generates heat and a large amount of electronics for emitting are under electrostatic field, bombards on crucible, makes
Temperature rise, in crucible6LiF target materials, which are just evaporated, is deposited on base lining.
Experimental example 1
It is a kind of6The preparation process of LiF target membranes, the technique include the following steps：
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 that step (a) obtains progress Glow Discharge Cleaning in vacuum is put into inhale on bottom liner further to remove
Attached or contamination impurity, this step is more important, and it is hard to find miscellaneous that the naked eyes adsorbed on bottom liner can be removed 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, and thickness is 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, include mainly vacuum chamber 1, graphite crucible 5, no
Become rusty steel shielding cylinder 4, the first tungsten filament 3, the second tungsten filament 2 and power supply 7, wherein graphite crucible 5, stainless steel shielding cylinder 4, the first tungsten filament 3,
Second tungsten filament 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, so that electronics is all bombarded on graphite crucible 5 as far as possible, vacuum
Vacuum degree in room 1 is 10-4Pa.First tungsten filament, 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 filament height it is concordant with stainless steel shielding cylinder upper end；First tungsten filament 3 is exchanged with power supply 7
Pole connects.The graphite crucible 5 is stretched to from 4 bottom of stainless steel shielding cylinder in stainless steel shielding cylinder 4, which is used for
It places6LiF, there are one insulators for setting below, are equipped between the insulator and graphite crucible and are capable of providing high pressure and can adjust
Save the second tungsten filament of graphite crucible height, a diameter of 0.9~1.2mm of second tungsten filament, the bottom of one end and graphite crucible
Connection, the other end pass through the high-pressure stage of insulator and power supply to connect；
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 membranes
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 membranes；Bottom liner distance6The distance of LiF materials upper end be 10~
15cm。
It prepares6During LiF target membranes, the parameter for exchanging pole is that voltage is fixed as 12V, and electric current is 8~10A, high-pressure stage
Parameter be voltage is adjusted from 0, per 10min increase 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 membranes it is non-fusible at liquid in the case of 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.
It is that applicant is dexterously utilized in one insulator of graphite crucible following settings and non-conductor in this experimental example
The principle of electric field, the effect brought is 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 filament transmitting will be moved parallelly to high pressure direction from top to down
It is dynamic, and in this experimental example, below graphite crucible it is insulator, electric field is then focused on similar tapered form on graphite crucible,
Heat is more concentrated.Meanwhile second tungsten filament 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 is：Diameter 8mm, thickness 7mm.
The parameter when electron bombardment is set as：High pressure is adjusted from 0,25V is increased per 10min, 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 synthesis of the first tungsten filament of LiF distances is realized6The successful preparation of LiF, keeps away
Exempt from6The target membrane rough surface that LiF is molten into the fluid spills that liquid is brought and brings is uneven.
Experimental result：1. being prepared for a diameter of Ф 50mm on the Al substrates that thickness is 100 μm, thickness is 22 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, with wipings such as gauzes
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, as a result display surface is not almost any change, and surface is not fallen off, with hundred a ten thousandth microbalances to be heat-treated it is front and back into
Row is weighed, and as a result shows that quality is almost unchanged.
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 membranes, which is characterized in that the technique includes the following steps：
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 that step (a) obtains is 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 mainly vacuum chamber, graphite crucible, stainless steel shielding cylinder, the first tungsten filament, the second tungsten filament
And power supply, wherein graphite crucible, stainless steel shielding cylinder, the first tungsten filament, the second tungsten filament are respectively positioned on internal vacuum chamber；First tungsten
Wire tray is circle, is located above graphite crucible, which is less than the diameter and the first tungsten filament height of stainless steel shielding cylinder
It 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 alternating current respectively
And high voltage direct current, the first tungsten filament exchange pole connection with power supply；Voltage, electric current and the power parameter of the power supply high-pressure stage all may be used
To be continuously adjusted since 0；
The graphite crucible is stretched to from stainless steel shielding cylinder bottom in stainless steel shielding cylinder, and the graphite crucible is for placing6LiF,
There are one insulators for setting below, are equipped between the insulator and graphite crucible and are capable of providing high pressure and can adjust graphite crucible
The bottom connection of second tungsten filament of height, a diameter of 0.9~1.2mm of second tungsten filament, one end and 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 stablize, vacuum stablize after degasification terminate；
3) prepared by electron bombardment6LiF target membranes
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 is depending on required in the step6The thickness of LiF target membranes；
The parameter of wherein exchange 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, 25V increased per 10min, 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 membranes, which is characterized in that the aura described in step 1)
The main operating parameters of Discharge Cleaning include 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 membranes, 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 membranes, which is characterized in that vacuum chamber described in step 2)
Vacuum degree be better than 10-3Pa。
5. one kind according to claim 16The preparation process of LiF target membranes, 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 membranes, which is characterized in that shape of reuniting described in step (2)
's6LiF is cylindrical shape and cylinder dimensions are：6~9mm of diameter, thickness 5-8mm.
7. one kind according to claim 16The preparation process of LiF target membranes, which is characterized in that the bottom liner and quartz crystal
Film thickness monitor connects.
8. a kind of preparation process of 6LiF target membranes according to claim 1, which is characterized in that the bottom liner is apart from graphite earthenware
In crucible6The distance of LiF materials upper end is 10~15cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810120468.2A CN108342698B (en) | 2018-02-07 | 2018-02-07 | It is a kind of6The preparation process of LiF target membrane |
Publications (2)
| Publication Number | Publication Date |
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| CN108342698A true CN108342698A (en) | 2018-07-31 |
| CN108342698B CN108342698B (en) | 2019-10-15 |
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ID=62959104
Family Applications (1)
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20080074552A (en) * | 2007-02-09 | 2008-08-13 | (주)올레돈 | Manufacturing equipment using belt source for flexible oled and white oled |
| CN101540371A (en) * | 2009-04-15 | 2009-09-23 | 河北大学 | Flexible polymer solar battery of anode layer of metal grid and preparation method |
| CN106868480A (en) * | 2017-01-03 | 2017-06-20 | 中国原子能科学研究院 | It is a kind of6The preparation method of the compound target membranes of Li D |
-
2018
- 2018-02-07 CN CN201810120468.2A patent/CN108342698B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20080074552A (en) * | 2007-02-09 | 2008-08-13 | (주)올레돈 | Manufacturing equipment using belt source for flexible oled and white oled |
| CN101540371A (en) * | 2009-04-15 | 2009-09-23 | 河北大学 | Flexible polymer solar battery of anode layer of metal grid and preparation method |
| CN106868480A (en) * | 2017-01-03 | 2017-06-20 | 中国原子能科学研究院 | It is a kind of6The preparation method of the compound target membranes of Li D |
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| Publication number | Publication date |
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| CN108342698B (en) | 2019-10-15 |
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