CN109680261A - Microchannel plate and microchannel plate inner wall preparation Cu adulterate Al2O3The method of high resistance film - Google Patents
Microchannel plate and microchannel plate inner wall preparation Cu adulterate Al2O3The method of high resistance film Download PDFInfo
- Publication number
- CN109680261A CN109680261A CN201910068958.7A CN201910068958A CN109680261A CN 109680261 A CN109680261 A CN 109680261A CN 201910068958 A CN201910068958 A CN 201910068958A CN 109680261 A CN109680261 A CN 109680261A
- Authority
- CN
- China
- Prior art keywords
- microchannel plate
- film
- high resistance
- settling chamber
- resistance film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000151 deposition Methods 0.000 claims abstract description 63
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 40
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 40
- 230000008021 deposition Effects 0.000 claims abstract description 36
- NFFYXVOHHLQALV-UHFFFAOYSA-N copper(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Cu].[Cu] NFFYXVOHHLQALV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000010926 purge Methods 0.000 claims description 18
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 16
- 239000010410 layer Substances 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 12
- IPSRAFUHLHIWAR-UHFFFAOYSA-N zinc;ethane Chemical compound [Zn+2].[CH2-]C.[CH2-]C IPSRAFUHLHIWAR-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 10
- 238000007664 blowing Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000005137 deposition process Methods 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000006227 byproduct Substances 0.000 claims description 6
- 239000002356 single layer Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000003475 lamination Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000001839 systemic circulation Effects 0.000 abstract description 12
- 238000000137 annealing Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 67
- 239000010408 film Substances 0.000 description 58
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 13
- 229910001868 water Inorganic materials 0.000 description 12
- 239000007788 liquid Substances 0.000 description 6
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 230000004087 circulation Effects 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002346 layers by function Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 230000005355 Hall effect Effects 0.000 description 1
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 1
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- -1 propoxyl Chemical group 0.000 description 1
- 238000009790 rate-determining step (RDS) Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45529—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making a layer stack of alternating different compositions or gradient compositions
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
-
- 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]
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Al is adulterated the present invention relates to a kind of microchannel plate and in microchannel plate inner wall preparation Cu2O3The method of high resistance film, microchannel plate inner wall prepare Cu and adulterate Al2O3High resistance film, high resistance film are to carry out different component material deposition in microchannel plate inner wall by Atomic layer deposition method to adulterate Al to obtain Cu2O3High resistance film, when deposition, in the systemic circulation, pass through control Al2O3Frequency of depositing and Cu frequency of depositing, to control Cu doping ratio, so as to 106‑1010The resistivity of accuracy controlling film within the scope of Ω cm；Cycle-index by controlling systemic circulation controls the thickness of film.Under high-temperature work environment or after high annealing, resistivity is held essentially constant prepared film, solves the existing microchannel plate surface film technical problem that change in resistance causes greatly microchannel plate performance unstable under the high temperature conditions.
Description
Technical field
The invention belongs to film doping correlative technology fields, are related to a kind of preparation method of photoelectric material high resistance film, tool
Body is related to a kind of in microchannel plate inner wall preparation Cu doping Al2O3The method of high resistance film.
Background technique
For traditional lead silicate glass microchannel plate after complicated preparation process processing, inner wall surface roughness is high,
The problems such as will lead to gain reduction, noise increase, limits the further promotion of its performance.By thin film preparation process micro- logical
Guidance tape inner wall prepares functional layer, can further promote the performance of microchannel plate, uses atomic layer deposition (Atomic at present
Layer Deposition) microchannel plate functional layer is prepared separately in film preparing technology, and it can be made to obtain very in aspect of performance
It is big to be promoted.
In order to guarantee the normal work of microchannel plate, the resistance value of resistive layer is generally 106~1010Between Ω cm, mesh
Before can with film type it is few, most commonly used is AZO film.AZO film is manufactured using atomic layer deposition method, is led in manufacturing process
Zn/Al ratio is overregulated, it is 10 that resistivity, which can be obtained,6The high resistance film of Ω cm or more.But when microchannel plate temperature compared with
When working under conditions of height, the variation of the order of magnitude can occur for the resistance of the film, cause microchannel plate performance unstable, service life drop
It is low.
Summary of the invention
Lead to microchannel plate performance greatly not to solve existing microchannel plate surface film in hot conditions change in resistance
Stable technical problem, the present invention provide a kind of microchannel plate and in microchannel plate inner wall preparation Cu doping Al2O3High resistance film
Method.
The technical solution of the invention is as follows provides a kind of microchannel plate, including microchannel plate ontology and setting in microchannel
The high resistance film of plate inner body wall, is characterized in that
Above-mentioned high resistance film is that Cu adulterates Al2O3High resistance film, above-mentioned Cu adulterate Al2O3High resistance film includes overlapping setting
Al2O3Film layer and Cu film layer.
Further, above-mentioned Al2O3Film layer includes the 8-12 layer Al of lamination setting2O3Film；Above-mentioned Cu film layer includes
One layer of Cu film.
The present invention also provides one kind to adulterate Al in microchannel plate inner wall preparation Cu2O3The method of high resistance film, including following step
It is rapid:
S1, cleaning treatment is carried out to microchannel plate ontology, and is packed into settling chamber；
S2, settling chamber is evacuated to 10-1~10-5After Pa, by deposition chamber heat to 100-120 DEG C；
S3,8-12 Al is first carried out on microchannel plate ontology using atomic layer deposition method2O3After deposition, then carry out primary
Cu deposition；
S4, it repeats step S3 450-650 times.
Further, single Al2O3Deposition process is as follows:
S311, it is passed through gaseous state TMA to settling chamber is deposited, inert gas purge settling chamber is then used, before extra
It is clean to drive body TMA purging；
S312, it is passed through gaseous state deionized water again, single layer Al is obtained by reaction2O3Film；
S313, inert gas purge settling chamber is used again, extra presoma gaseous state deionized water and by-product are purged dry
Only；
Cu deposition process is as follows:
S321, settling chamber is vacuumized, is passed through gaseous state Cu (dmap) to settling chamber2It is deposited, then uses inert gas
Settling chamber is purged, by extra presoma Cu (dmap)2Purging is clean；
S322, it is passed through gaseous state Et again2Zn obtains single layer Cu by reaction, uses inert gas purge settling chamber later, will be more
Remaining presoma gaseous state Et2Zn and by-product purging are clean.
Further, in order to accelerate being uniformly distributed for each substance in atomic layer deposition process, the condition existing for carrier gas
Under, gaseous state TMA, gaseous state deionized water, gaseous state Cu (dmap)2And gaseous state Et2Zn is passed through settling chamber with impulse form.
Further, Al in step S32O3Frequency of depositing is 12 times, and Cu frequency of depositing is 1 time；Repetition time in step S4
Number is 450 times.
Further, Al in step S32O3Frequency of depositing is 11 times, and Cu frequency of depositing is 1 time；Repetition time in step S4
Number is 500 times.
Further, Al in step S32O3Frequency of depositing is 10 times, and Cu frequency of depositing is 1 time；Repetition time in step S4
Number is 550 times.
Further, Al in step S32O3Frequency of depositing is 9 times, and Cu frequency of depositing is 1 time；Number of repetition in step S4
It is 600 times.
Further, exposure duration of the TMA in settling chamber is 0.03S in step S311, and inert blowing gas flyback time is
10S；
Exposure duration of the deionized water in settling chamber is 0.03S in step S312；
Inert blowing gas flyback time is 10S in step S313；
Cu (dmap) in step S3212Exposure duration in settling chamber is 2S, and inert blowing gas flyback time is 10S；
Step S322) in Et2Exposure duration of the Zn in settling chamber is 0.5S, and inert blowing gas flyback time is 10S.
Further, above-mentioned inert gas is nitrogen or argon gas.
Compared with prior art, the present invention beneficial effect is:
1, the present invention adulterates Al in microchannel plate inner wall preparation Cu2O3High resistance film, by adjusting Al2O3The film number of plies and
The Cu film number of plies, can be 106-1010The resistivity of accuracy controlling film within the scope of Ω cm；The adhesive force is strong, and Cu makees
It is just very stable for film itself attribute, it will not vary with temperature very big, it is ensured that the high resistance film is under high-temperature work environment or high
After temperature annealing, resistivity is held essentially constant, and film thermostabilization is very excellent, so that microchannel plate long service life, also can be used
In electron multiplier.
2, the present invention adulterates Al in microchannel plate inner wall preparation Cu2O3The method of high resistance film, simple process, deposition process
Controllably, pass through rate-determining steps 3) in Al2O3The control of frequency of depositing and Cu frequency of depositing, to control Cu doping ratio, so as to
106-1010The resistivity of accuracy controlling film within the scope of Ω cm；It is controlled by the whole cycle-index of step 4), it can be micro-
Compact structure, surfacing, film in homogeneous thickness are prepared on channel plate, so that the performance of microchannel plate is promoted.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of microchannel plate of the embodiment of the present invention；
Fig. 2 is the embodiment of the present invention in microchannel plate inner wall preparation Cu doping Al2O3The flow chart of high resistance film；
Fig. 3 is Cu of embodiment of the present invention doping ratio and its corresponding film resiativity schematic diagram.
Specific embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in detail.
As shown in Figure 1, the inner wall of microchannel plate of the invention is provided with high resistance film, high resistance film is that Cu adulterates Al2O3It is high
Film is hindered, Cu adulterates Al2O3High resistance film includes the Al of overlapping setting2O3Layer and Cu layers.
As shown in Fig. 2, the present invention adulterates Al in microchannel plate inner wall preparation Cu2O3The method of high resistance film is to utilize atom
Layer deposition techniques are alternately passed through precursor source, Oxidizing and Reducing Agents to settling chamber, Al are carried out on depositing base2O3Deposition and
What Cu was deposited.Settling chamber of the invention refers to the settling chamber of atomic layer deposition apparatus.In deposition, microchannel plate can lead to
Cross RCA standard cleaning liquid and HF solution ultrasonic cleaning processing.Precursor source of the present invention refers to using trimethyl aluminium (TMA) as the source Al,
Deionized water (H2O oxygen source, depositing Al) are used as2O3；With bis- (dimethylamino -2- the propoxyl group) (Cu (dmap) of copper (II)2) conduct
The source Cu, diethyl zinc (Et2Zn reducing agent, depositing Cu metal simple substance) are used as；High-purity argon gas (Ar) is used as carrier gas and purge gas.
Al2O3Deposition process is: settling chamber is evacuated to 10-1~10-5After Pa, TMA is passed through to settling chamber and is deposited,
Then settling chamber is purged with Ar, extra presoma is purged completely, then be passed through gaseous state deionized water, single layer is obtained by reaction
Al2O3, settling chamber finally is purged with Ar again, extra presoma and by-product are purged clean.Precursor source is in the sudden and violent of settling chamber
The purge time for revealing time and Ar is TMA/Ar/H2O/Ar=(0.03S/10S/0.03S/10S).
Cu deposition process is: settling chamber is evacuated to 10-1~10-5After Pa, Cu (dmap) is passed through to settling chamber2It is sunk
Then product purges settling chamber with Ar, extra presoma is purged completely, then be passed through gaseous state Et2Zn obtains single layer by reaction
Cu finally purges settling chamber with Ar again, and extra presoma and by-product are purged completely, metal simple-substance Cu film is obtained.Before
It is (Cu (dmap) that body source, which is driven, in the exposure duration of settling chamber and the purge time of Ar2/Ar/Et2Zn/Ar)=(2s/10s/0.5s/
10s)。
Cu adulterates Al2O3Film is exactly to carry out 8-12 Al2O3After deposition cycle, a Cu deposition process is carried out, once
As a systemic circulation, i.e., according to Al in one systemic circulation of control2O3Frequency of depositing and the ratio of Cu frequency of depositing control Cu
Doping ratio, doping ratio be deposit the number of plies ratio；Systemic circulation number is controlled again, and film thickness is controlled with this.
The present invention carries out 8~12 Al when carrying out film preparation2O3After deposition cycle, carries out a Cu deposition and follow
Ring, in this, as a systemic circulation, systemic circulation is carried out 450~650 times, obtains adulterating Al with a thickness of the Cu of 75~110nm2O3It is high
Film is hindered, resistivity meets 106-1010The requirement of Ω cm.
It is specific several embodiments of the invention below.
Embodiment one:
Microchannel plate is placed in RCA standard cleaning liquid SC-2 (HCl:H2O2:H2O=1:1:5 in), ultrasound is clear at 85 DEG C
It washes after ten minutes, is placed in (HF:H in HF solution at room temperature2O=1:50) after ultrasonic cleaning processing, microchannel plate is packed into former
In sublayer settling chamber, it is evacuated to 10-1Pa, and settling chamber and microchannel plate temperature are heated to 100 DEG C, start to carry out Al2O3
Deposition, i.e. TMA/Ar/H2O/Ar=(0.03s/10s/0.03s/10s) after recycling 12 times, carries out 1 Cu deposition, i.e. Cu
(dmap)2/Ar/Et2Zn/Ar=(2s/10s/0.5s/10s), 12 Al2O3After deposition cycle and 1 Cu deposition is 1 big
Circulation, systemic circulation stop deposition after carrying out 450 times, and room to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Cu doping
Al2O3The microchannel plate of film.
Embodiment two:
Microchannel plate is placed in RCA standard cleaning liquid SC-2 (HCl:H2O2:H2O=1:1:5 in), ultrasound is clear at 85 DEG C
It washes after ten minutes, is placed in (HF:H in HF solution at room temperature2O=1:50) after ultrasonic cleaning processing, microchannel plate is packed into former
In sublayer settling chamber, it is evacuated to 10-2Pa, and settling chamber and microchannel plate temperature are heated to 105 DEG C, start to carry out Al2O3
Deposition, i.e. TMA/Ar/H2O/Ar=(0.03s/10s/0.03s/10s) after recycling 11 times, carries out 1 Cu deposition, i.e. Cu
(dmap)2/Ar/Et2Zn/Ar=(2s/10s/0.5s/10s), 11 Al2O3After deposition cycle and 1 Cu deposition is 1 big
Circulation, systemic circulation stop deposition after carrying out 500 times, and room to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Cu doping
Al2O3The microchannel plate of film.
Embodiment three:
Microchannel plate is placed in RCA standard cleaning liquid SC-2 (HCl:H2O2:H2O=1:1:5 in), ultrasound is clear at 85 DEG C
It washes after ten minutes, is placed in (HF:H in HF solution at room temperature2O=1:50) after ultrasonic cleaning processing, microchannel plate is packed into former
In sublayer settling chamber, it is evacuated to 10-3Pa, and settling chamber and microchannel plate temperature are heated to 110 DEG C, start to carry out Al2O3
Deposition, i.e. TMA/Ar/H2O/Ar=(0.03s/10s/0.03s/10s) after recycling 10 times, carries out 1 Cu deposition, i.e. Cu
(dmap)2/Ar/Et2Zn/Ar=(2s/10s/0.5s/10s), 10 Al2O3After deposition cycle and 1 Cu deposition is 1 big
Circulation, systemic circulation stop deposition after carrying out 550 times, and room to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Cu doping
Al2O3The microchannel plate of film.
Example IV:
Microchannel plate is placed in RCA standard cleaning liquid SC-2 (HCl:H2O2:H2O=1:1:5 in), ultrasound is clear at 85 DEG C
It washes after ten minutes, is placed in (HF:H in HF solution at room temperature2O=1:50) after ultrasonic cleaning processing, microchannel plate is packed into former
In sublayer settling chamber, it is evacuated to 10-4Pa, and settling chamber and microchannel plate temperature are heated to 115 DEG C, start to carry out Al2O3
Deposition, i.e. TMA/Ar/H2O/Ar=(0.03s/10s/0.03s/10s) after recycling 9 times, carries out 1 Cu deposition, i.e. Cu
(dmap)2/Ar/Et2Zn/Ar=(2s/10s/0.5s/10s), 9 Al2O3After deposition cycle and 1 Cu deposition is 1 big
Circulation, systemic circulation stop deposition after carrying out 600 times, and room to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Cu doping
Al2O3The microchannel plate of film.
Embodiment five:
Microchannel plate is placed in RCA standard cleaning liquid SC-2 (HCl:H2O2:H2O=1:1:5 in), ultrasound is clear at 85 DEG C
It washes after ten minutes, is placed in (HF:H in HF solution at room temperature2O=1:50) after ultrasonic cleaning processing, microchannel plate is packed into former
In sublayer settling chamber, it is evacuated to 10-5Pa, and settling chamber and microchannel plate temperature are heated to 120 DEG C, start to carry out Al2O3
Deposition, i.e. TMA/Ar/H2O/Ar=(0.03s/10s/0.03s/10s) after recycling 8 times, carries out 1 Cu deposition, i.e. Cu
(dmap)2/Ar/Et2Zn/Ar=(2s/10s/0.5s/10s), 8 Al2O3After deposition cycle and 1 Cu deposition is 1 big
Circulation, systemic circulation stop deposition after carrying out 650 times, and room to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Cu doping
Al2O3The microchannel plate of film.
Al is adulterated to Cu on HALL8800 Hall effect tester2O3Film carries out electric property evaluation.Fig. 3 mixes for Cu
The schematic diagram of miscellaneous ratio and its corresponding film resiativity；Table 1 is that the Cu of embodiment one~five adulterates Al2O3Film at normal temperature and
400 DEG C of resistivity contrasts after annealing at a high temperature.
Table one
From above-described embodiment it follows that
It is in 8%~12% range in Cu doping ratio, when film thickness is 75~110nm, film resiativity is controllable
106~1010Within the scope of Ω cm, and after 400 DEG C of high annealings, film resiativity variation is less than an order of magnitude,
Film heat stability is excellent.
Claims (10)
1. a kind of microchannel plate, including microchannel plate ontology and the high resistance film of microchannel plate inner body wall, feature be set
It is:
The high resistance film is that Cu adulterates Al2O3High resistance film, the Cu adulterate Al2O3High resistance film includes overlapping setting
Al2O3Film layer and Cu film layer.
2. microchannel plate according to claim 1, it is characterised in that: the Al2O3Film layer includes the 8-12 of lamination setting
Layer Al2O3Film；The Cu film layer includes one layer of Cu film.
3. a kind of adulterate Al in microchannel plate inner wall preparation Cu2O3The method of high resistance film, which comprises the following steps:
S1, cleaning treatment is carried out to microchannel plate ontology, and is packed into settling chamber；
S2, settling chamber is evacuated to 10-1~10-5After Pa, settling chamber and microchannel plate ontology are heated to 100-120 DEG C；
S3,8-12 Al is first carried out on microchannel plate ontology using atomic layer deposition method2O3After deposition, then carries out a Cu and sink
Product；
S4, it repeats step S3450-650 times.
4. adulterating Al in microchannel plate inner wall preparation Cu according to claim 32O3The method of high resistance film, it is characterised in that:
Single Al2O3Deposition process is as follows:
S311, it is passed through gaseous state TMA to settling chamber is deposited, inert gas purge settling chamber is then used, by extra presoma
TMA purging is clean；
S312, it is passed through gaseous state deionized water again, single layer Al is obtained by reaction2O3Film；
S313, inert gas purge settling chamber is used again, extra presoma gaseous state deionized water and by-product are purged clean；
Cu deposition process is as follows:
S321, settling chamber is vacuumized, is passed through gaseous state Cu (dmap) to settling chamber2It is deposited, it is then heavy with inert gas purge
Product room, by extra presoma Cu (dmap)2Purging is clean；
S322, it is passed through gaseous state Et again2Zn obtains single layer Cu by reaction, uses inert gas purge settling chamber later, will be extra
Presoma gaseous state Et2Zn and by-product purging are clean.
5. adulterating Al in microchannel plate inner wall preparation Cu according to claim 42O3The method of high resistance film, it is characterised in that:
Under the conditions of existing for the carrier gas, gaseous state TMA, gaseous state deionized water, gaseous state Cu (dmap)2And gaseous state Et2Zn is with pulse form
Formula is passed through settling chamber；
The inert gas is nitrogen or argon gas.
6. according to claim 4 adulterate Al in microchannel plate inner wall preparation Cu2O3The method of high resistance film, feature exist
In: Al in step S32O3Frequency of depositing is 12 times, and Cu frequency of depositing is 1 time；Number of repetition in step S4 is 450 times.
7. according to claim 4 adulterate Al in microchannel plate inner wall preparation Cu2O3The method of high resistance film, feature exist
In: Al in step S32O3Frequency of depositing is 11 times, and Cu frequency of depositing is 1 time；Number of repetition in step S4 is 500 times.
8. according to claim 4 adulterate Al in microchannel plate inner wall preparation Cu2O3The method of high resistance film, feature exist
In: Al in step S32O3Frequency of depositing is 10 times, and Cu frequency of depositing is 1 time；Number of repetition in step S4 is 550 times.
9. according to claim 4 adulterate Al in microchannel plate inner wall preparation Cu2O3The method of high resistance film, feature exist
In: Al in step S32O3Frequency of depositing is 9 times, and Cu frequency of depositing is 1 time；Number of repetition in step S4 is 600 times.
10. described adulterating Al in microchannel plate inner wall preparation Cu according to claim 6 to 9 is any2O3The method of high resistance film,
It is characterized by:
Exposure duration of the TMA in settling chamber is 0.03S in step S311, and inert blowing gas flyback time is 10S；
Exposure duration of the deionized water in settling chamber is 0.03S in step S312；
Inert blowing gas flyback time is 10S in step S313；
Cu (dmap) in step S3212Exposure duration in settling chamber is 2S, and inert blowing gas flyback time is 10S；
Step S322) in Et2Exposure duration of the Zn in settling chamber is 0.5S, and inert blowing gas flyback time is 10S.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910068958.7A CN109680261A (en) | 2019-01-24 | 2019-01-24 | Microchannel plate and microchannel plate inner wall preparation Cu adulterate Al2O3The method of high resistance film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910068958.7A CN109680261A (en) | 2019-01-24 | 2019-01-24 | Microchannel plate and microchannel plate inner wall preparation Cu adulterate Al2O3The method of high resistance film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109680261A true CN109680261A (en) | 2019-04-26 |
Family
ID=66194502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910068958.7A Pending CN109680261A (en) | 2019-01-24 | 2019-01-24 | Microchannel plate and microchannel plate inner wall preparation Cu adulterate Al2O3The method of high resistance film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109680261A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111613500A (en) * | 2020-06-03 | 2020-09-01 | 鲁东大学 | Preparation method of aluminum oxide ion feedback prevention film of microchannel plate |
| CN113205996A (en) * | 2021-05-21 | 2021-08-03 | 东莞市中科原子精密制造科技有限公司 | Microchannel plate |
| CN115692140A (en) * | 2022-11-03 | 2023-02-03 | 北方夜视科技(南京)研究院有限公司 | Microchannel plate for inhibiting snowflake noise of low-light-level image intensifier and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108588680A (en) * | 2018-05-21 | 2018-09-28 | 中国科学院西安光学精密机械研究所 | Preparation of Mo-doped Al by atomic layer deposition2O3Method for forming high-resistance thin film |
| CN109182998A (en) * | 2018-07-18 | 2019-01-11 | 中国科学院西安光学精密机械研究所 | Microchannel plate and method for preparing Ni-doped Al on inner wall of microchannel plate2O3Method for forming high-resistance thin film |
-
2019
- 2019-01-24 CN CN201910068958.7A patent/CN109680261A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108588680A (en) * | 2018-05-21 | 2018-09-28 | 中国科学院西安光学精密机械研究所 | Preparation of Mo-doped Al by atomic layer deposition2O3Method for forming high-resistance thin film |
| CN109182998A (en) * | 2018-07-18 | 2019-01-11 | 中国科学院西安光学精密机械研究所 | Microchannel plate and method for preparing Ni-doped Al on inner wall of microchannel plate2O3Method for forming high-resistance thin film |
Non-Patent Citations (2)
| Title |
|---|
| BYUNG KOOK LEE ET.AL.: "Charge-Trapping Characteristics of Al2O3/Cu/Al2O3 Nanolaminate Structures Prepared Through Atomic Layer Deposition", 《JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY》 * |
| 熊鹏鹏: "利用原子层沉积技术改善有机电致发光器件电极层性能的研究", 《中国优秀硕士学位论文全文数据库（信息科技辑）》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111613500A (en) * | 2020-06-03 | 2020-09-01 | 鲁东大学 | Preparation method of aluminum oxide ion feedback prevention film of microchannel plate |
| CN111613500B (en) * | 2020-06-03 | 2023-03-31 | 鲁东大学 | Preparation method of aluminum oxide ion feedback prevention film of microchannel plate |
| CN113205996A (en) * | 2021-05-21 | 2021-08-03 | 东莞市中科原子精密制造科技有限公司 | Microchannel plate |
| CN115692140A (en) * | 2022-11-03 | 2023-02-03 | 北方夜视科技(南京)研究院有限公司 | Microchannel plate for inhibiting snowflake noise of low-light-level image intensifier and preparation method thereof |
| CN115692140B (en) * | 2022-11-03 | 2023-10-17 | 北方夜视科技(南京)研究院有限公司 | Microchannel plate for inhibiting snowflake point noise of low-light-level image intensifier and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109680261A (en) | Microchannel plate and microchannel plate inner wall preparation Cu adulterate Al2O3The method of high resistance film | |
| CN109709192B (en) | Gas-sensitive nanomaterial based on tungsten oxide/tin oxide core-shell nanosheet structure, preparation process and application thereof | |
| CN104485425B (en) | The processing method of perovskite-type material preparation method and equipment and its photovoltaic device | |
| CN109355638B (en) | Preparation method of phase-change controllable all-inorganic perovskite film and device application | |
| TWI586828B (en) | Doping method of atomic layer deposition | |
| CN107119264A (en) | Iridium alumina high temperature coating apparatus and technique are deposited with chamber In-situ reaction | |
| CN109182998A (en) | Microchannel plate and method for preparing Ni-doped Al on inner wall of microchannel plate2O3Method for forming high-resistance thin film | |
| CN107946176B (en) | Ga2O3Preparation method of thin film transistor | |
| CN106609392A (en) | Two-dimension nano-film preparation device and method | |
| CN113782639A (en) | PECVD process for reducing EL (electro-deposition) plating contamination of crystalline silicon solar cell | |
| CN106756877A (en) | C axles crystallization IGZO films and preparation method thereof | |
| CN111020487A (en) | Method for preparing film of quasi-one-dimensional structure material with controllable orientation | |
| CN110323270B (en) | Preparation method of graphene conductive film and thin film transistor | |
| CN108493083A (en) | Ultralow temperature stablizes the microchannel plate and preparation method thereof of temperature resistance characteristic | |
| CN105779971A (en) | Method for depositing p-type semi-conductor zinc oxide film on atomic layer | |
| CN104451600B (en) | Preparation method of bismuth oxide thin film material | |
| CN107425053A (en) | A kind of method that the concentric more iron heterojunction arrays of nucleocapsid three-dimensional manometer are built with ALD | |
| CN108588680A (en) | Preparation of Mo-doped Al by atomic layer deposition2O3Method for forming high-resistance thin film | |
| JPH01179423A (en) | Manufacture of insulating thin film | |
| CN108707875A (en) | A kind of tubular type CVD stoves connector, two-dimensional material and its grower and method | |
| CN110819958A (en) | Method for changing electrical properties of antimony selenide film and antimony selenide solar cell | |
| CN106048528A (en) | Method and device for membrane electrode manufacturing process | |
| CN109019571A (en) | The preparation method of the controllable nitrogen-doped graphene of the number of plies | |
| CN105220131B (en) | The method that air pulse method prepares thin film transistor (TFT) IGZO semiconductor film layers | |
| CN105132875B (en) | A kind of method that diffusion method prepares high concentration gradient AZO monocrystalline conductive films |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190426 |
|
| RJ01 | Rejection of invention patent application after publication |