CN107123582A - A kind of chemical cleaning method of GaAs photocathodes - Google Patents
A kind of chemical cleaning method of GaAs photocathodes Download PDFInfo
- Publication number
- CN107123582A CN107123582A CN201710324608.3A CN201710324608A CN107123582A CN 107123582 A CN107123582 A CN 107123582A CN 201710324608 A CN201710324608 A CN 201710324608A CN 107123582 A CN107123582 A CN 107123582A
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- CN
- China
- Prior art keywords
- gaas
- cleaning
- photocathodes
- gaas photocathodes
- degreasing
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/12—Manufacture of electrodes or electrode systems of photo-emissive cathodes; of secondary-emission electrodes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
Abstract
The present invention discloses a kind of chemical cleaning method of GaAs photocathodes, comprises the following steps:(10) cleaning by degreasing:GaAs photocathodes are inserted into organic solvent, ultrasonic degreasing cleaning is carried out;(20) etch cleaner:GaAs photocathodes Jing Guo cleaning by degreasing are inserted into etching liquid, cleaning is performed etching;(30) deionized water rinsing:It will be rinsed by the GaAs photocathodes of etch cleaner with ionized water, the GaAs photocathodes cleaned.The chemical cleaning method of the GaAs photocathodes of the present invention, good purification, spectral response is high.
Description
Technical field
The invention belongs to semiconductor optoelectronic emissive material preparing technical field, and in particular to a kind of good purification, spectrum
The chemical cleaning method of the high GaAs photocathodes of response.
Background technology
GaAs (GaAs) photocathode has higher responding ability and less dark in visible ray and near infrared region
Emission current, therefore be widely applied in LLL night-vision imaging device.GaAs photocathodes are used as modern lll night vision
The core component of device, determines the spectral response range and overall performance of device.It is cloudy for GaAs photocathodes
The preparation technology of pole directly determines the photoemission performance of negative electrode.
At present, most of techniques for preparing GaAs photocathodes still use the preparation process first cleaned and activated afterwards.
GaAs easily adsorbs O in surface2、H2O、CO、CO2Isoreactivity composition, and form new surface composition, table as caused by electric charge transfer
Thus there is natural oxide and carbide in face.If not removing these pollutions, the life-span of GaAs photocathodes, stability and the moon
Pole activating sensitivity will be severely impacted.Therefore need to carry out surface cleaning processing, to reduce the pollution that negative electrode is subject to as far as possible.
GaAs purifications are generally completed by processes such as degreasing, wet-chemical cleanings.
Conventional wet-chemical cleaning includes:1st, using sulfuric acid and hydrogen peroxide mixed solution and hydrochloric acid solution to GaAs negative electrodes
Surface progress Chemical cleaning (Z.Liu, Y.Sun, F.Machuca, P.Pianetta, W.E.Spicer, and R.F.W.Pease,
Preparation of clean GaAs(100)studied by synchrotron radiationphotoemission,
Journal of Vacuum Science&Technology A:Vacuum,Surfaces,and Films,2003,21(1):
212-218).This method can effectively remove the oxide of the carbon on GaAs surfaces, Ga oxide and As, but be due to that sulfuric acid is molten
Corrosion is strong, destroys larger to GaAs cathode surfaces structure.2nd, chemistry is carried out to GaAs cathode surfaces using hydrofluoric acid solution
Clean (M.Ohno, Y.Ishii, and S.Miyazawa, Effect of Photoirradiation of GaAs Surface
during HF Treatment,Journal of the Electrochemical Society,1984,131(10):2441-
2443).This method can effectively remove the oxide on GaAs surfaces, but more carbon is still remained on GaAs surfaces.3rd, utilize
Hydrochloric acid and isopropyl alcohol mixture GaAs cathode surfaces are carried out Chemical cleaning (O.E.Tereshchenko,
S.I.Chikichev,A.S.Terekhov,Atomic structure and electronic properties of HCl–
isopropanoltreated and vacuum annealed GaAs(100)surface,Applied Surface
Science,1999,142:75-80).This method can substantially remove the carbon on GaAs surfaces, but remove GaAs oxide on surface
It is less efficient.
In a word, the problem of prior art is present be:To the Chemical cleaning of GaAs photocathodes, clean-up effect is not good enough, shadow
Ring the spectral response of GaAs photocathodes.
The content of the invention
It is an object of the invention to provide a kind of chemical cleaning method of GaAs photocathodes, good purification, spectrum rings
Ying Gao.
The technical scheme for realizing the object of the invention is:
A kind of chemical cleaning method of GaAs photocathodes, comprises the following steps:
(10) cleaning by degreasing:GaAs photocathodes are inserted into organic solvent, ultrasonic degreasing cleaning is carried out;
(20) etch cleaner:GaAs photocathodes Jing Guo cleaning by degreasing are inserted into etching liquid, cleaning is performed etching;
(30) deionized water rinsing:It will be rinsed by the GaAs photocathodes of etch cleaner with ionized water, obtain clear
Clean GaAs photocathodes.
Preferably, described (10) cleaning by degreasing step is specially:
GaAs photocathodes are inserted into carbon tetrachloride, acetone, absolute ethyl alcohol and deionized water successively and carry out ultrasonic degreasing
Cleaning.
Preferably, in described (10) cleaning by degreasing step, ultrasonic wave scavenging period is no less than 5 minutes.
Preferably, described (20) etch cleaner step includes:
(21) hf etching:GaAs photocathodes Jing Guo cleaning by degreasing are inserted into hydrofluoric acid solution, etch period is not
Less than 5 minutes;
(22) mixed liquor is etched:Hydrochloric acid isopropyl alcohol mixture will be inserted by the GaAs photocathodes of hf etching,
Etch period is no less than 5 minutes.
Preferably, in the hydrochloric acid isopropyl alcohol mixture, hydrochloric acid solution HCl contents be 36%~38%, hydrochloric acid with it is different
The volume ratio of propyl alcohol is 1:10.
Compared with prior art, the present invention has the advantages that:
1st, good purification:First used in cleaning step of the present invention and use hydrochloric acid and isopropanol after hydrofluoric acid solution etch cleaner again
Mixed solution etch cleaner can more effectively remove oxide of organic matter, Ga oxide and As of cathode surface absorption etc.
Pollutant, makes negative electrode obtain atomically clean surfaces, and will not damage GaAs photocathode emission layer surface crystal structures.
2nd, spectral response is high:Under identical activation condition, the GaAs photocathodes prepared through cleaning method of the present invention
Spectral response is higher than the GaAs photocathode spectral responses through traditional cleaning method preparation.
Brief description of the drawings
Fig. 1 is the flow chart of the chemical cleaning method of GaAs photocathodes of the present invention.
Fig. 2 is the structural representation of GaAs photocathodes.
Fig. 3 is the XPS analysis power spectrum using GaAs photocathodes surface gallium and arsenic after the inventive method Chemical cleaning.
Fig. 4 is using GaAs photocathodes surface carbon and the XPS analysis power spectrum of oxygen after the inventive method Chemical cleaning.
Fig. 5 is using the spectral response after the GaAs photocathodes activation after the inventive method Chemical cleaning.
Embodiment
For ease of understanding and verifying effectiveness of the invention, the present invention is made into one with specific embodiment below in conjunction with the accompanying drawings
Step is described in detail.
Embodiment 1
Fig. 1 for the GaAs photocathodes in the present invention used in embodiment modular construction schematic diagram.GaAs photocathodes
From bottom to top by high-quality n-type GaAs (100) substrate (1), p-type AlxGa1-xAs cushions (2), p-type GaAs emission layers (3).
The GaAs photocathodes of 3 such as Fig. 1 structures are taken, sample 1,2 and 3 is respectively designated as.
The present embodiment includes 3 laboratory samples, carries out Chemical cleaning using distinct methods respectively.The cleaning method of sample 1 is
5min is cleaned with HF (40%) solution;The cleaning method of sample 2 is to use HCl:IPA(1:10) solution cleaning 5min;The cleaning of sample 3
The cleaning method that method is proposed by this patent.
First by organic solvent four GaAs photocathodes samples are carried out with preliminary cleaning, according to carbon tetrachloride, third
The sequencing of ketone, absolute ethyl alcohol and deionized water is respectively put into ultrasonic washing instrument and cleaned 5 minutes.This step can be cleaned
The organic matter of GaAs photocathodes surface physics absorption and the oxygen of part free state.
Secondly, sample 1 is cleaned 5 minutes using HF solution;Sample 2 is cleaned 5 minutes using hydrochloric acid and isopropyl alcohol mixture;
Sample 3 is first cleaned 5 minutes using HF solution, reuses hydrochloric acid and isopropyl alcohol mixture is cleaned 5 minutes.Wherein HF solution is dense
The mixed proportion for spending hydrochloric acid and isopropanol in the HF solution for 40%, hydrochloric acid and isopropyl alcohol mixture is 1:10.
Finally, 3 samples are rinsed using deionized water, complete Chemical cleaning.
XPS surface analyses are carried out to the GaAs photocathodes sample after Chemical cleaning, as a result as shown in Figures 2 and 3.And
The percentage composition of GaAs photocathodes surface-element after Chemical cleaning is calculated, as shown in table 1.
Table 1, GaAs photocathode surface-element percentage compositions
From table 1 it follows that 3 samples are after Chemical cleaning, surface C and O content are reduced.The surface O of sample 1
Although content is seldom, C content is appointed so a lot, and the surface of sample 2 is then that C content is few, and O content is a lot, only the surface of sample 3
It can realize that C and O percentage composition are minimum.Therefore, first cleaned 5 minutes using HF solution, reuse hydrochloric acid and isopropanol is mixed
Close solution to clean 5 minutes, the surface cleanness of GaAs photocathodes can be improved.
The heating location that 3 samples after cleaning are sent to activation system respectively carries out heating purification, treats at sample heating
Reason terminates after natural cooling, enters line activating.Spectral response measurement is carried out to the GaAs photocathodes sample after activation, shown in Fig. 4
For the spectral response curve of GaAs photocathodes.Figure 4, it is seen that the spectral response of the GaAs photocathodes of the present invention is whole
Body is higher than the spectral response of other 2 groups of samples.It is computed, the integral sensitivity of sample 1 is 2236 μ A/lm, the integration spirit of sample 2
Sensitivity is 1695 μ A/lm, and the integral sensitivity of sample 3 is 2523 μ A/lm.Compared with sample 1 and 2, the integral sensitivity of sample 3
12.84% and 48.85% has been respectively increased.
Embodiment 2
The present embodiment step is same as Example 1, and sample cleans 8min, HCl using HF (40%) solution:IPA(1:10)
Solution cleans 8min.The percentage composition of GaAs photocathodes surface-element is as shown in table 2 after cleaning.It is computed, sample activation
The integral sensitivity measured afterwards is 2587 μ A/lm.As a result it is approximate with embodiment 1.Therefore, first cleaned 8 minutes using HF solution, then
Cleaned 8 minutes using hydrochloric acid and isopropyl alcohol mixture, the surface cleanness of GaAs photocathodes can be improved, and lift its light
Spectrum response.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail good embodiment, it will be understood by those within the art that, can be to skill of the invention
Art scheme is modified or equivalent substitution, and without departing from the objective and scope of technical solution of the present invention, it all should cover at this
Among the right of invention.
Claims (5)
1. a kind of chemical cleaning method of GaAs photocathodes, it is characterised in that comprise the following steps:
(10) cleaning by degreasing:GaAs photocathodes are inserted into organic solvent, ultrasonic degreasing cleaning is carried out;
(20) etch cleaner:GaAs photocathodes Jing Guo cleaning by degreasing are inserted into etching liquid, cleaning is performed etching;
(30) deionized water rinsing:It will be rinsed, cleaned with deionized water by the GaAs photocathodes of etch cleaner
GaAs photocathodes.
2. chemical cleaning method according to claim 1, it is characterised in that (10) the cleaning by degreasing step is specially:
GaAs photocathodes are inserted into progress ultrasonic degreasing in carbon tetrachloride, acetone, absolute ethyl alcohol and deionized water successively clear
Wash, scavenging period is no less than 5 minutes.
3. chemical cleaning method according to claim 1, it is characterised in that (20) the etch cleaner step includes:
(21) hf etching:GaAs photocathodes Jing Guo cleaning by degreasing are inserted into hydrofluoric acid solution, etch period is no less than 5
Minute;
(22) mixed liquor is etched:Hydrochloric acid isopropyl alcohol mixture will be inserted by the GaAs photocathodes of hf etching, etched
Time is no less than 5 minutes.
4. chemical cleaning method according to claim 3, it is characterised in that the concentration of the hydrofluoric acid solution is 40%.
5. chemical cleaning method according to claim 2, it is characterised in that in the hydrochloric acid isopropyl alcohol mixture, salt
Acid solution HCl contents are 36%~38%, and hydrochloric acid and isopropanol mixed proportion are 1:10.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109427517A (en) * | 2017-09-02 | 2019-03-05 | 南京理工大学 | A kind of monochromatic light exposure Activiation method improving GaAs photocathode spectral response and stability |
CN110813902A (en) * | 2019-09-05 | 2020-02-21 | 南京理工大学 | Method for cleaning gallium arsenide photocathode |
Citations (1)
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CN1906738A (en) * | 2004-06-28 | 2007-01-31 | 住友电气工业株式会社 | GaAs substrate cleaning method, GaAs substrate manufacturing method, epitaxial substrate manufacturing method and GaAs wafer |
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2017
- 2017-05-10 CN CN201710324608.3A patent/CN107123582A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1906738A (en) * | 2004-06-28 | 2007-01-31 | 住友电气工业株式会社 | GaAs substrate cleaning method, GaAs substrate manufacturing method, epitaxial substrate manufacturing method and GaAs wafer |
Non-Patent Citations (7)
Title |
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A.SALETES等: ""Residual Carbon and Oxygen Surface Contamination of Chemically Etched GaAs(001) Substrates"", 《JAPANESE JOURNAL OF APPLIED PHYSICS》 * |
O.E.TERESHCHENKO等: ""Atomic structure and electronic properties of HCl–isopropanol treated and vacuum annealed GaAs(100) surface"", 《APPLIED SURFACE SCIENCE》 * |
O.E.TERESHCHENKO等: ""Composition and structure of chemically prepared GaAs(1 1 1)A and (1 1 1)B surfaces"", 《SURFACE SCIENCE》 * |
O.E.TERESHCHENKO等: ""Composition and structure of chemically prepared GaAs(111)A and (111)B surfaces"", 《SURFACE SCIENCE》 * |
P.LAUKKANEN等: ""Scanning tunneling microscopy study of GaAs(1 0 0) surface prepared by HC1-isopropanol treatment"", 《APPLIED SURFACE SCIENCE》 * |
V.L.ALPEROVICH等: ""Surface passivation and morphology of GaAs(1 0 0) treated in HCl-isopropanol solution"", 《APPLIED SURFACE SCIENCE》 * |
葛仲浩: ""GaAs基片吸附脱附的研究"", 《中国优秀硕士学位论文全文数据库信息科技辑》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109427517A (en) * | 2017-09-02 | 2019-03-05 | 南京理工大学 | A kind of monochromatic light exposure Activiation method improving GaAs photocathode spectral response and stability |
CN110813902A (en) * | 2019-09-05 | 2020-02-21 | 南京理工大学 | Method for cleaning gallium arsenide photocathode |
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