CN111584327B - Activation method for improving quantum efficiency of gallium arsenide photocathode - Google Patents

Activation method for improving quantum efficiency of gallium arsenide photocathode Download PDF

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CN111584327B
CN111584327B CN202010358215.6A CN202010358215A CN111584327B CN 111584327 B CN111584327 B CN 111584327B CN 202010358215 A CN202010358215 A CN 202010358215A CN 111584327 B CN111584327 B CN 111584327B
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source
photocurrent
activation
quantum efficiency
cesium
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CN111584327A (en
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张益军
李诗曼
张锴珉
舒昭鑫
荣敏敏
钱芸生
石峰
程宏昌
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Nanjing University of Science and Technology
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    • 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

Abstract

The invention discloses an activation method for improving the quantum efficiency of a gallium arsenide photocathode, which comprises the following steps: the cesium source is turned on, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value; when the photoelectric current is reduced to 50% -90% of the peak current, the oxygen source is started, and the cesium source is kept in a starting state; turning off the oxygen source when the photocurrent reaches the peak value again; and when the photoelectric current drops to 50-90% of the peak value, opening the oxygen source, repeating the activation process until the peak current of the photoelectric current is 100-110% of the previous peak current, opening the fluorine source when the photoelectric current drops to 50-90% of the peak current, and closing the fluorine source and the cesium source successively when the photoelectric current rises to a new peak value to finish the activation process. The invention can obtain the gallium arsenide photocathode with better photoelectric emission performance, is compatible with the traditional cesium-oxygen activation process, has a computer-aided control activation mode, is simple to operate and is easy to popularize.

Description

Activation method for improving quantum efficiency of gallium arsenide photocathode
Technical Field
The invention belongs to the technology of activating photoelectric emission materials, and particularly relates to an activating method for improving the quantum efficiency of a gallium arsenide photocathode.
Background
The GaAs photocathode with a clean surface is activated in an ultrahigh vacuum environment, and the gallium arsenide negative electron affinity (GaAs NEA) photocathode with the advantages of high quantum efficiency, high current density, small dark emission, high polarizability, concentrated emitted electron energy distribution and the like can be effectively prepared. The GaAs NEA photocathode is widely applied to a plurality of fields such as a high-performance micro-light image intensifier, an accelerator photocathode injector, a transmission electron microscope, a novel solar cell and the like. In the current photocathode application, a GaAs NEA photocathode is taken as an important component of a three-generation micro-light image intensifier, and the integral sensitivity, the spectral response range and the stability of the GaAs NEA photocathode greatly influence the imaging quality, the service life and other important performances of a device. In order to improve the quality and the service life of the three-generation low-light-level image intensifier in China, a novel activation process of a GaAs NEA photocathode is required to be explored, and the photocathode with the quantum efficiency as high as possible can be prepared while the stability is ensured. However, the high quantum efficiency and good stability of the cathode are conflicting problems in the fabrication of GaAs NEA photocathodes.
In the conventional activation research of GaAs photocathode, cesium source and oxygen source (Cs/O) are adopted 2 ) The activation pattern has been studied relatively much. Existing Cs/O 2 The activation method adopted for activation generally has two types: firstly, cesium source is continuous, and an oxygen source is interrupted; secondly, cesium source and oxygen source are alternately intermittent. The first activation method, which in turn is widely used by researchers due to its simpler control, is however based on this Cs/O 2 The quantum efficiency and stability of GaAs NEA photocathodes prepared by the activation method are still not ideal. However, in practical applications, it is necessary to ensure that the GaAs NEA photocathode has high quantum efficiency and good stability, so an activation method capable of further improving the quantum efficiency of the GaAs photocathode still needs to be explored.
Disclosure of Invention
The invention aims to provide an activation method for improving the quantum efficiency of a gallium arsenide photocathode.
The technical solution for realizing the purpose of the invention is as follows: an activation method for improving the quantum efficiency of a gallium arsenide photocathode comprises cesium source activation, oxygen source activation and fluorine source activation, wherein a halogen tungsten lamp is used for vertically irradiating the whole cathode surface in a white light mode in the activation process, and the specific steps are as follows:
step 1, carrying out chemical cleaning and high-temperature purification on a sample to be activated;
step 2, a cesium source is started, the cesium source vertically irradiates a sample to be activated, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
step 3, when the photoelectric current falls to a first threshold range, starting an oxygen source, keeping the cesium source in a starting state, and converting the photoelectric current into an increase;
step 4, when the photocurrent reaches the peak value again, the oxygen source is closed, and the photocurrent firstly rises slightly and then immediately falls;
step 5, when the photoelectric current falls to a first threshold range, opening an oxygen source, and converting the photoelectric current into rising after continuously falling;
step 6, repeating the step 4 and the step 5 until the peak current of the photocurrent is within a second threshold range, turning on a fluorine source when the photocurrent falls into a third threshold range, and converting the photocurrent into the rising again;
and 7, when the photocurrent rises to a new peak value, closing the fluorine source and the cesium source in sequence, and ending the activation process.
Preferably, the step 1 chemical cleaning method comprises the following steps: ultrasonically cleaning a sample by sequentially adopting acetone, methanol and deionized water to finish the degreasing step;
sequentially placing the sample into a HF solution and a mixed solution of HCl and IPA for chemical etching;
the sample was rinsed thoroughly with deionized water.
Preferably, the high-temperature purification step in step 1 is: putting the sample after chemical cleaning into an ultrahigh vacuum system for heating for 15-60 minutes, wherein the heating temperature is 550-650 ℃, and the vacuum degree of the ultrahigh vacuum system is not lower than 10 -7 Of the order of Pa.
Preferably, step 2, step 3, step 4, step 5, step 6 and step 7 are all performed in an ultra-high vacuum system.
Preferably, the cesium source and the oxygen source in step 2, step 3, step 4, step 5, and step 6 are all solid-state sources packaged with nickel tubes.
Preferably, the fluorine source in step 7 is a gaseous source, and the gas inlet method comprises the following steps: the opening and closing number of the micro air inlet valve can be adjusted electrically to control the inlet of the ultra-vacuum system NF 3 The intake air amount.
Preferably, the first threshold range is 50% to 90% of the peak current.
Preferably, the second threshold range is 100-110% of the previous peak current.
Preferably, the third threshold range is 50% to 90% of the peak current.
Compared with the prior art, the invention has the beneficial effects that: 1) activation of the inventionThe GaAs photocathode has higher quantum efficiency and better photoemission performance; 2) the invention is compatible with the traditional cesium oxygen activation process and only increases the NF 3 The method has the advantages of simple operation and easy popularization; 3) the opening and closing of all the activation sources in the invention utilizes computer-aided control to NF 3 The air inflow can be controlled precisely in a micro-scale manner, and the activation requirement is met.
Drawings
FIG. 1 is a flow chart of the activation method for improving the quantum efficiency of the GaAs photocathode of the present invention.
FIG. 2 is a diagram of conventional Cs/O 2 Photocurrent curve of the activated GaAs photocathode.
Fig. 3 is a graph of photocurrent for an activated GaAs photocathode of the present invention.
FIG. 4 shows the present invention with Cs/O 2 Graph comparing quantum efficiency of activated GaAs photocathodes.
FIG. 5 shows the present invention with Cs/O 2 Graph showing the photo-current decay of the activated GaAs photocathode.
Detailed Description
With reference to fig. 1, the activating method for improving the quantum efficiency of the gallium arsenide photocathode of the present invention specifically comprises the following steps:
step 1, carrying out chemical cleaning and high-temperature purification on a sample to be activated;
the chemical cleaning method comprises the following steps: firstly, ultrasonically cleaning a sample by sequentially adopting acetone, methanol and deionized water to finish the degreasing step; then, the sample is sequentially put into a HF solution and a mixed solution of HCl and IPA for chemical etching; and finally, fully washing the sample with deionized water.
The high-temperature purification step is as follows: putting the sample after chemical cleaning into an ultrahigh vacuum system for heating for 15-60 minutes, wherein the heating temperature is 550-650 ℃, and the vacuum degree of the ultrahigh vacuum system is not less than 10 -7 Of the order of Pa.
Step 2, opening the cesium source, and gradually raising the photocurrent which falls after reaching a peak value;
step 3, when the photoelectric current is reduced to 50% -90% of the peak current, starting the oxygen source, keeping the cesium source in a starting state, and converting the photoelectric current into rising;
step 4, when the photocurrent reaches the peak value again, the oxygen source is closed, and the photocurrent firstly rises slightly and then immediately falls;
step 5, when the photoelectric current drops to 50% -90% of the peak value, opening an oxygen source, and converting the photoelectric current into rising after continuously dropping;
step 6, repeating the step 4 and the step 5 until the peak current of the photocurrent is 100-110% of the previous peak current, turning on a fluorine source when the photocurrent drops to 50-90% of the peak current, and converting the photocurrent to rise again;
and 7, when the photocurrent rises to a new peak value, closing the fluorine source and the cesium source in sequence, and ending the activation process.
The above operations are all carried out in an ultrahigh vacuum system, and the vacuum degree of the ultrahigh vacuum system is not lower than 10 -7 In the order of Pa. During the activation process, the whole cathode surface is vertically irradiated by white light of a halogen tungsten lamp.
In the activation process, the cesium source and the oxygen source are controlled by computer assistance, namely the current of an external current source is adjusted, and the energizing and air-releasing quantities of the cesium source and the oxygen source are controlled; the fluorine source can be electrically adjusted to adjust the number of the micro air inlet valve switches to control the fluorine source to enter the ultra-vacuum system NF 3 An intake air amount. The air intake mode can realize micro accurate control of air intake quantity.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The activation flow is shown in fig. 1.
In Cs/O 2 /NF 3 Before activation, the GaAs photoelectric cathode material is subjected to chemical cleaning and high-temperature purification.
The chemical cleaning step is that firstly, acetone, methanol and deionized water are adopted to ultrasonically clean a sample in sequence to finish the degreasing step; then, sequentially putting the sample into a HF solution and a mixed solution of HCl and IPA with the ratio of 1:10 for chemical etching; and finally, fully washing the sample with deionized water and drying.
The high-temperature purification step is to put the sample after chemical cleaning into a vacuum degreeLess than 10 -7 Heating is carried out for 60 minutes in an ultrahigh vacuum system of Pa magnitude, and the heating temperature is 650 ℃. When the sample is naturally cooled to room temperature, the sample is sent to an activation position, and the Cs/O is started 2 /NF 3 And (6) activating.
When the cesium source is activated, the white light of a halogen tungsten lamp is adopted to vertically irradiate the whole cathode surface, and the on or off of the cesium source, the oxygen source and the fluorine source is determined by measuring and observing the photocurrent generated by the cathode in real time. And the cesium source and the oxygen source used for activation are solid sources packaged by nickel tubes, wherein the cesium source is a solid source for reducing cesium chromate by using zirconium-aluminum alloy powder, and the oxygen source is a solid source for reducing barium peroxide. The size of the electrification and deflation amount of the cesium source and the oxygen source can be controlled through computer-aided control, namely the size of the current of the solid source externally connected with a current source is adjusted. The emission amounts of the cesium source and the oxygen source from different sources may be different, so that the current of the external current source of the cesium source and the external current source of the oxygen source during the activation process are different, and a proper cesium-oxygen ratio should be obtained through an experimental method after the cesium oxygen source is replaced. Activating the used fluorine source as a gaseous source, and controlling NF by electrically adjusting the number of the micro air inlet valve switches 3 The gas enters the ultra-high vacuum system, in the embodiment, the NF entering the ultra-high vacuum system can be determined by combining the vacuum degree feedback of the computer real-time monitoring system 3 And if the gas is proper, adjusting the switch of the adjustable micro gas inlet valve in time. The specific activation steps are as follows:
(1) the cesium source is turned on, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
(2) when the photoelectric current is reduced to about 80% of the peak current, the oxygen source is started, the cesium source is kept in a starting state, and the photoelectric current is converted into an increase;
(3) when the photocurrent reaches the peak value again, the oxygen source is closed, and the photocurrent firstly rises slightly and then immediately falls;
(4) when the photoelectric current drops to about 80% of the peak value, the oxygen source is opened, and the photoelectric current continuously drops and then is converted into rising;
(5) repeating the step 4 and the step 5 until the peak current of the photocurrent is 100-110% of the previous peak current, turning on a fluorine source when the photocurrent drops to about 90% of the peak current, and converting the photocurrent to rise again;
(6) and when the photocurrent rises to a new peak value, the fluorine source and the cesium source are closed in sequence, and the activation process is ended.
Under the same GaAs photocathode and the same chemical cleaning, high temperature cleaning and activation environment conditions, we performed comparative experiments, and as shown in FIG. 2, Cs/O 2 Activating a photocurrent curve of the GaAs photocathode, wherein the cesium source is continuously activated by adopting an activation method, the oxygen source is interrupted, the oxygen source is started when the photocurrent drops to about 80% of the cesium peak, and the oxygen source is closed when the photocurrent reaches the oxygen peak; FIG. 3 shows Cs/O of the present invention 2 /NF 3 And activating a photocurrent curve of the GaAs photocathode, wherein the activating method is adopted to ensure that the cesium source is continuous, the oxygen source is interrupted, the oxygen source is started when the photocurrent drops to about 80% of the cesium peak, the oxygen source is closed when the photocurrent reaches the oxygen peak until the photocurrent peak value is not increased any more and the fluorine source is started when the photocurrent peak value drops to about 90% of the peak value, and the fluorine source and the cesium source are closed when the photocurrent continuously rises to a new peak value. FIG. 4 is a GaAs photocathode quantum efficiency curve and conventional Cs/O of the activation method of the present invention 2 Comparative plot of activation method, where Curve 1 is Cs/O 2 The quantum efficiency of the cathode obtained by activation, where Curve 2 is the Cs/O of the invention 2 /NF 3 The quantum efficiency of the cathode obtained by activation can be seen to be obviously higher than that of the cathode obtained by activation of the invention 2 Activation and Cs/NF 3 And (4) activating. FIG. 5 is the light current decay curve and Cs/O of GaAs photocathode of the activation method of the present invention 2 A contrast diagram of the activation method, in which the cathode surface after activation is vertically irradiated by white light of a halogen tungsten lamp, and the curve 1 is Cs/O 2 Activation, curve 2 Cs/O 2 /NF 3 Activation can be seen that cathode photocurrents activated by the two methods both rise and then fall, but the cathode photocurrents activated by the method are higher and still have good stability, and still have the photoemission capability after being attenuated for 10 hours under strong white light irradiation.
Example 2
An activation method for improving the quantum efficiency of a gallium arsenide photocathode comprises cesium source activation, oxygen source activation and fluorine source activation, and specifically comprises the following steps:
step 1, carrying out chemical cleaning and high-temperature purification on a sample to be activated;
the chemical cleaning method comprises the following steps: firstly, ultrasonically cleaning a sample by sequentially adopting acetone, methanol and deionized water to finish the degreasing step; then, sequentially putting the sample into a HF solution and a mixed solution of HCl and IPA with the ratio of 1:10 for chemical etching; and finally, fully washing the sample with deionized water.
The high-temperature purification step is as follows: putting the sample after chemical cleaning into an ultrahigh vacuum system for heating for 15 minutes, wherein the heating temperature is 550 ℃, and the vacuum degree of the ultrahigh vacuum system is not lower than 10 -7 Of the order of Pa.
Step 2, opening the cesium source, and gradually raising the photocurrent which falls after reaching a peak value;
step 3, when the photoelectric current is reduced to about 80% of the peak current, starting the oxygen source, keeping the cesium source in a starting state, and converting the photoelectric current into an increase;
step 4, when the photocurrent reaches the peak value again, the oxygen source is closed, and the photocurrent firstly rises slightly and then immediately falls;
step 5, when the photoelectric current drops to about 80% of the peak value, opening an oxygen source, and converting the continuous drop of the photoelectric current into the rise of the photoelectric current;
step 6, repeating the step 3 and the step 4 until the peak current of the photocurrent is 100-110% of the previous peak current, turning on a fluorine source when the photocurrent drops to about 90% of the peak current, and converting the photocurrent to rise again;
and 7, when the photocurrent rises to a new peak value, closing the fluorine source and the cesium source in sequence, and ending the activation process.
The above operations are all carried out in an ultrahigh vacuum system, and the vacuum degree of the ultrahigh vacuum system is not lower than 10 -7 Of the order of Pa. During the activation process, the whole cathode surface is vertically irradiated by white light of a halogen tungsten lamp.
In the activation process, the cesium source and the oxygen source are controlled by computer assistance, namely, the current of an external current source is adjustedControlling the electrification and air release amount of the cesium source and the oxygen source; the fluorine source can be electrically adjusted to adjust the number of the micro air inlet valve switches to control the fluorine source to enter the ultra-vacuum system NF 3 The intake air amount. The air intake mode can realize micro accurate control of air intake quantity.

Claims (9)

1. An activation method for improving the quantum efficiency of a gallium arsenide photocathode is characterized by comprising cesium source activation, oxygen source activation and fluorine source activation, wherein a halogen tungsten lamp is used for vertically irradiating the whole cathode surface in a white light mode in the activation process, and the specific steps are as follows:
step 1, carrying out chemical cleaning and high-temperature purification on a sample to be activated;
step 2, a cesium source is started, the cesium source vertically irradiates a sample to be activated, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
step 3, when the photoelectric current falls to a first threshold range, starting an oxygen source, keeping the cesium source in a starting state, and converting the photoelectric current into an increase;
step 4, when the photocurrent reaches the peak value again, the oxygen source is closed, and the photocurrent firstly rises slightly and then immediately falls;
step 5, when the photoelectric current falls to a first threshold range, opening an oxygen source, and converting the continuous falling of the photoelectric current into the rising of the photoelectric current;
step 6, repeating the step 4 and the step 5 until the peak current of the photocurrent is within a second threshold range, turning on a fluorine source when the photocurrent falls into a third threshold range, and converting the photocurrent into the rising again;
and 7, when the photocurrent rises to a new peak value, closing the fluorine source and the cesium source in sequence, and ending the activation process.
2. The activation method for improving the quantum efficiency of the gallium arsenide photocathode according to claim 1, wherein the chemical cleaning method in step 1 is: ultrasonically cleaning a sample by sequentially adopting acetone, methanol and deionized water to finish the degreasing step;
sequentially placing the sample into a HF solution and a mixed solution of HCl and IPA for chemical etching;
the sample was rinsed thoroughly with deionized water.
3. The activation method for improving the quantum efficiency of the gallium arsenide photocathode according to claim 1, wherein the high temperature purification step in step 1 is: putting the sample after chemical cleaning into an ultrahigh vacuum system for heating for 15-60 minutes, wherein the heating temperature is 550-650 ℃, and the vacuum degree of the ultrahigh vacuum system is not lower than 10 -7 Of the order of Pa.
4. The activation method for improving quantum efficiency of GaAs photocathode according to claim 1, wherein step 2, step 3, step 4, step 5, step 6 and step 7 are all performed in an ultra-high vacuum system.
5. The activation method for improving the quantum efficiency of gallium arsenide photocathode according to claim 1, wherein the cesium source and the oxygen source in step 2, step 3, step 4, step 5 and step 6 are all solid state sources packaged by nickel tube.
6. The activation method for improving quantum efficiency of gallium arsenide photocathode according to claim 1, wherein the fluorine source in step 7 is a gaseous source, and the gas inlet method is: the opening and closing number of the micro air inlet valve can be adjusted electrically to control the inlet of the ultra-vacuum system NF 3 The intake air amount.
7. The activation method for improving the quantum efficiency of gallium arsenide photocathode according to claim 1, wherein the first threshold range is 50% to 90% of the peak current.
8. The activation method for improving the quantum efficiency of gallium arsenide photocathode according to claim 1, wherein the second threshold is in the range of 100-110% of the previous peak current.
9. The activation method for improving the quantum efficiency of gallium arsenide photocathode according to claim 1, wherein the third threshold range is 50% to 90% of the peak current.
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CN111584326B (en) * 2020-04-29 2022-09-27 南京理工大学 Activation method for improving quantum efficiency of InGaAs photocathode
CN112885684B (en) * 2021-02-03 2022-09-27 南京理工大学 Activation method for improving stability of GaAs photocathode

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CN110706989A (en) * 2019-10-30 2020-01-17 南京工程学院 Cs/NF3 activation method for improving stability of GaAs photocathode

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