CN111584326B - Activation method for improving quantum efficiency of InGaAs photocathode - Google Patents
Activation method for improving quantum efficiency of InGaAs photocathode Download PDFInfo
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- CN111584326B CN111584326B CN202010358213.7A CN202010358213A CN111584326B CN 111584326 B CN111584326 B CN 111584326B CN 202010358213 A CN202010358213 A CN 202010358213A CN 111584326 B CN111584326 B CN 111584326B
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Abstract
The invention discloses an activation method for improving quantum efficiency of an InGaAs photocathode, which comprises cesium activation, oxygen activation, cesium activation and NF 3 Two activations of activation are specifically: pair InGaAs performing high temperature purification on the photocathode; the cesium source is started, when the photoelectric current is reduced to 50% -85% of the peak current, the oxygen source is started, the cesium source is kept started, and when the photoelectric current reaches the peak value again, the oxygen source is closed; performing secondary high-temperature purification on the InGaAs photocathode; opening the cesium source, and opening NF when the photoelectric current is reduced to 50-85% of the peak current 3 The gas inlet valve enables NF3 gas to enter the activation cavity and keeps the cesium source open, and when the rising rate of the photocurrent curve is less than 0.2 muA/min, the NF is closed 3 And an air inlet valve for closing the cesium source. The invention can obtain the InGaAs photocathode with higher quantum efficiency.
Description
Technical Field
The invention belongs to an InGaAs photocathode activation technology, in particular to an activation method for improving quantum efficiency of an InGaAs photocathode.
Background
InGaAs is a ternary semiconductor material widely applied in the field of low-light-level night vision detection imaging, and the surface of InGaAs is appropriately sensitized to generate a Negative Electron Affinity (NEA) surface. The InGaAs photocathode has good spectral response in a near-infrared region of 1-3 mu m, and is of great significance in preparing high-performance near-infrared low-light-level night vision devices and systems. In the current photocathode application, the low quantum efficiency of the near-infrared band of the InGaAs photocathode is a technical problem, and the practical development of the cathode is hindered. Therefore, how to reduce the surface electron affinity of the InGaAs cathode to prepare an InGaAs photocathode with high quantum efficiency becomes crucial. The activation process under the ultrahigh vacuum environment determines the performance of the NEA InGaAs photocathode to a great extent, and factors such as the types of the active source materials, the alternating sequence of the active sources, the flow ratio of the active source gases and the like in the activation process have great influence on the quantum efficiency of the photocathode.
In the current two-step activation process, the most common is cesium oxygen high and low temperature two-step activation process. In an ultrahigh vacuum environment, firstly, carrying out first cesium-oxygen alternative activation on the surface of the InGaAs photocathode subjected to chemical cleaning and high-temperature purification, and then carrying out second cesium-oxygen alternative activation on the surface of the InGaAs photocathode subjected to low-temperature purification. During activation, a white light source is adopted to irradiate the surface of the cathode, and cesium oxygen is activated to reduce the potential barrier on the surface of the InGaAs photocathode, so that the negative electron affinity photocathode is obtained. However, the quantum efficiency of the InGaAs photocathode obtained by the high-temperature and low-temperature two-step activation method is low, and the improvement of the quantum efficiency of the second activation is smaller than that of the first activation.
Disclosure of Invention
The invention aims to provide an activation method for improving quantum efficiency of an InGaAs photocathode.
The technical solution for realizing the purpose of the invention is as follows: an activation method for improving quantum efficiency of an InGaAs photocathode comprises the following specific steps:
step 3, when the photocurrent drops to a set threshold range after reaching a peak value, starting an oxygen source, keeping the cesium source started, converting the photocurrent into the photocurrent to rise, and closing the oxygen source when the photocurrent reaches the peak value again;
step 5, performing secondary high-temperature purification on the InGaAs photocathode;
and 7, when the photoelectric current falls to a set threshold range, enabling NF3 gas to enter an activation cavity of the ultrahigh vacuum system, keeping the cesium source on, gradually increasing the photoelectric current, and when the rising rate of a photoelectric current curve is less than 0.2 muA/min, closing the NF 3 And (4) an air inlet valve, a cesium source is closed, and the whole activation process is finished.
Preferably, the chemical cleaning method in step 1 specifically comprises:
removing grease on the surface of the InGaAs photocathode;
placing the InGaAs photocathode into a mixed solution of hydrochloric acid and isopropanol for etching;
and washing the InGaAs photocathode by deionized water.
Preferably, the high-temperature purification step in step 1 is: and (3) putting the sample subjected to chemical cleaning into an ultrahigh vacuum system for heating for 15-40 minutes at the heating temperature of 550-650 ℃.
Preferably, the cesium source and the oxygen source are both solid sources packaged by nickel tubes, the cesium source is a solid source for reducing cesium chromate by using zirconium-aluminum alloy powder, the oxygen source is a solid source of barium peroxide, and NF is 3 The source is a high purity gaseous source.
Preferably, the vacuum degree of the ultrahigh vacuum system is not lower than 10 -7 In the order of Pa.
Preferably, the set threshold range in steps 3 and 5 is 50% to 85% of the peak current.
Preferably, the specific method for performing the second high-temperature purification on the InGaAs photocathode is the same as that for the first high-temperature purification.
Compared with the prior art, the invention has the remarkable advantages that:
1. the InGaAs photocathode activated by the method has higher quantum efficiency;
2. the operation method is simple, the heating and purifying processes before the two times of activation are the same, and the method is easy to realize;
3. the invention has less operation steps, the first activation uses the traditional Cs and O activation process, and the second activation uses Cs and NF 3 The method has few activation experimental steps, can successfully activate without repeated alternation, and obviously improves the quantum efficiency.
Drawings
FIG. 1 is a flow chart of the present invention.
Fig. 2 is a photocurrent curve of a first cesium oxygen activated InGaAs photocathode of the present invention.
FIG. 3 shows a second cesium, NF reaction of the present invention 3 Photocurrent curves for the activated InGaAs photocathode.
Fig. 4 is a graph showing the quantum efficiency comparison of the InGaAs photocathodes after the first and second activations of the present invention.
Detailed Description
As shown in FIG. 1, an activation method for improving quantum efficiency of InGaAs photocathode comprises activating cesium and oxygen source, and activating cesium and NF 3 Activating twice, and specifically comprises the following steps:
the chemical cleaning method comprises the following steps: firstly removing grease on the surface of a sample, then placing the sample into a mixed solution of hydrochloric acid and isopropanol for etching, and finally washing the sample clean by deionized water.
The high-temperature purification step is as follows: putting the sample after chemical cleaning into an ultrahigh vacuum system for heating for 15-40 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.
step 3, when the photoelectric current is reduced to 50% -85% of the peak current, starting the oxygen source, keeping the cesium source started, converting the photoelectric current to rise, and when the photoelectric current reaches the peak value again, closing the oxygen source, wherein the photoelectric current rises slightly and then falls immediately;
step 5, performing secondary high-temperature purification on the InGaAs photocathode;
step 7, when the photoelectric current is reduced to 50% -85% of the peak current, the NF is started 3 An air inlet valve is used for enabling NF3 gas to enter the activation cavity of the ultrahigh vacuum system, the cesium source is kept opened, the photocurrent rises gradually, and when the rising rate of the photocurrent curve is less than 0.2 muA/min, the NF is closed 3 And (4) an air inlet valve, a cesium source is closed, and the whole activation process is finished.
The above reactions are all carried out in an ultrahigh vacuum system, and the vacuum degree of the ultrahigh vacuum system is not less than 10 -7 Of the order of Pa. During the activation process, a tungsten halogen lamp is used to vertically irradiate the cathode surface. The cesium source and the oxygen source are solid sources packaged by nickel tubes, the cesium source is a solid source of cesium chromate reduced by aluminum zirconium alloy powder, the oxygen source is a solid source of barium peroxide, and NF 3 The source is a high purity gaseous source.
The present invention is further illustrated by the following examples.
Example 1
An activation method for improving quantum efficiency of an InGaAs photocathode specifically comprises the following steps:
and chemically cleaning and purifying the InGaAs photocathode material at high temperature.
The chemical cleaning step is that firstly, grease on the surface of the sample is removed, then the sample is put into a mixed solution of hydrochloric acid and isopropanol for etching, and finally the sample is washed clean by deionized water.
The high-temperature purification step is to send the sample to a vacuum degree of not less than 10 -7 In an ultra-high vacuum system with Pa magnitude order, the heating temperature is 550 ℃ and the heating time is 30 minutes. After the sample had cooled naturally to room temperature, the sample was brought to the activation site and cesium oxygen activation was initiated.
When the cesium source is activated, a white light source of a halogen tungsten lamp is used for vertically irradiating the cathode surface, and the on or off of the cesium source and an oxygen source is determined by measuring and collecting photocurrent generated by the cathode in real time. By regulating the outsideThe current of the current source is connected to control the discharge amount of the cesium source and the oxygen source during electrifying. Because the outgassing amount of cesium oxygen sources from different sources may be different, the current of the cesium oxygen sources used in the activation process will also be different, and a suitable cesium-oxygen ratio should be obtained by an experimental method after replacing the cesium oxygen sources, in this example, the current of the cesium source in the activation process is 4.1A, the current of the oxygen source is 1.3A, and NF is 1.3A 3 Is controlled by an intake valve. The activation steps are as follows:
1. carrying out chemical cleaning and first high-temperature purification on the InGaAs photocathode;
2. the cesium source is turned on, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
3. when the photoelectric current is reduced to 50% of the peak current, the oxygen source is started, the cesium source is kept started, the photoelectric current is converted to rise, when the photoelectric current reaches the peak value again, the oxygen source is closed, and the photoelectric current firstly rises in a small range and then immediately falls;
4. repeating the step 3 until the photocurrent reaches the maximum peak value, successively closing the oxygen source and the cesium source, and ending the first activation process;
5. performing secondary high-temperature purification on the InGaAs photocathode;
6. the cesium source is turned on, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
7. NF was turned on when the photocurrent dropped to 50% of the peak current 3 The gas inlet valve enables NF3 gas to enter the activation cavity, the cesium source is kept open, the photocurrent rises gradually, and when the rising rate of the photocurrent curve is less than 0.2 mu A/min, the NF is closed 3 And (4) an air inlet valve, a cesium source is closed, and the whole activation process is finished.
Example 2
An activation method for improving quantum efficiency of an InGaAs photocathode specifically comprises the following steps:
and chemically cleaning and purifying the InGaAs photocathode material at high temperature.
The chemical cleaning step is that firstly removing grease on the surface of the sample, then placing the sample into a mixed solution of hydrochloric acid and isopropanol for etching, and finally washing the sample clean by deionized water.
The high-temperature purification step is to send the sample to a vacuum degree of not less than 10 -7 In an ultra-high vacuum system of Pa magnitude, the heating temperature is 550 ℃ and the heating time is 30 minutes. After the sample had cooled naturally to room temperature, the sample was brought to the activation site and cesium oxygen activation was initiated.
When the cesium source is activated, a white light source of a halogen tungsten lamp is used for vertically irradiating the cathode surface, and the on or off of the cesium source and an oxygen source is determined by measuring and collecting photocurrent generated by the cathode in real time. The size of the electrification and deflation amount of the cesium source and the oxygen source is controlled by adjusting the current of the external current source. Since the outgassing amount of cesium oxygen sources from different sources may be different, the current of the cesium oxygen source used in the activation process will also be different, and a suitable cesium-oxygen ratio should be obtained by an experimental method after replacing the cesium oxygen source, in this example, the current of the cesium source during the activation process is 4.1A, the current of the oxygen source is 1.3A, and NF is 1.3A 3 Is controlled by an intake valve. The activation steps are as follows:
1. carrying out chemical cleaning and first high-temperature purification on the InGaAs photocathode;
2. the cesium source is turned on, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
3. when the photoelectric current is reduced to 70% of the peak current, the oxygen source is started, the cesium source is kept started, the photoelectric current is converted to rise, when the photoelectric current reaches the peak value again, the oxygen source is closed, and the photoelectric current firstly rises in a small range and then immediately falls;
4. repeating the step 3 until the photocurrent reaches the maximum peak value, successively closing the oxygen source and the cesium source, and ending the first activation process;
5. performing secondary high-temperature purification on the InGaAs photocathode;
6. the cesium source is turned on, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
7. NF was turned on when the photocurrent dropped to 70% of the peak current 3 Inlet valve to NF 3 Gas enters the activation cavity and keeps the cesium source open, the photocurrent rises gradually, and when the rising rate of the photocurrent curve is less than 0.2 muA/min, the NF is closed 3 And (4) an air inlet valve, a cesium source is closed, and the whole activation process is finished.
Example 3
An activation method for improving quantum efficiency of an InGaAs photocathode specifically comprises the following steps:
and chemically cleaning and purifying the InGaAs photocathode material at high temperature.
The chemical cleaning step is that firstly, grease on the surface of the sample is removed, then the sample is put into a mixed solution of hydrochloric acid and isopropanol for etching, and finally the sample is washed clean by deionized water.
The high-temperature purification step is to send the sample to a vacuum degree of not less than 10 -7 In an ultra-high vacuum system of Pa magnitude, the heating temperature is 550 ℃ and the heating time is 30 minutes. After the sample had cooled naturally to room temperature, the sample was brought to the activation site and cesium oxygen activation was initiated.
When the cesium source is activated, a white light source of a halogen tungsten lamp is used for vertically irradiating the cathode surface, and the on or off of the cesium source and an oxygen source is determined by measuring and collecting photocurrent generated by the cathode in real time. The size of the electrification and deflation amount of the cesium source and the oxygen source is controlled by adjusting the current of the external current source. Because the outgassing amount of cesium oxygen sources from different sources may be different, the current of the cesium oxygen sources used in the activation process will also be different, and a suitable cesium-oxygen ratio should be obtained by an experimental method after replacing the cesium oxygen sources, in this example, the current of the cesium source in the activation process is 4.1A, the current of the oxygen source is 1.3A, and NF is 1.3A 3 Is controlled by an intake valve. The activation steps are as follows:
1. carrying out chemical cleaning and first high-temperature purification on the InGaAs photocathode;
2. the cesium source is turned on, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
3. when the photoelectric current is reduced to 85% of the peak current, the oxygen source is started, the cesium source is kept started, the photoelectric current is converted to rise, when the photoelectric current reaches the peak value again, the oxygen source is closed, and the photoelectric current firstly rises in a small range and then immediately falls;
4. repeating the step 3 until the photocurrent reaches a maximum peak value, successively closing the oxygen source and the cesium source, and ending the first activation process;
5. performing secondary high-temperature purification on the InGaAs photocathode;
6. the cesium source is turned on, the photocurrent gradually rises, and the photocurrent drops after reaching a peak value;
7. when the photocurrent dropped to 85% of the peak current, NF was turned on 3 The gas inlet valve enables NF3 gas to enter the activation cavity, the cesium source is kept open, the photocurrent rises gradually, and when the rising rate of the photocurrent curve is less than 0.2 mu A/min, the NF is closed 3 And (4) an air inlet valve, a cesium source is closed, and the whole activation process is finished. FIG. 3 shows second cesium, NF of the present invention 3 The peak value of the photocurrent curve of the InGaAs photocathode is 11.526 muA when the InGaAs photocathode is activated. From FIGS. 2 and 3, it can be seen that cesium, NF, the second time 3 The maximum photocurrent for activating the InGaAs photocathode is greater than for the first cesium oxygen activation method. Fig. 4 is a graph comparing quantum efficiencies of the InGaAs photocathode after the first and second activations of the present invention, and it can be seen that the quantum efficiency of the InGaAs photocathode obtained by the second activation is higher than that of the first activation.
Claims (8)
1. An activation method for improving quantum efficiency of an InGaAs photocathode is characterized by comprising the following specific steps:
step 1, chemically cleaning an InGaAs photocathode, and placing the InGaAs photocathode into an ultrahigh vacuum system for first high-temperature purification;
step 2, starting a cesium source in an ultrahigh vacuum system, and vertically irradiating an InGaAs photocathode;
step 3, when the photocurrent drops to a set threshold range after reaching a peak value, starting an oxygen source, keeping the cesium source started, converting the photocurrent into the photocurrent to rise, and closing the oxygen source when the photocurrent reaches the peak value again;
step 4, repeating the step 3 until the photocurrent reaches the maximum peak value, successively closing the oxygen source and the cesium source, and ending the first activation process;
step 5, performing secondary high-temperature purification on the InGaAs photocathode;
step 6, the cesium source is turned on, the photocurrent rises gradually, and the photocurrent drops after reaching a peak value;
step 7, when the photoelectric current is reduced to a set threshold value range, enabling NF3Gas enters an activation cavity of the ultrahigh vacuum system, the cesium source is kept on, the photocurrent gradually rises, and the NF is turned off when the rising rate of the photocurrent curve is smaller than a set threshold value 3 And (4) an air inlet valve, a cesium source is closed, and the whole activation process is finished.
2. The activation method for improving quantum efficiency of an InGaAs photocathode according to claim 1, wherein the chemical cleaning method in step 1 specifically comprises:
removing grease on the surface of the InGaAs photocathode;
placing the InGaAs photocathode into a mixed solution of hydrochloric acid and isopropanol for etching;
and washing the InGaAs photocathode by deionized water.
3. The activation method for improving quantum efficiency of InGaAs photocathode according to claim 1, wherein the high temperature purification step in step 1 is: and (3) putting the sample subjected to chemical cleaning into an ultrahigh vacuum system for heating for 15-40 minutes at the heating temperature of 550-650 ℃.
4. The activation method for improving quantum efficiency of InGaAs photocathode according to claim 1, wherein said cesium source and oxygen source are both solid sources packaged by nickel tube, cesium source is solid source of cesium chromate reduced from zirconium aluminum alloy powder, oxygen source is solid source of barium peroxide, NF is solid source of barium peroxide 3 The source is a high purity gaseous source.
5. The activation method for improving quantum efficiency of InGaAs photocathode according to claim 1, wherein the degree of vacuum of said ultra-high vacuum system is not less than 10 -7 Of the order of Pa.
6. The activation method for improving quantum efficiency of InGaAs photocathode according to claim 1, wherein the threshold setting range in steps 3 and 5 is 50-85% of the peak current.
7. The activation method according to claim 1, wherein the InGaAs photocathode is subjected to a second high temperature cleaning in the same manner as the first high temperature cleaning.
8. The activation method for improving quantum efficiency of InGaAs photocathode according to claim 1, wherein the threshold value for the rising rate of photocurrent curve is set to be 0.2 μ A/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4477294A (en) * | 1981-05-06 | 1984-10-16 | The United States Of America As Represented By The Secretary Of The Army | Method of forming GaAs on Aly Ga1-y As transmission mode photocathodehode |
| CN109427518A (en) * | 2017-09-02 | 2019-03-05 | 南京理工大学 | A kind of Activiation method improving GaAs photocathode quantum efficiency and service life |
| CN111584327A (en) * | 2020-04-29 | 2020-08-25 | 南京理工大学 | Activation method for improving quantum efficiency of gallium arsenide photocathode |
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| US8017176B2 (en) * | 2008-01-25 | 2011-09-13 | Mulhollan Gregory A | Robust activation method for negative electron affinity photocathodes |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4477294A (en) * | 1981-05-06 | 1984-10-16 | The United States Of America As Represented By The Secretary Of The Army | Method of forming GaAs on Aly Ga1-y As transmission mode photocathodehode |
| CN109427518A (en) * | 2017-09-02 | 2019-03-05 | 南京理工大学 | A kind of Activiation method improving GaAs photocathode quantum efficiency and service life |
| CN111584327A (en) * | 2020-04-29 | 2020-08-25 | 南京理工大学 | Activation method for improving quantum efficiency of gallium arsenide photocathode |
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