CN109755081B - Automatic antimony current regulation and control method for manufacturing high-performance alkali metal antimonide photocathode - Google Patents
Automatic antimony current regulation and control method for manufacturing high-performance alkali metal antimonide photocathode Download PDFInfo
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Abstract
The invention provides an antimony current automatic regulation and control method for manufacturing a high-performance alkali metal antimonide photocathode, which comprises the following steps: alkali metal evaporation, antimony evaporation, photocurrent curve fitting and prediction, photocurrent curve slope judgment and antimony evaporation current adjustment. The method is suitable for the stage of simultaneously evaporating alkali metal and antimony, and comprises the steps of firstly fitting a photocurrent curve, then predicting whether the slope of the photocurrent curve in a future fixed time range reaches an expected value, then judging whether the slope of the actual photocurrent curve reaches the expected value, if any one of the slope of the actual photocurrent curve and the slope of the actual photocurrent curve reaches the expected value, judging whether the slope of the actual photocurrent curve reaches a specified value, finally adjusting the antimony evaporation current according to judgment conditions, and repeating the process until the slope of the photocurrent curve reaches a specified angle. The invention can solve the problem of imbalance of the ratio of alkali metal to antimony caused by uncontrollable antimony output in the process of manufacturing the alkali metal antimonide photocathode and improve the photoelectric emission performance of the alkali metal antimonide photocathode.
Description
Technical Field
The invention relates to the technical field of vacuum photoelectric detectors, in particular to a method for automatically regulating and controlling antimony current for manufacturing a high-performance alkali metal antimonide photoelectric cathode.
Background
The vacuum photoelectric detector is an electronic device for converting optical signals into electric signals, can effectively detect weak light, and is widely applied to the research fields of infinitesimal light detection, photon detection, chemiluminescence, bioluminescence and the like. Including micro-optical image intensifiers, photomultiplier tubes, streak tubes, and the like. The core part of the vacuum photoelectric detection device is a photocathode, the performance of the photocathode directly influences the performance of the whole device, and the main performance parameter of the vacuum photoelectric detection device is quantum efficiency, namely the quantity of electrons emitted by the photocathode when receiving 100 photons. The currently commonly used alkali antimonides include various monobasic, dibasic and polybase antimonides with potassium, sodium, lithium, cesium as the alkali metal material, including: k3Sb、Cs3Sb、K2CsSb、K2NaSb，K2L iSb and KNaCsSb, and the like.
The preparation method of the alkali metal antimonide photocathode is mainly distinguished according to whether alkali metal and antimony are evaporated at the same time, and comprises an independent evaporation method and a common evaporation method, and the preparation method is a preparation process aiming at vacuum evaporation whether the alkali metal antimonide photocathode is evaporated independently or together. A combined photocurrent monitoring and reflectivity monitoring K as set forth in the patent application No. 201610856127.22The CsSb photocathode preparation method adopts a preparation flow of bottom potassium, simultaneous evaporation of potassium and antimony and final cesium feeding; na is proposed in patent application No. 201510438585.X2Method for preparing CsSb photocathode by adoptingThe preparation process of adding sodium by steaming cesium antimony, adding sodium by steaming cesium antimony and adding antimony by steaming antimony; the patent of application No. 201710743036.2 firstly applies the built-in electric field diffusion theory of semiconductor carriers to the preparation of the double-alkali cathode, namely, a built-in electric field exists in the energy band bending region, which is beneficial to the electron transportation in the material to the surface.
As can be seen from the above patents, the alkali metal antimonide photocathodes currently use the co-evaporation of alkali metal and antimony, rather than the separate evaporation. This is because the co-evaporation can realize the control of the plating film composition by adjusting the ratio of the alkali metal and antimony, thereby effectively providing the quantum efficiency of the photocathode. Two schemes can be adopted for common evaporation, the first scheme is that a large number of tests are carried out to grope out fixed time and fixed evaporation capacity; the second method is to adjust the evaporation amount in real time according to the change of the photocurrent curve. The first scheme is suitable for the premise that the vacuum atmosphere, the alkali metal evaporation source and the antimony evaporation source have high consistency, otherwise, the second scheme has universality and is easier to manufacture a photoelectric cathode with high performance. Therefore, the amount of evaporation of the alkali metal is solidified during co-evaporation, and how to effectively control the amount of evaporation of antimony according to the trend of the photocurrent curve becomes a key factor affecting the performance of the cathode.
Disclosure of Invention
The invention aims to provide an antimony current automatic regulation and control method for manufacturing a high-performance alkali metal antimonide photocathode.
In order to achieve the above object, the present invention provides an antimony current automatic control method for high-performance alkali metal antimonide photocathode fabrication, which is characterized in that the method comprises:
alkali metal evaporation, namely stably separating out alkali metal with fixed evaporation capacity by adjusting alkali metal evaporation current;
antimony evaporation, namely degassing antimony, and adjusting antimony current to a precipitation value;
fitting and predicting photocurrent curve, fitting the trend of the collected photocurrent curve, and predicting the slope of the subsequent photocurrent curveα；
The slope of the photocurrent curve is judged,firstly, the slope of the predicted photocurrent curve is judgedαWhether the slope reaches the expected value or not, if so, continuing to judge the actual photocurrent curve slope after waitingβIf the expected value is reached, otherwise, immediately increasing the antimony current;
if the actual photocurrent curve slopeβWhen the expected value is reached, the slope of the actual photocurrent curve is continuously judged after waitingβIf not, the slope of the actual photocurrent curve is immediately judgedβWhether it is a positive value:
if the actual photocurrent curve slopeβIf the actual photocurrent curve slope is positive, continuously judging whether the actual photocurrent curve slope is present after waitingβIf the expected value is reached, otherwise, immediately increasing the antimony current;
if the actual photocurrent curve slope is continuously judgedβWhen the expected value is reached, the slope of the actual photocurrent curve is judged after waitingβIf the value reaches the specified value, otherwise, the antimony current is increased immediately;
if the slope of the actual photocurrent curve is judgedβIf the value reaches the specified value, the antimony adjusting stage is ended, otherwise, the antimony current is increased immediately;
adjusting antimony current by evaporation according to the slope of predicted photocurrent curveαWhether the desired value is reached, and the actual photocurrent curve slopeβThe antimony current is adjusted for deviations from the desired and specified values.
Further, the alkali metal vapor deposition means that an alkali metal atmosphere is formed in a vacuum environment before antimony is evaporated, and the sign of the end of the alkali metal vapor deposition is that the photocurrent starts to fall back after rising to the maximum value.
Further, fitting is carried out on the photocurrent curve, and a polynomial fitting algorithm or a least square method curve fitting algorithm is adopted.
Further, the fitted photocurrent curve was trended at a predetermined time of △ T1The range is 0-5 min.
Further, the predicted photocurrent curve slope is at the predetermined time △ T2The range is 0-2 min.
Further, for the set photocurrent regulating gear, the expected value and the specified value should be fixed values or fixed range values, and the specified value is faster than the photocurrent rising rate corresponding to the expected value.
Further, the photocurrent regulation gear includes 16 gears of 1mA, 500 μ a, 200 μ a, 100 μ a, 50 μ a, 20 μ a, 10 μ a, 5 μ a, 2 μ a, 1 μ a, 500 nA, 200 nA, 100 nA, 50 nA, 20 nA, and 10 nA.
Further, the predicted photocurrent curve slopeαAnd actual photocurrent curve slopeβAnd selecting the minimum photocurrent regulation gear where the light current regulation gear can be positioned.
Further, the slope of the curve for the predicted photocurrentαAnd actual photocurrent curve slopeβThe increased antimony current that does not reach the desired value needs to be adjusted more than the increased antimony current that does not reach the specified value.
Further, the slope of the curve for the actual photocurrentβIn the case where the desired or specified value is not reached, the adjustment increases the antimony current in proportion to the angular deviation.
From the above technical solutions, the foregoing implementation method of the present invention has significant advantages in that:
1) because the method of adjusting the evaporation capacity in real time according to the change of a photocurrent curve is adopted in the common evaporation of alkali metal and antimony, the component proportion control can be realized;
2) the change of an actual photocurrent curve is referred to, and the change of a predicted photocurrent theoretical curve is referred to, so that the judgment content increased in the antimony regulation process enables the finished antimony current evaporation judgment to be more accurate;
3) the deviation comparison is carried out on the actual photocurrent curve, the expected value and the theoretical value, and the antimony current to be regulated is more accurate due to the increased judgment condition in the antimony regulating process;
4) the high-performance alkali metal antimonide photocathode antimony current regulation and control method is established on the basis of an automatic regulation and control system, has low error rate and high repeatability relative to manual antimony regulation, and the prepared photocathode is used for detecting K in a large-size photomultiplier by using mesogens2The quantum efficiency of the CsSb photocathode at 410 nm reaches 35 percentAbove, the effect is obviously superior to the existing manual regulation and control effect.
Drawings
FIG. 1 is a flow diagram of antimony current autoregulation for alkali antimonide photocathodes according to certain embodiments of the present invention.
FIG. 2 is an antimony current automatic regulation system for an alkali antimonide photocathode according to some embodiments of the present invention, illustrating cathode fabrication parameters and photocurrent tap maps on a regulatory software interface.
FIG. 3 is a photocurrent curve for antimony current autoregulation of alkali antimonide photocathodes, illustrating judgment, in accordance with certain embodiments of the present inventionβThe photocurrent versus theoretical curve for the expected value was reached.
FIG. 4 is a plot of photocurrent, graphically determined for automatic regulation of antimony current for an alkali antimonide photocathode, in accordance with certain embodiments of the present inventionβThe photocurrent versus theoretical curve for the specified value was reached.
Figure 5 is a plot of photocurrent versus theory for automatic regulation of antimony current for an alkali antimonide photocathode, according to some embodiments of the present invention, illustrating the photocurrent after antimony regulation is complete.
Fig. 6 is a comparison of the quantum efficiency distribution of a sample tube prepared by the automatic antimony quantity control method for an alkali antimonide photocathode according to some embodiments of the present invention and the quantum efficiency distribution prepared by manually controlling antimony.
Detailed Description
FIG. 1 is a flow diagram of antimony current autoregulation for alkali antimonide photocathodes according to certain embodiments of the present invention. The method comprises the following steps: adding antimony 101, predictionαWhether or not the desired value 102 is reached is judgedβWhether or not the expected value 103 is reached is judgedβWhether it is a positive value 104 or not, and a judgmentβWhether or not the expected value 105 is reached is judgedβWhether the specified value 106 has been reached and end tuning 107.
Generally, the method for automatically regulating and controlling the antimony current of the alkali metal antimonide photocathode comprises the following steps: alkali metal evaporation, antimony evaporation, photocurrent curve fitting and prediction, photocurrent curve slope judgment and antimony current evaporation regulation according to the photocurrent curve slope judgment result.
The alkali metal vapor deposition means that an alkali metal is stably precipitated at a fixed amount of evaporation by adjusting an alkali metal evaporation current.
And (4) antimony evaporation, namely degassing antimony, and adjusting the current of the antimony to a precipitation value.
Fitting and predicting photocurrent curve, fitting the trend of the collected photocurrent curve, and predicting the slope of the subsequent photocurrent curveα。
The photocurrent curve slope judgment specifically comprises:
firstly, the slope of the predicted photocurrent curve is judgedαWhether the slope reaches the expected value or not, if so, continuing to judge the actual photocurrent curve slope after waitingβIf the expected value is reached, otherwise, immediately increasing the antimony current;
if the actual photocurrent curve slopeβWhen the expected value is reached, the slope of the actual photocurrent curve is continuously judged after waitingβIf not, the slope of the actual photocurrent curve is immediately judgedβWhether it is a positive value:
if the actual photocurrent curve slopeβIf the actual photocurrent curve slope is positive, continuously judging whether the actual photocurrent curve slope is present after waitingβIf the expected value is reached, otherwise, immediately increasing the antimony current;
if the actual photocurrent curve slope is continuously judgedβWhen the expected value is reached, the slope of the actual photocurrent curve is judged after waitingβIf the value reaches the specified value, otherwise, the antimony current is increased immediately;
if the slope of the actual photocurrent curve is judgedβWhen the specified value is reached, the antimony regulating stage is ended, otherwise, the antimony current is increased immediately.
Adjusting antimony current by evaporation according to the slope of predicted photocurrent curveαWhether the desired value is reached, and the actual photocurrent curve slopeβThe antimony current is adjusted for deviations from the desired and specified values.
Combining the flow shown in FIG. 1, after adjusting the antimony current to the precipitation value, adding antimony 101 for a total of four stepsAntimony adding operation is respectivelyαAdding antimony after the expected value 102 is not reached, and judgingβAdding antimony after the value is not positive 104, judgingβAdding antimony and judging if the expected value 105 is not reachedβAntimony was added after the specified value of 106 was not reached.
According to an embodiment of the invention, for a 20 inch photomultiplier tube K2For the CsSb photocathode, the antimony current increment of the four antimony adding operations is respectively 0.4A, 0.2A, 0.5A and 0.3A, and the corresponding waiting time is 2.0 min. And the above-mentioned judgmentβAdding antimony and judging if the expected value 105 is not reachedβThe increased antimony currents 0.5A and 0.3A after not reaching the specified value of 106 are only base amounts, which are also subject toβThe difference from the expected value and the specified value.
PredictionαAnd in the step of whether the current reaches the expected value 102, automatically adjusting the gear by the curve to ensure that the displayed photocurrent is larger than 4.5 grids in the coordinate, and otherwise, reducing the current by 1 gear for display. In conjunction with the cathode manufacturing parameters and photocurrent shift map on the interface of the control software given in fig. 2, it can be seen that the shift positions include 16 shift positions of 1mA, 500 μ a, 200 μ a, 100 μ a, 50 μ a, 20 μ a, 10 μ a, 5 μ a, 2 μ a, 1 μ a, 500 nA, 200 nA, 100 nA, 50 nA, 20 nA, and 10 nA. And each gear only displays 10 grids in the photocurrent coordinate system. For example, when the photocurrent tap was 5 μ a, 1 bar represents 0.5 μ a; when the photocurrent shift was 100 nA, 1 bar represents 10 nA. According to the display method, when the photocurrent is in the 10 th grid, the gear can be automatically increased by 1, and the photocurrent can also automatically fall back to the 5 th grid; when the photocurrent is less than 4.5 grids, the gear position is automatically reduced by 1, and the photocurrent is automatically increased to twice the grid number. In addition, other cathode manufacturing parameters are also displayed on the regulation software interface, including: photocurrent, leakage current, current slope, reflectivity, and reflectivity slope.
Based on the gear change principle, the photocurrent corresponding to the expected value should stay in the minimum gear where the photocurrent can be located. The expected value is defined as the angle between the slope of the photocurrent in the first quadrant of the coordinate system and the vertical, fixed range angle of 30 deg.. When in useαWhen the expected value is reached, the judgment is carried out after waiting for 1 minβWhether or not to reach the expectationA value of 103; otherwise whenαWhen this value is not reached, the antimony current is immediately increased by 0.4A, i.e. the step of adding antimony 101 is repeated.
Judgment ofβIn the step of detecting whether the desired value 103 is reached, the desired value is also 30 ° of the slope of the photocurrent in the first quadrant with respect to the vertical direction. When in useβWhen the expected value is reached, waiting for 5 min and judgingβWhether the specified value 106 is reached; otherwise whenβWhen the expected value is not reached, immediately judgingβWhether positive 104.
Judgment ofβIn the step of determining whether the desired value 105 is reached, the desired value is also 30 ° of the slope of the photocurrent in the first quadrant with respect to the vertical direction. When in useβWhen the expected value is reached, waiting for 5 min and judgingβWhether the specified value 106 is reached; otherwise whenβWhen the desired value is not reached, the control unit,βfor every 5 ° decrease, the antimony current increases by 0.05A and the latency increases by 0.5 min, as shown in table 1.
TABLE 1 whenβIncrease in Sb Current without reaching the desired value
| β | 0°~5° | 5°~10° | 10°~15° | 15°~20° | 20°~25° | 25°~30° |
| Evaporation current of Sb | 0.75 A | 0.7 A | 0.65 A | 0.6 A | 0.55 A | 0.5 A |
| Waiting time | 4.5 |
4 min | 3.5 |
3 min | 2.5 |
2 min |
Judgment ofβAnd whether a specified value 106 is reached, wherein the specified value is defined as an included angle of 45 degrees between the slope of the photocurrent in the first quadrant of the coordinate system and the vertical direction. When in useβWhen the specified value is reached, waiting for 2 min and finishing antimony regulation 107; otherwise whenβWhen the value is not reached, the value is,βfor every 5 ° decrease, the antimony current increases by 0.05A and the latency increases by 0.5 min, as shown in table 2.
TABLE 2 whenβSb current increase when the specified value is not reached
| β | 25°~30° | 30°~35° | 35°~40° | 40°~45° |
| Evaporation current of Sb | 0.45 A | 0.4 A | 0.35 A | 0.3 A |
| Waiting time | 3.5 |
3 min | 2.5 |
2 min |
FIG. 3 is a photocurrent curve for antimony current autoregulation of alkali antimonide photocathodes, illustrating judgment, in accordance with certain embodiments of the present inventionβThe photocurrent versus theoretical curve for the expected value was reached. Wherein, the curve 1 is an actual photocurrent curve, and the curve 2 is a theoretical curve. Adding antimony at 6.5 min, and performing theoretical fitting on the curve after adding antimony for a certain period△T 1Is 2 min, time predicted△T 2Is 1 min. In the end of this process,α37 deg. has reached the desired value (30 deg.),β13 ° did not reach the desired value (30 °), and therefore, the photocurrent was curvedThe line should continue to add antimony with an antimony current of 0.65A and a waiting time of 3.5 min.
FIG. 4 is a plot of photocurrent, graphically determined for automatic regulation of antimony current for an alkali antimonide photocathode, in accordance with certain embodiments of the present inventionβThe photocurrent versus theoretical curve for the specified value was reached. Wherein, the curve 1 is an actual photocurrent curve, and the curve 2 is a theoretical curve. Adding antimony at 8.3 min, and performing theoretical fitting on the curve after adding antimony for fitting time△T 1Is 2 min, time predicted△T 2Is 1 min. In the end of this process,αis 56 deg. has reached the desired value (30 deg.),βthe specified value (45 °) has been reached for 58 °, so the photocurrent curve can end up tuning the antimony.
Figure 5 is a plot of photocurrent, as measured by actual photocurrent versus theoretical after antimony trimming, for automatic antimony current regulation of an alkali antimonide photocathode according to certain embodiments of the present invention. Wherein, the curve 1 is an actual photocurrent curve, and the curve 2 is a theoretical curve. Adding antimony in 5 min, and theoretically fitting the curve with antimony for a certain time△ T 1Is 3 min, time predicted△T 2Is 1 min. In the end of this process,αis 66 deg. has reached the desired value (30 deg.),βwhen the antimony adjustment is finished after the specified value (45 ℃) is reached for 74 degrees, the photocurrent starts to stably rise, and when the photocurrent rises to the 10 th grid, the shift position is automatically increased by 1 step, and the gear shifting is carried out for 3 times in total in the graph 5.
Fig. 6 is a comparison of the quantum efficiency distribution of a sample tube prepared by the automatic antimony quantity control method for an alkali antimonide photocathode according to some embodiments of the present invention and the quantum efficiency distribution prepared by manually controlling antimony. Both methods sample data volumes greater than 200. It can be seen that the sample tubes prepared by the method for automatically regulating and controlling the amount of antimony are superior to the sample tubes prepared by the method for manually regulating and controlling the amount of antimony in the ratio that the quantum efficiency is more than 27%, which shows that the method for automatically regulating and controlling the amount of antimony for the alkali metal antimonide photocathode according to some embodiments of the present invention has an obvious effect on improving the quantum efficiency of the cathode.
Claims (10)
1. An antimony current automatic regulation and control method for manufacturing a high-performance alkali metal antimonide photocathode is characterized by comprising the following steps:
alkali metal evaporation, namely stably separating out alkali metal with fixed evaporation capacity by adjusting alkali metal evaporation current;
antimony evaporation, namely degassing antimony, and adjusting antimony current to a precipitation value;
fitting and predicting the photocurrent curve, fitting the trend of the collected photocurrent curve, and obtaining the slope of the predicted photocurrent curveα；
The slope of the photocurrent curve is judged by first judging the slope of the predicted photocurrent curveαWhether the slope reaches the expected value or not, if so, continuing to judge the actual photocurrent curve slope after waitingβIf the expected value is reached, otherwise, immediately increasing the antimony current;
if the actual photocurrent curve slopeβWhen the expected value is reached, the slope of the actual photocurrent curve is continuously judged after waitingβIf not, the slope of the actual photocurrent curve is immediately judgedβWhether it is a positive value:
if the actual photocurrent curve slopeβIf the actual photocurrent curve slope is positive, continuously judging whether the actual photocurrent curve slope is present after waitingβIf the expected value is reached, otherwise, immediately increasing the antimony current;
if the actual photocurrent curve slope is continuously judgedβWhen the expected value is reached, the slope of the actual photocurrent curve is judged after waitingβIf the value reaches the specified value, otherwise, the antimony current is increased immediately;
if the slope of the actual photocurrent curve is judgedβIf the value reaches the specified value, the antimony adjusting stage is ended, otherwise, the antimony current is increased immediately;
adjusting antimony current by evaporation according to the slope of predicted photocurrent curveαWhether the desired value is reached, and the actual photocurrent curve slopeβThe antimony current is adjusted for deviations from the desired and specified values.
2. The method as claimed in claim 1, wherein the alkali metal evaporation is performed by forming an alkali metal atmosphere in a vacuum environment before evaporating antimony, and the mark of the completion of the alkali metal evaporation is that a photocurrent starts to fall back after rising to a maximum value.
3. The method of claim 1, wherein the photocurrent curve is fitted using a polynomial fitting or least squares curve fitting algorithm.
4. The method as claimed in claim 1, wherein the fitted photocurrent curve trend is △ T at a predetermined time1The range is 0-5 min.
5. The method as claimed in claim 1, wherein the slope of the predicted photocurrent curve is △ T at a predetermined time2The range is 0-2 min.
6. The method as claimed in claim 1, wherein the expected value and the specified value are fixed values or fixed range values for the photocurrent control gear, and the increase rate of the photocurrent is faster than the expected value.
7. The method for automatically regulating and controlling the antimony current for manufacturing the high-performance alkali metal antimonide photocathode as claimed in claim 6, wherein the photocurrent regulation gear comprises 16 gears of 1mA, 500 μ A, 200 μ A, 100 μ A, 50 μ A, 20 μ A, 10 μ A, 5 μ A, 2 μ A, 1 μ A, 500 nA, 200 nA, 100 nA, 50 nA, 20 nA and 10 nA.
8. According to claim6 or 7, the antimony current automatic regulation and control method for the high-performance alkali metal antimonide photocathode is characterized in that the slope of the predicted photocurrent curveαAnd actual photocurrent curve slopeβAnd selecting the minimum photocurrent regulation gear where the light current regulation gear can be positioned.
9. The method of claim 1, wherein the method comprises predicting the slope of the photocurrent curveαAnd actual photocurrent curve slopeβThe increased antimony current that does not reach the desired value needs to be adjusted more than the increased antimony current that does not reach the specified value.
10. The method as claimed in claim 1, wherein the slope of the actual photocurrent curve is determined by the method of automatic control of the antimony current for the fabrication of high performance alkali antimonide photocathodesβIn the case where the desired or specified value is not reached, the adjustment increases the antimony current in proportion to the angular deviation.
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| RU2594986C1 (en) * | 2015-04-17 | 2016-08-20 | Общество с ограниченной ответственностью Владикавказский Технологический центр "Баспик" (ООО ВТЦ "Баспик") | Method for electronic degassing microchannel plate during manufacture of vacuum device |
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