CN109755081A - Antimony electric current method for automatically regulating for the production of performance alkali metal antimonide photocathode - Google Patents
Antimony electric current method for automatically regulating for the production of performance alkali metal antimonide photocathode Download PDFInfo
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Abstract
The present invention provides a kind of antimony electric current method for automatically regulating for the production of performance alkali metal antimonide photocathode, comprising: alkali metal vapor deposition, antimony vapor deposition, photocurrent curve fitting and prediction, the judgement of photocurrent curve slope and antimony evaporation current adjust.The stage is deposited simultaneously suitable for alkali metal and antimony, photocurrent curve is fitted first, then predict whether the photocurrent curve slope within the scope of the following set time reaches desired value, judge whether practical photocurrent curve slope reaches desired value again, if the two any one reach desired value, then judge whether practical photocurrent curve slope reaches designated value, the adjustment of antimony evaporation current is finally carried out according to Rule of judgment, repeating the above process terminates until photocurrent curve slope reaches specified angle.It can solve the problems, such as to improve alkali antimonide photocathode photoemission performance since the uncontrollable caused alkali metal of antimony output and antimony are out of proportion in alkali antimonide photocathode manufacturing process using the present invention.
Description
Technical field
The present invention relates to the preparations of Vacuum Photoelectric Detectors part technical field more particularly to cathode, in particular to one
Antimony electric current method for automatically regulating of the kind for the production of performance alkali metal antimonide photocathode.
Background technique
Vacuum Photoelectric Detectors part is the electronic device for converting optical signals into electric signal, can be had to faint light
The detection of effect is widely used in the research fields such as atomic weak light detection, photon detection, chemiluminescence, bioluminescence.Including low-light
Image intensifier, photomultiplier tube, streak tube etc..The core of above-mentioned Vacuum Photoelectric Detectors part is photocathode, performance
Quality directly affects the performance of entire device, and Specifeca tion speeification is quantum efficiency, i.e. 100 photons of the every reception of photocathode
The electron amount that can emit.Currently used alkali antimonide includes with potassium, sodium, lithium, and caesium is the various of alkali metal material
Single alkali, double alkali and polybase antimonide, comprising: K3Sb、Cs3Sb、K2CsSb、K2NaSb, K2LiSb and KNaCsSb etc..
The preparation method of alkali antimonide photocathode is mainly distinguished according to whether alkali metal and antimony are deposited simultaneously, is had
Independent vapour deposition method and co-evaporation method, either independent vapor deposition or co-evaporation, both for the preparation process of vacuum evaporation.
What a kind of photoelectricity flow monitoring and the reflectivity monitoring proposed in the patent application of application number 201610856127.2 combined
K2CsSb photocathode preparation method uses bottom potassium, and potassium antimony is the same as the preparation flow for steaming most laggard caesium；Application number
201510438585.X patent in propose a kind of Na2The preparation method of CsSb photocathode, which employs caesium-antimonies to mend sodium with steaming,
It steams caesium and mends sodium, caesium-antimony steams the preparation flow of antimony with benefit sodium is steamed；For the first time by semiconductor in the patent of application number 201710743036.2
The built in field diffusion theory of carrier is applied in the preparation of Bialkali photocathode, i.e., there are a built-in electricity in band curvature area
, be conducive to electronics in material and transported to surface.
As can be seen that current alkali antimonide photocathode was all made of is that alkali metal and antimony are common from above-mentioned patent
Vapor deposition, and non-individual is deposited.This is because co-evaporation can realize film coating composition by adjusting the ratio of alkali metal and antimony
Control, to effectively provide the quantum efficiency of photocathode.Co-evaporation can use two schemes, the first is by a large amount of
Test, find out set time and fixed evaporation capacity；It is for second the variation according to photocurrent curve, adjustment evaporation in real time
Amount.The applicable premise of the first scheme is that vacuum, alkali-metal evaporation source and antimony evaporation source have high consistency, otherwise the
Two kinds of schemes have more universality, and are easier to produce photocathode with high performance.Therefore, in co-evaporation by alkali gold
Belong to evaporation capacity solidification, the antimony evaporation capacity how to efficiently control according to photocurrent curve variation tendency just becomes influence cathode performance
Key element.
Summary of the invention
It is an object of that present invention to provide a kind of antimony electric current for the production of performance alkali metal antimonide photocathode is automatic
Regulation method.
To reach above-mentioned purpose, the present invention propose it is a kind of for performance alkali metal antimonide photocathode production
Antimony electric current method for automatically regulating, which is characterized in that this method comprises:
Alkali metal vapor deposition makes alkali metal by adjusting alkali metal evaporation current to fix stable evaporation capacity precipitation；
Antimony vapor deposition adjusts antimony electric current to precipitation value after carrying out degasification to antimony；
Photocurrent curve fitting and prediction, are fitted collected photocurrent curve tendency, while predicting subsequent optical
Current curve slope；
The judgement of photocurrent curve slope, first determines whether prediction photocurrent curve slope reaches desired value, if reached
It arrives, then continues to judge whether practical photocurrent curve slope β reaches desired value after waiting, otherwise increase antimony electric current immediately；
If the practical photocurrent curve slope β reaches desired value, continue to judge practical photocurrent curve after waiting
Whether slope β reaches designated value, otherwise judges whether practical photocurrent curve slope β is positive value immediately:
If the practical photocurrent curve slope β is positive value, continue to judge the practical photocurrent curve after waiting
Whether whether β reaches desired value to slope, otherwise increases antimony electric current immediately；
If described continue to judge that practical photocurrent curve slope β reaches desired value, the practical photoelectric current of judgement after waiting
Whether slope of curve β reaches designated value, otherwise increases antimony electric current immediately；
If the practical photocurrent curve slope β of judgement reaches designated value, adjusts the antimony stage to terminate, otherwise increase immediately
Antimony electric current；
Whether the vapor deposition adjustment of antimony electric current reaches desired value, and practical photoelectric current song according to prediction photocurrent curve slope
The deviation size of line slope β and desired value and designated value carries out the adjustment of antimony electric current.
Further, the alkali metal vapor deposition refers to forms alkali metal atmosphere, alkali metal before steaming antimony under vacuum conditions
The mark that vapor deposition terminates is to start to fall after rise after photoelectric current rises to maximum value.
Further, photocurrent curve is fitted, is calculated using fitting of a polynomial or least square method curve matching
Method.
Further, the photocurrent curve tendency being fitted is in predetermined time △ T1In range, value 0~5min it
Between.
Further, the photocurrent curve slope predicted is in predetermined time △ T2In range, value 0~2min it
Between.
Further, gear is regulated and controled for the photoelectric current of setting, the desired value and designated value should be definite value or fixed model
Value is enclosed, and designated value photoelectric current climbing speed more corresponding than desired value is faster.
Further, photoelectric current regulation gear include 1mA, 500 μ A, 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, 500nA, 500nA, 200nA, 100nA, 50nA, 20nA and 10nA totally 18 gear
Further, the photocurrent curve slope of the prediction and actual photocurrent curve slope β, select its energy
The smallest photoelectric current regulation gear being in.
Further, for the photocurrent curve slope of prediction and practical photocurrent curve slope β, expectation is not reached
The increased antimony electric current of adjustment, which is greater than, required for value does not reach the increased antimony electric current of designated value.
Further, in the case where not reaching desired value or designated value for practical photocurrent curve slope β, adjustment increases
The antimony electric current added is directly proportional to angular deviation.
By above technical scheme, the remarkable advantage of implementation method above-mentioned of the invention is:
1) evaporation capacity is adjusted in real time due to using to change according to photocurrent curve in alkali metal and antimony co-evaporation
Component ratio control may be implemented in method；
2) do not change only with reference to actual photocurrent curve, referring also to predict the variation of photoelectric current theoretical curve, it is this
Increased judgement content judges completed antimony electric current vapor deposition more accurate during tune antimony；
3) deviation comparison carried out to practical photocurrent curve and desired value and theoretical value, it is increased during this tune antimony to sentence
Broken strip part keeps the quasi- antimony electric current to be carried out adjustment more accurate；
4) performance alkali metal antimonide photocathode antimony current regulation method is established on the basis of automatic regulating system,
Manually adjust that antimony fault rate is low, repeated height relatively, the photocathode of preparation is used in neutrino detection large scale photomultiplier tube
K2CsSb photocathode, the quantum efficiency at 410nm reach 35% or more, are significantly better than the effect of existing artificial regulatory
Fruit.
Detailed description of the invention
Fig. 1 is the antimony electric current auto-control stream for alkali antimonide photocathode of some embodiments according to the present invention
Cheng Tu.
Fig. 2 is the antimony electric current auto-control system for alkali antimonide photocathode of some embodiments according to the present invention
System is illustrated as cathode production parameter and photoelectric current gear display figure on regulation software interface.
Fig. 3 is the antimony electric current auto-control for alkali antimonide photocathode of some embodiments according to the present invention
Photocurrent curve is illustrated as judging photoelectric current and theoretical curve when whether β reaches desired value.
Fig. 4 is the antimony electric current auto-control for alkali antimonide photocathode of some embodiments according to the present invention
Photocurrent curve is illustrated as judging photoelectric current and theoretical curve when whether β reaches designated value.
Fig. 5 is the antimony electric current auto-control for alkali antimonide photocathode of some embodiments according to the present invention
Photocurrent curve is illustrated as end and adjusts photoelectric current and theoretical curve after antimony.
Fig. 6 is the antimony amount method for automatically regulating for alkali antimonide photocathode of some embodiments according to the present invention
Prepare the quantum efficiency distribution and the artificial quantum efficiency profiles versus's situation for adjusting antimony preparation of sample pipe.
Specific embodiment
Fig. 1 is the antimony electric current auto-control stream for alkali antimonide photocathode of some embodiments according to the present invention
Cheng Tu.Include: plus whether antimony 101, prediction α reach desired value 102, judge whether β reaches desired value 103, judges whether β is positive
Value 104 judges whether β reaches desired value 105, judges whether β reaches designated value 106 and terminate to adjust antimony 107.
In general, it is proposed that the antimony electric current method for automatically regulating packet for alkali antimonide photocathode
Include: alkali metal vapor deposition, antimony vapor deposition, photocurrent curve fitting are with prediction, the judgement of photocurrent curve slope and according to photoelectric current song
Adjustment is deposited in the antimony electric current that line slope judging result carries out.
Alkali metal vapor deposition, refers to by adjusting alkali metal evaporation current, makes alkali metal to fix stable evaporation capacity precipitation.
Antimony vapor deposition adjusts antimony electric current to precipitation value after carrying out degasification to antimony.
Photocurrent curve fitting and prediction, are fitted collected photocurrent curve tendency, while predicting subsequent optical
Current curve slope.
The judgement of photocurrent curve slope, specifically includes:
It first determines whether prediction photocurrent curve slope reaches desired value, if reached, it is real to continue judgement after waiting
Whether border photocurrent curve slope β reaches desired value, otherwise increases antimony electric current immediately；
If the practical photocurrent curve slope β reaches desired value, continue to judge practical photocurrent curve after waiting
Whether slope β reaches designated value, otherwise judges whether practical photocurrent curve slope β is positive value immediately:
If the practical photocurrent curve slope β is positive value, continue to judge the practical photocurrent curve after waiting
Whether whether β reaches desired value to slope, otherwise increases antimony electric current immediately；
If described continue to judge that practical photocurrent curve slope β reaches desired value, the practical photoelectric current of judgement after waiting
Whether slope of curve β reaches designated value, otherwise increases antimony electric current immediately；
If the practical photocurrent curve slope β of judgement reaches designated value, adjusts the antimony stage to terminate, otherwise increase immediately
Antimony electric current.
Whether the vapor deposition adjustment of antimony electric current reaches desired value, and practical photoelectric current song according to prediction photocurrent curve slope
The deviation size of line slope β and desired value and designated value carries out the adjustment of antimony electric current.
Process as shown in connection with fig. 1 is adjusted by antimony electric current to precipitation value, and adding 101 step of antimony, there are four types of add antimony altogether
Operation is to add antimony after α does not reach desired value 102 respectively, and judging β not is to add antimony after 104, judges that β does not reach expectation
Add antimony after value 105 and judges to add antimony after β does not reach designated value 106.
According to an embodiment of the invention, for 20 inches of photomultiplier tube K2For CsSb photocathode, above-mentioned four kinds add
The antimony electric current incrementss of antimony operation are respectively 0.4A, 0.2A, 0.5A and 0.3A, and the corresponding waiting time is 2.0min.And it is above-mentioned
Judge after β does not reach desired value 105 plus antimony and judges increased antimony electric current 0.5A and 0.3A after β does not reach designated value 106
Only basic crack is also influenced by β and the difference of desired value and designated value.
Whether prediction α reaches in 102 step of desired value, and curve automatically adjusts to locating gear, guarantees the light of display
Electric current is greater than 4.5 lattice in coordinate, the display that otherwise subtracts 1 grade.On the regulation software interface provided in conjunction with Fig. 2 cathode production parameter and
Photoelectric current gear display figure, it can be seen that the gear include 1mA, 500 μ A, 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, 500nA, 500nA, 200nA, 100nA, 50nA, 20nA and 10nA totally 18 gears.And each gear
10 lattice are all only shown in photoelectric current coordinate system.For example, 1 lattice represent 0.5 μ A when photoelectric current gear is 5 μ A；When photoelectric current shelves
When position is 100nA, 1 lattice represent 10nA.The display methods, when photoelectric current is in 10 lattice, gear can add 1 grade automatically, light
Electric current can also drop back into the 5th lattice automatically；When photoelectric current is in less than 4.5 lattice, gear can subtract 1 automatically grade, and photoelectric current also can be automatic
It is increased to twice of lattice number.In addition, also showing other cathode production parameters on the regulation software interface, comprising: photoelectric current, leakage
The information such as electric current, current slope, reflectivity and reflectance slope.
Based on above-mentioned gear change principle, the corresponding photoelectric current of desired value should rest on its minimum gear that can be in.
Desired value is defined as the photoelectric current slope of first quartile and the angle of vertical direction in the coordinate system, and 30 ° of fixed range angle.
When α reaches desired value, judge whether β reaches desired value 103 after waiting 1min；Otherwise when α does not reach the value, increase immediately
Add 0.4A antimony electric current, i.e., repeatedly step adds antimony 101.
Judge whether β reaches in 103 step of desired value, the desired value is similarly the photoelectric current slope in first quartile
With 30 ° of angle of vertical direction.When β reaches desired value, judge whether β reaches designated value 106 after waiting 5min；Otherwise work as β
When not reaching desired value, judge whether β is positive value 104 immediately.
Judge whether β is in 104 steps of positive value, and the positive value refers to that photoelectric current is in first quartile in coordinate system, is responsible for
Photoelectric current decline, slope enter the second quadrant of coordinate system.The positive value is set as 5 ° of ﹣, it is therefore an objective to exclude because signal jitter is to sentencing
Whether disconnected β is on the occasion of the interference generated.When β is positive value, 1min is waited to judge whether β reaches desired value 105；When β is not positive
When value, increase 0.2A antimony electric current immediately, i.e., repeatedly step adds antimony 101.
Judge whether β reaches in 105 step of desired value, the desired value is similarly the photoelectric current slope in first quartile
With 30 ° of angle of vertical direction.When β reaches desired value, judge whether β reaches designated value 106 after waiting 5min；Otherwise work as β
When not reaching desired value, β is every to reduce 5 °, and the antimony electric current increases 0.05A, and the waiting time increases 0.5min, specific feelings
Condition is as shown in table 1.
The Sb electric current when β does not reach desired value of table 1 increases situation
| β | 0 °~5 ° | 5 °~10 ° | 10 °~15 ° | 15 °~20 ° | 20 °~25 ° | 25 °~30 ° |
| Sb evaporation current | 0.75A | 0.7A | 0.65A | 0.6A | 0.55A | 0.5A |
| Waiting time | 4.5min | 4min | 3.5min | 3min | 2.5min | 2min |
Judge whether β reaches in 106 step of designated value, the designated value is defined as the light in first quartile in coordinate system
Current slope and 45 ° of the angle of vertical direction.When β reaches designated value, terminate to adjust antimony 107 after waiting 2min；Otherwise when β does not have
When reaching the value, β is every to reduce 5 °, and the antimony electric current increases 0.05A, and the waiting time increases 0.5min, concrete condition such as table 2
It is shown.
The Sb electric current when β does not reach designated value of table 2 increases situation
| β | 25 °~30 ° | 30 °~35 ° | 35 °~40 ° | 40 °~45 ° |
| Sb evaporation current | 0.45A | 0.4A | 0.35A | 0.3A |
| Waiting time | 3.5min | 3min | 2.5min | 2min |
Fig. 3 is the antimony electric current auto-control for alkali antimonide photocathode of some embodiments according to the present invention
Photocurrent curve is illustrated as judging photoelectric current and theoretical curve when whether β reaches desired value.Wherein, curve 1 is practical photoelectricity
Flow curve, curve 2 are theoretical curve.It has been carried out in 6.5min plus antimony, then to adding the curve after antimony to carry out theoretical fitting,
Fit time △ T1For 2min, predicted time △ T2For 1min.Finally, α has reached desired value (30 °) for 37 °, and β, which is 13 °, not to be had
Reach desired value (30 °), therefore, which should continue plus antimony, and adding antimony electric current is 0.65A, waiting time 3.5min.
Fig. 4 is the antimony electric current auto-control for alkali antimonide photocathode of some embodiments according to the present invention
Photocurrent curve is illustrated as judging photoelectric current and theoretical curve when whether β reaches designated value.Wherein, curve 1 is practical photoelectricity
Flow curve, curve 2 are theoretical curve.It has been carried out in 8.3min plus antimony, then to adding the curve after antimony to carry out theoretical fitting,
Fit time △ T1For 2min, predicted time △ T2For 1min.Finally, α has reached desired value (30 °) for 56 °, and β is 58 ° and has reached
To designated value (45 °), therefore, which can terminate to adjust antimony.
Fig. 5 is the antimony electric current auto-control for alkali antimonide photocathode of some embodiments according to the present invention
Photocurrent curve is illustrated as end and adjusts practical photoelectric current and theoretical curve after antimony.Wherein, curve 1 is practical photocurrent curve, bent
Line 2 is theoretical curve.It has been carried out in 5min plus antimony, then to adding the curve after antimony to carry out theoretical fitting, fit time △
T1For 3min, predicted time △ T2For 1min.Finally, α has reached desired value (30 °) for 66 °, and β is 74 ° and has reached designated value
Terminate to adjust antimony after (45 °), photoelectric current starts to stablize rising, and when photoelectric current rises to 10 lattice, gear adds 1 grade automatically, in Fig. 5
Gear shift 3 times altogether.
Fig. 6 is the antimony amount method for automatically regulating for alkali antimonide photocathode of some embodiments according to the present invention
Prepare the quantum efficiency distribution and the artificial quantum efficiency profiles versus's situation for adjusting antimony preparation of sample pipe.Two methods sampled data output
It is all larger than 200.It can be seen that sample pipe prepared by the method for antimony amount auto-control is greater than 27% or more accounting in quantum efficiency
In be superior to manually antimony method be adjusted to prepare sample pipe, illustrate some embodiments according to the present invention for alkali antimonide photoelectricity yin
The antimony amount method for automatically regulating of pole has positive effect on improving cathode quantum efficiency.
Claims (10)
1. a kind of antimony electric current method for automatically regulating for the production of performance alkali metal antimonide photocathode, which is characterized in that
This method comprises:
Alkali metal vapor deposition makes alkali metal by adjusting alkali metal evaporation current to fix stable evaporation capacity precipitation；
Antimony vapor deposition adjusts antimony electric current to precipitation value after carrying out degasification to antimony；
Photocurrent curve fitting and prediction, are fitted collected photocurrent curve tendency, while predicting subsequent photoelectric current
Slope of curve α；
The judgement of photocurrent curve slope, first determines whether prediction photocurrent curve slope reaches desired value, if reached,
Continue to judge whether practical photocurrent curve slope β reaches desired value after waiting, otherwise increases antimony electric current immediately；
If the practical photocurrent curve slope β reaches desired value, continue to judge practical photocurrent curve slope β after waiting
Whether reach designated value, otherwise judge whether practical photocurrent curve slope β is positive value immediately:
If the practical photocurrent curve slope β is positive value, continue to judge the practical photocurrent curve slope after waiting
Whether whether β reaches desired value, otherwise increases antimony electric current immediately；
If described continue to judge that practical photocurrent curve slope β reaches desired value, the practical photocurrent curve of judgement after waiting
Whether slope β reaches designated value, otherwise increases antimony electric current immediately；
If the practical photocurrent curve slope β of judgement reaches designated value, the antimony stage is adjusted to terminate, otherwise increases antimony electricity immediately
Stream；
Whether the vapor deposition adjustment of antimony electric current reaches desired value according to prediction photocurrent curve slope, and practical photocurrent curve is oblique
The deviation size of rate β and desired value and designated value carries out the adjustment of antimony electric current.
2. the antimony electric current auto-control side according to claim 1 for the production of performance alkali metal antimonide photocathode
Method, which is characterized in that the alkali metal vapor deposition refers to forms alkali metal atmosphere under vacuum conditions before steaming antimony, alkali metal vapor deposition
The mark of end is to start to fall after rise after photoelectric current rises to maximum value.
3. the antimony electric current auto-control side according to claim 1 for the production of performance alkali metal antimonide photocathode
Method, which is characterized in that photocurrent curve is fitted, using fitting of a polynomial or least square method curve fitting algorithm.
4. the antimony electric current auto-control side according to claim 1 for the production of performance alkali metal antimonide photocathode
Method, which is characterized in that the photocurrent curve tendency being fitted is in predetermined time △ T1In range, value is between 0~5min.
5. the antimony electric current auto-control side according to claim 1 for the production of performance alkali metal antimonide photocathode
Method, which is characterized in that the photocurrent curve slope predicted is in predetermined time △ T2In range, value is between 0~2min.
6. the antimony electric current auto-control side according to claim 1 for the production of performance alkali metal antimonide photocathode
Method, which is characterized in that gear is regulated and controled for the photoelectric current of setting, the desired value and designated value should be definite value or fixed range
Value, and designated value photoelectric current climbing speed more corresponding than desired value is faster.
7. the antimony electric current auto-control side according to claim 6 for the production of performance alkali metal antimonide photocathode
Method, which is characterized in that the photoelectric current regulation gear includes 1mA, 500 μ A, 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, 500nA, 500nA, 200nA, 100nA, 50nA, 20nA and 10nA totally 18 gears.
8. the antimony electric current according to claim 6 or 7 for the production of performance alkali metal antimonide photocathode is adjusted automatically
Prosecutor method, which is characterized in that the photocurrent curve slope of the prediction and actual photocurrent curve slope β select its energy
The smallest photoelectric current regulation gear being in.
9. the antimony electric current auto-control side according to claim 1 for the production of performance alkali metal antimonide photocathode
Method, which is characterized in that for the photocurrent curve slope and practical photocurrent curve slope β of prediction, do not reach desired value institute
It needs to adjust increased antimony electric current and is greater than and do not reach the increased antimony electric current of designated value.
10. the antimony electric current auto-control according to claim 1 for the production of performance alkali metal antimonide photocathode
Method, which is characterized in that in the case where not reaching desired value or designated value for practical photocurrent curve slope β, adjustment increases
The antimony electric current added is directly proportional to angular deviation.
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| CN113451090A (en) * | 2021-06-28 | 2021-09-28 | 北方夜视技术股份有限公司 | Method for improving controllability and consistency of cathode quantum efficiency of photomultiplier |
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