CN117352351A - Method for treating excessive sodium-antimony co-evaporation during preparation of super-second-generation polybasic photoelectric cathode - Google Patents
Method for treating excessive sodium-antimony co-evaporation during preparation of super-second-generation polybasic photoelectric cathode Download PDFInfo
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- CN117352351A CN117352351A CN202311260414.3A CN202311260414A CN117352351A CN 117352351 A CN117352351 A CN 117352351A CN 202311260414 A CN202311260414 A CN 202311260414A CN 117352351 A CN117352351 A CN 117352351A
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- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000010549 co-Evaporation Methods 0.000 title claims abstract description 27
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title description 5
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 55
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000011734 sodium Substances 0.000 claims abstract description 51
- 238000010025 steaming Methods 0.000 claims abstract description 40
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 39
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 230000000630 rising effect Effects 0.000 claims abstract description 8
- 238000003672 processing method Methods 0.000 claims abstract description 5
- 230000035945 sensitivity Effects 0.000 abstract description 24
- 239000003513 alkali Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 5
- 238000001704 evaporation Methods 0.000 description 12
- 230000008020 evaporation Effects 0.000 description 8
- 238000003384 imaging method Methods 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052792 caesium Inorganic materials 0.000 description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004590 computer program Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/12—Manufacture of electrodes or electrode systems of photo-emissive cathodes; of secondary-emission electrodes
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/52—Alloys
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Image-Pickup Tubes, Image-Amplification Tubes, And Storage Tubes (AREA)
Abstract
The invention discloses a processing method for excessive sodium-antimony co-evaporation in the process of manufacturing a super-second generation polybasic photoelectric cathode, which detects photocurrent in the process of manufacturing, judges that excessive sodium-antimony is excessive in the process of sodium-antimony co-evaporation in a basal layer if the photocurrent is lower than 1500nA, and carries out the following processing: switching on a Na steaming power supply, and adjusting the Na steaming current to an initial value; increasing sodium steaming current at a rate of 400mA/min, stopping increasing the sodium steaming current and maintaining the current sodium steaming current when the rising or falling of the photocurrent is detected; after one minute, the antimony steaming power supply is turned on; the antimony steaming current is adjusted to an initial value, and the antimony steaming current is increased at a rate of 500 mA/min; when the rising or falling of the photocurrent is detected, firstly turning off the antimony steaming power supply within 30 seconds; and after one minute, the sodium steaming power supply is turned off, and the next process is carried out. The method is used for solving the problem of low sensitivity caused by excessive antimony of the basal layer in the process of manufacturing the super-second-generation multi-alkali photocathode, and has remarkable effect of improving the sensitivity of the photocathode.
Description
Technical Field
The invention belongs to the technical field of photocathodes, and particularly relates to a treatment method for sodium-antimony co-evaporation of excessive antimony in the process of manufacturing a super-second-generation multi-alkali photocathode.
Background
The photocathode is a key component for photoelectric conversion of various micro-light image intensifiers, plays a role in converting a weak photoelectronic image into electrons, is a key technology for manufacturing the image intensifier, the sensitivity of the photocathode directly influences various performance indexes of the image intensifier, the sensitivity of the photocathode after being manufactured directly influences the tube selection rate of a company, the manufacturing yield of the image intensifier is influenced, along with the higher and higher performance requirements of users on the image intensifier, the sensitivity of the photocathode is improved, the image intensifier of the company is impacted by the third-generation image intensifier and a CMOS solid device, the manufacturing cost of the image intensifier is high, the market competitiveness is reduced, and currently, the cost of the image intensifier of China is reduced.
Referring to fig. 1, the manufacturing of the multi-alkali photocathode is carried out in a vacuum environment, the main evaporation components are potassium, sodium, cesium and antimony, and the evaporation process comprises the following steps:
(1) Evaporating potassium;
(2) Evaporating sodium;
(3) Co-evaporation of sodium and antimony;
(4) Co-evaporation of potassium, sodium and antimony;
(5) Surface cesium activation.
The manufacturing according to the above steps is usually performed under the automatic control of a process computer program, during the manufacturing process, the photocurrent and the leakage current are detected in real time by switching on/off the process lamp (the process lamp is turned on to detect the photocurrent, and the process lamp is turned off to detect the leakage current), and usually the photocurrent is always detected in the whole manufacturing process, and at the end of each process, the process lamp is turned off to detect the leakage current, and in general, the leakage current is lower than a certain value (for example, 1000nA or less) as normal.
It should be noted that, when the sodium and antimony are co-evaporated on the substrate layer in the process of manufacturing the photocathode, an excessive antimony condition (about 30% according to statistics of the inventor) occurs when the process is automatically controlled by a process computer program, the average sensitivity of the photocathode with excessive antimony is lower than 700 μa/lm, and the requirement of general standard tube selection of the super-second-generation image intensifier cannot be met, so that the micro-light image intensifier is scrapped, and therefore, a solution is needed to be provided for the condition.
Disclosure of Invention
The invention aims to solve the technical problems that: aiming at the problem that the sensitivity is lower due to excessive antimony during co-evaporation of sodium and antimony during the preparation of the super-second-generation polybasic photoelectric cathode, the treatment method is provided.
The invention effectively solves the problem of unqualified sensitivity of the photocathode caused by excessive antimony in the manufacturing process of the multi-alkali photocathode by controlling the current and time of evaporating sodium and antimony sources, effectively improves the sensitivity of the super-second-generation multi-photocathode, and simultaneously can reduce the manufacturing cost of the image intensifier.
The technical scheme of the invention is as follows:
a method for treating excessive sodium-antimony co-evaporation when preparing super-second generation polybasic photocathode comprises detecting photocurrent by irradiation of process lamp during photocathode preparation process, judging excessive sodium-antimony co-evaporation when the photocurrent is lower than a certain value, and treating according to the following steps:
step 1: switching on a Na steaming power supply, and adjusting the Na steaming current to an initial value;
step 2: increasing sodium steaming current at a rate of 400mA/min, stopping increasing the sodium steaming current and maintaining the current sodium steaming current when the rising or falling of the photocurrent is detected;
step 3: after one minute, the antimony steaming power supply is turned on;
step 4: the antimony steaming current is adjusted to an initial value, and the antimony steaming current is increased at a rate of 500 mA/min;
step 5: when the rising or falling of the photocurrent is detected, firstly turning off the antimony steaming power supply within 30 seconds;
step 6: and after one minute, the sodium evaporation power supply is turned off, the treatment when the sodium and antimony co-evaporation is excessive is completed, and the next step of potassium, sodium and antimony co-evaporation process is carried out.
Further, the excessive antimony means that the photoelectric current value is detected after the co-evaporation of sodium and antimony is finished, and if the photoelectric current value is lower than 1500nA, the excessive antimony is judged to be during the co-evaporation of sodium and antimony.
Further, the initial value of the sodium current in the step 1 is 2000-2500mA.
The mechanism of the invention is as follows:
the manufacture of the photoelectric cathode substrate layer is to form Na by co-evaporating sodium antimony in a vacuum environment 3 Sb，Na 3 Sb is a single crystal semiconductor structure, and if excessive Sb is evaporated, it cannot react with Na sufficiently to form Na 3 Sb, which causes defects of the photoelectric cathode crystal structure and affects photoelectron escapeThe method can fully react excessive antimony with sodium to form Na 3 Sb。
The beneficial effects of the invention include:
(1) In the process of preparing the multi-alkali photocathode, the phenomenon of excessive antimony during the co-evaporation of sodium and antimony on a basal layer is obvious and easy to identify;
(2) The method for treating excessive antimony in the process of co-evaporation of sodium and antimony on the substrate layer of the multi-alkali photocathode is simple and easy to operate, and can be widely popularized and used;
(3) The average value of the sensitivity of the photocathode processed by the method reaches 840 mu A/lm, thereby effectively improving the manufacturing sensitivity of the photocathode, improving the tube selection rate, reducing the manufacturing cost of an image intensifier and achieving the value of saving the wound.
Drawings
FIG. 1 is a schematic diagram of a multi-alkali photocathode made in accordance with the present invention.
FIG. 2 is a schematic diagram of a process flow of a treatment method for improving the sensitivity of the super second generation polybasic photoelectric negative electrode.
FIG. 3 is a graph of the imaging effect of the microimage intensifier processed by the method, and the brightness gain of the field of view is high, so that the general specification tube selection requirement of the supersecond-generation image intensifier can be met.
FIG. 4 is a graph of the imaging effect of a microimage intensifier not processed by the method, and the brightness gain of a field of view is low, so that the general specification tube selection requirement of the supersecond-generation image intensifier cannot be met.
In fig. 1: 1-art lamp; 2-a substrate; 3-positive electrode collecting plate; 4-an alkali source evaporation source; 5-antimony evaporation source; 6-heating wires of an antimony evaporation source; 7, collecting and connecting the positive electrode; 8-an alkali source heating power line; 9-a reaction chamber; 10-vacuum pump piping; 11-heating mantle.
Detailed Description
The invention aims to find a treatment method for the excessive sodium-antimony co-evaporation in the process of manufacturing the super-second-generation multi-alkali photocathode, so as to improve the manufacturing sensitivity of the multi-alkali photocathode and the tube selection rate of the photocathode. On a special device for manufacturing the photocathode, the evaporation time of antimony is controlled when sodium and antimony are co-evaporated on a substrate layer of the multi-alkali photocathode, and the photocathode is prepared by the processed photocathode according to a normal process.
As an embodiment, the processing method of the present invention includes:
a method for treating excessive sodium-antimony co-evaporation when preparing super-second generation polybasic photocathode comprises detecting photocurrent by irradiation of process lamp during photocathode preparation process, judging excessive sodium-antimony co-evaporation when the photocurrent is lower than a certain value, and treating according to the following steps:
step 1: switching on a Na steaming power supply, and adjusting the Na steaming current to an initial value;
step 2: increasing sodium steaming current at a rate of 400mA/min, stopping increasing the sodium steaming current and maintaining the current sodium steaming current when the rising or falling of the photocurrent is detected;
step 3: after one minute, the antimony steaming power supply is turned on;
step 4: the antimony steaming current is adjusted to an initial value, and the antimony steaming current is increased at a rate of 500 mA/min;
step 5: when the rising or falling of the photocurrent is detected, firstly turning off the antimony steaming power supply within 30 seconds;
step 6: and after one minute, the sodium evaporation power supply is turned off, the treatment when the sodium and antimony co-evaporation is excessive is completed, and the next step of potassium, sodium and antimony co-evaporation process is carried out.
As an example, the excessive amount of antimony is a value of a photoelectric current detected after the co-evaporation of sodium and antimony is completed, and if the value of the photoelectric current is lower than 1500nA, it is determined that the excessive amount of antimony is caused during the co-evaporation of sodium and antimony. Antimony overdose results in a decrease in the efficiency of photoelectron escape, which is directly manifested by a photocell value below 1500nA.
After the photocathode is processed by the method, the sensitivity of the two photocathodes is tested in a sensitivity test device, and the result is that: the sensitivity average value of the photocathode after treatment is 841 mu A/lm, sensitivity test data are shown in table 1, and the data in table 1 can be seen that all the sensitivity test data meet the tube selection requirement of the general specification of the super-second-generation image intensifier; the sensitivity average value of the abnormal photocathode which is not processed by the method is 662 mu A/lm, the sensitivity test data are shown in the table 2, and the data in the table 2 can not meet the tube selection requirement of the general specification of the super-second-generation image intensifier.
TABLE 1 photocathode sensitivity and luminance gain with this approach
| Pipe number | Sensitivity (mu A/lm) | Brightness gain |
| 5272335 | 855 | 12310 |
| 5235522 | 822 | 11550 |
| 5234422 | 812 | 12350 |
| 5269947 | 869 | 11080 |
| 5237755 | 853 | 13550 |
| 5632222 | 833 | 12100 |
| 5327772 | 801 | 11200 |
| 5324471 | 839 | 12360 |
| 5231236 | 856 | 13500 |
| 5236647 | 877 | 13580 |
Table 2 photocathode sensitivity and luminance gain without this approach
| Pipe number | Sensitivity (mu A/lm) | Brightness gain |
| 4236117 | 655 | 7800 |
| 4237533 | 678 | 7900 |
| 5237715 | 622 | 7530 |
| 5326977 | 598 | 7000 |
| 5326774 | 700 | 8010 |
| 5326112 | 711 | 8100 |
| 5326344 | 658 | 7500 |
| 4236122 | 668 | 7580 |
| 4233566 | 632 | 7320 |
| 4144522 | 699 | 7950 |
The working voltage is applied to the low-light-level image intensifier, the working voltage of the photocathode is-200V, the imaging quality of the photocathode is observed after the photocathode is not processed and is processed by the method of the invention, and the result is that: the imaging effect after the treatment by the method is shown in fig. 3, and the imaging effect of the image intensifier without the treatment is shown in fig. 4. The result shows that the field brightness gain of the imaging (figure 3) image intensifier after the photocathode is processed is high, and the requirements of general specification tube selection of the super-second-generation image intensifier are met; the field of view brightness gain of the unprocessed image intensifier is low (fig. 4), and the brightness gain does not meet the common specification tube selection requirement of the super-second generation image intensifier.
Claims (4)
1. A processing method for the excessive sodium-antimony co-evaporation when preparing a super-second generation polybasic photoelectric cathode is characterized in that a photoelectric current is detected in a process lamp irradiation mode in the manufacturing process of the photoelectric cathode, a photoelectric current value is detected after the sodium-antimony co-evaporation is finished, if the photoelectric current is lower than a certain value, the excessive sodium-antimony co-evaporation is judged as a basal layer, and the processing is carried out according to the following steps:
step 1: switching on a Na steaming power supply, and adjusting the Na steaming current to an initial value;
step 2: increasing sodium steaming current at a rate of 400mA/min, stopping increasing the sodium steaming current and maintaining the current sodium steaming current when the rising or falling of the photocurrent is detected;
step 3: after one minute, the antimony steaming power supply is turned on;
step 4: the antimony steaming current is adjusted to an initial value, and the antimony steaming current is increased at a rate of 500 mA/min;
step 5: when the rising or falling of the photocurrent is detected, firstly turning off the antimony steaming power supply within 30 seconds;
step 6: and after one minute, the sodium steaming power supply is turned off, the treatment when the sodium and antimony co-steam antimony is excessive is completed, and the next process is carried out.
2. A processing method according to claim 1, characterized in that:
the antimony excess is the excess of antimony when the detected photoelectric value after the sodium-antimony co-evaporation is finished is less than 1500nA.
3. A processing method according to claim 1, characterized in that:
the initial value of the sodium steaming current in the step 1 is 2000-2500mA.
4. A process according to any one of claims 1 to 3, wherein:
and in the step 4, the initial value of the antimony steaming current is 1000-1500mA.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311260414.3A CN117352351A (en) | 2023-09-27 | 2023-09-27 | Method for treating excessive sodium-antimony co-evaporation during preparation of super-second-generation polybasic photoelectric cathode |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311260414.3A CN117352351A (en) | 2023-09-27 | 2023-09-27 | Method for treating excessive sodium-antimony co-evaporation during preparation of super-second-generation polybasic photoelectric cathode |
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| Publication Number | Publication Date |
|---|---|
| CN117352351A true CN117352351A (en) | 2024-01-05 |
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| CN202311260414.3A Pending CN117352351A (en) | 2023-09-27 | 2023-09-27 | Method for treating excessive sodium-antimony co-evaporation during preparation of super-second-generation polybasic photoelectric cathode |
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| Country | Link |
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- 2023-09-27 CN CN202311260414.3A patent/CN117352351A/en active Pending
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