CN104112634A - NEA photoelectric cathode preparation process - Google Patents
NEA photoelectric cathode preparation process Download PDFInfo
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- CN104112634A CN104112634A CN201410351946.2A CN201410351946A CN104112634A CN 104112634 A CN104112634 A CN 104112634A CN 201410351946 A CN201410351946 A CN 201410351946A CN 104112634 A CN104112634 A CN 104112634A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000004913 activation Effects 0.000 claims abstract description 47
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 238000000746 purification Methods 0.000 claims abstract description 22
- 238000004140 cleaning Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 4
- 125000004122 cyclic group Chemical group 0.000 claims description 22
- 238000011534 incubation Methods 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- 238000003486 chemical etching Methods 0.000 claims description 3
- 238000005530 etching Methods 0.000 claims description 3
- 230000002000 scavenging effect Effects 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 241000769223 Thenea Species 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 description 5
- 238000003795 desorption Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004297 night vision Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
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Abstract
The invention discloses an NEA photoelectric cathode preparation process. The method comprises performing high-temperature Cs/O circulated activation and low-temperature Cs activation on P-type GaN materials. The method also comprises the steps of chemical cleaning and high-temperature heating and purification before the high-temperature Cs/O circulated activation, low-temperature heating and purification between the high-temperature Cs/O circulated activation and the low-temperature Cs activation, and low-temperature Cs/O circulated activation after the low-temperature Cs activation, wherein the chemical cleaning comprises ultrasonic cleaning of samples, the high-temperature heating and purification comprises a heating step, a heat conservation step and a cooling step which are sequentially implemented, and the low-temperature heating and purification comprises a low-temperature heating step, a low-temperature heat conservation step and a low-temperature cooling step; the activation vacuum degree of the high-temperature heating and purification, the high-temperature Cs/O circulated activation, the low-temperature Cs activation, the low-temperature Cs activation, the low-temperature heating and purification and the low-temperature Cs/O circulated activation is between 10(-7) Pa and 5*10(-6) Pa. The NEA photoelectric cathode activation method is intuitive in activation degree, easy to control and beneficial to the property of products.
Description
Technical field
The present invention relates to the miniature lamp production technology for throwing light on or indicating, particularly relate to a kind of NEA photocathode preparation technology.
Background technology
Negative electron affinity (NEA) photocathode have spectral response range wide, highly sensitive, secretly launch the advantages such as little, emitted electron energy distributes and angular distribution is concentrated, long-wave response expansion potentiality are large, be widely used in vehicle-mounted, airborne and individual soldier's night-vision equipment, simultaneously, as a kind of high-performance rotating electron source, NEA photocathode is also widely applied in fields such as high-energy physics, microelectric technique, electron beam planographic and electron microscopes.Through the development of more than ten years, domesticly aspect the research of NEA photocathode, obtaining huge advance made, but three generations's low-light level tube still has larger gap at aspects such as sensitivity, stability, noise, life-span and rate of finished productss with comparing abroad.Activation technology is the important content in NEA photocathode preparation process, is the principal element that determines photocathode sensitivity and stability, and the control of procedural order and technological parameter in activation technology is the key point that determines photocathode sensitivity and stability.
Summary of the invention
For above-mentioned activation technology, it is the important content in NEA photocathode preparation process, it is the principal element that determines photocathode sensitivity and stability, the control of procedural order and technological parameter in activation technology, be the problem that determines the key point of photocathode sensitivity and stability, the invention provides a kind of NEA photocathode preparation technology.
For the problems referred to above, a kind of NEA photocathode preparation technology provided by the invention reaches goal of the invention by following technical essential: a kind of NEA photocathode preparation technology, comprise that high temperature Cs/O cyclic activation and low temperature Cs that P type GaN material sequences is carried out activate, before described high temperature Cs/O cyclic activation step, also comprise that chemical cleaning, high-temperature heating purify in sequence, high temperature Cs/O cyclic activation and low temperature Cs activate between step and also comprise that low-temperature heat purifies, and low temperature Cs also comprises low temperature Cs/O cyclic activation step after activating step;
Described chemical cleaning comprises and adopts carbon tetrachloride, acetone, absolute ethyl alcohol, deionized water to carry out sequentially Ultrasonic Cleaning in sample, and scavenging period is all within the scope of 4-5min;
Described high-temperature heating purifies and comprises heating step, incubation step and cooling step in sequence, the temperature upper limit of described heating step is not less than 680 ℃, and the heating-up time is not less than 150min, the duration of incubation step is no less than 20min, and the duration of cooling step is no less than 100min;
Described low-temperature heat purifies and comprises low temperature heating step, low temperature incubation step and low temperature cooling step in sequence, the temperature upper limit of described low temperature heating step is not less than 630 ℃, and the low temperature heating-up time is not less than 40min, the duration of low temperature incubation step is no less than 20min, and the duration of low temperature cooling step is no less than 80min;
Described high-temperature heating purification, high temperature Cs/O cyclic activation, low temperature Cs activate step, low-temperature heat purification, low temperature Cs/O cyclic activation step all in vacuum degree 10
-7to 5 * 10
-6under the vacuum environment of Pa, carry out.
Further technical scheme is:
Described chemical cleaning also comprises and is arranged on the follow-up etch step of Ultrasonic Cleaning, and described etch step adopts the concentrated sulfuric acid, hydrogen peroxide, deionized water to carry out chemical etching according to the mixed liquor of 2:2:1 proportioning.
Described etch period is within the scope of 8min-10min, and etching temperature is between 25 ℃-32 ℃.
After described chemical etch step, also comprise cleaning step, described cleaning step is for adopting deionized water sample to be no less than to the Ultrasonic Cleaning of 2min.
The present invention has following beneficial effect:
This technique activate degree directly perceived, be convenient to control, the chemical cleaning arranging, for removing the organic substances such as greasy dirt of cathode surface, is removed the O of cathode surface, S, the defect that the pollutants such as Cl and elimination mechanical polishing cause at sample surfaces, is beneficial to the follow-up high low temperature activation effect carrying out; Adopt the operation setting of high-temperature heating purification and low-temperature heat purification temperature gradient-heated, be convenient to guaranteeing that Ga oxide, N oxide and carbide are from cathode surface desorption in above heating purification process; The incubation step of twice heating process be convenient to realize two steps and complete after the oxide on GaN surface be completely removed, carbon content is less than an atomic monolayer; Be arranged on the technological design that realizes described high-temperature heating purification, high temperature Cs/O cyclic activation, low temperature Cs activation step, low-temperature heat purification, low temperature Cs/O cyclic activation step under vacuum environment, be convenient to judge whether whether there is gas overflowing on photocathode surface according to the variation of degree of hollowness in above process, be convenient to judge that whether activation is complete, be conducive to obtain the respond well photocathode of desorption.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but structure of the present invention is not limited only to following examples.
Embodiment 1:
A kind of NEA photocathode preparation technology, comprise that high temperature Cs/O cyclic activation and low temperature Cs that P type GaN material sequences is carried out activate, before described high temperature Cs/O cyclic activation step, also comprise that chemical cleaning, high-temperature heating purify in sequence, high temperature Cs/O cyclic activation and low temperature Cs activate between step and also comprise that low-temperature heat purifies, and low temperature Cs also comprises low temperature Cs/O cyclic activation step after activating step;
Described chemical cleaning comprises and adopts carbon tetrachloride, acetone, absolute ethyl alcohol, deionized water to carry out sequentially Ultrasonic Cleaning in sample, and scavenging period is all within the scope of 4-5min;
Described high-temperature heating purifies and comprises heating step, incubation step and cooling step in sequence, the temperature upper limit of described heating step is not less than 680 ℃, and the heating-up time is not less than 150min, the duration of incubation step is no less than 20min, and the duration of cooling step is no less than 100min;
Described low-temperature heat purifies and comprises low temperature heating step, low temperature incubation step and low temperature cooling step in sequence, the temperature upper limit of described low temperature heating step is not less than 630 ℃, and the low temperature heating-up time is not less than 40min, the duration of low temperature incubation step is no less than 20min, and the duration of low temperature cooling step is no less than 80min;
Described high-temperature heating purification, high temperature Cs/O cyclic activation, low temperature Cs activate step, low-temperature heat purification, low temperature Cs/O cyclic activation step all in vacuum degree 10
-7to 5 * 10
-6under the vacuum environment of Pa, carry out.
In this technique, the chemical cleaning of setting, for removing the organic substances such as greasy dirt of cathode surface, is removed the O of cathode surface, S, and the defect that the pollutants such as Cl and elimination mechanical polishing cause at sample surfaces, is beneficial to the follow-up high low temperature activation effect carrying out; Adopt the operation setting of high-temperature heating purification and low-temperature heat purification temperature gradient-heated, be convenient to guaranteeing that Ga oxide, N oxide and carbide are from cathode surface desorption in above heating purification process; The incubation step of twice heating process be convenient to realize two steps and complete after the oxide on GaN surface be completely removed, carbon content is less than an atomic monolayer; Be arranged on the technological design that realizes described high-temperature heating purification, high temperature Cs/O cyclic activation, low temperature Cs activation step, low-temperature heat purification, low temperature Cs/O cyclic activation step under vacuum environment, be convenient to judge whether whether there is gas overflowing on photocathode surface according to the variation of degree of hollowness in above process, be convenient to judge that whether activation is complete, be conducive to obtain the respond well photocathode of desorption.
Embodiment 2:
The present embodiment is further qualified on the basis of embodiment 1, for further optimizing activation effect or obtaining the more photocathode of good quality, described chemical cleaning also comprises and is arranged on the follow-up etch step of Ultrasonic Cleaning, and described etch step adopts the concentrated sulfuric acid, hydrogen peroxide, deionized water to carry out chemical etching according to the mixed liquor of 2:2:1 proportioning.
Described etch period is within the scope of 8min-10min, and etching temperature is between 25 ℃-32 ℃.
After described chemical etch step, also comprise cleaning step, described cleaning step is for adopting deionized water sample to be no less than to the Ultrasonic Cleaning of 2min.
Above content is the further description of the present invention being done in conjunction with concrete preferred implementation, can not assert that the specific embodiment of the present invention is confined to these explanations.For general technical staff of the technical field of the invention, not departing from other execution modes that draw under technical scheme of the present invention, all should be included in protection scope of the present invention.
Claims (4)
1. a NEA photocathode preparation technology, comprise that high temperature Cs/O cyclic activation and low temperature Cs that P type GaN material sequences is carried out activate, it is characterized in that, before described high temperature Cs/O cyclic activation step, also comprise that chemical cleaning, high-temperature heating purify in sequence, high temperature Cs/O cyclic activation and low temperature Cs activate between step and also comprise that low-temperature heat purifies, and low temperature Cs also comprises low temperature Cs/O cyclic activation step after activating step;
Described chemical cleaning comprises and adopts carbon tetrachloride, acetone, absolute ethyl alcohol, deionized water to carry out sequentially Ultrasonic Cleaning in sample, and scavenging period is all within the scope of 4-5min;
Described high-temperature heating purifies and comprises heating step, incubation step and cooling step in sequence, the temperature upper limit of described heating step is not less than 680 ℃, and the heating-up time is not less than 150min, the duration of incubation step is no less than 20min, and the duration of cooling step is no less than 100min;
Described low-temperature heat purifies and comprises low temperature heating step, low temperature incubation step and low temperature cooling step in sequence, the temperature upper limit of described low temperature heating step is not less than 630 ℃, and the low temperature heating-up time is not less than 40min, the duration of low temperature incubation step is no less than 20min, and the duration of low temperature cooling step is no less than 80min;
Described high-temperature heating purification, high temperature Cs/O cyclic activation, low temperature Cs activate step, low-temperature heat purification, low temperature Cs/O cyclic activation step all in vacuum degree 10
-7to 5 * 10
-6under the vacuum environment of Pa, carry out.
2. a kind of NEA photocathode preparation technology according to claim 1, it is characterized in that, described chemical cleaning also comprises and is arranged on the follow-up etch step of Ultrasonic Cleaning, and described etch step adopts the concentrated sulfuric acid, hydrogen peroxide, deionized water to carry out chemical etching according to the mixed liquor of 2:2:1 proportioning.
3. a kind of NEA photocathode preparation technology according to claim 2, is characterized in that, described etch period is within the scope of 8min-10min, and etching temperature is between 25 ℃-32 ℃.
4. a kind of NEA photocathode preparation technology according to claim 2, is characterized in that, also comprises cleaning step after described chemical etch step, and described cleaning step is for adopting deionized water sample to be no less than to the Ultrasonic Cleaning of 2min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410351946.2A CN104112634A (en) | 2014-07-23 | 2014-07-23 | NEA photoelectric cathode preparation process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410351946.2A CN104112634A (en) | 2014-07-23 | 2014-07-23 | NEA photoelectric cathode preparation process |
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| CN201410351946.2A Pending CN104112634A (en) | 2014-07-23 | 2014-07-23 | NEA photoelectric cathode preparation process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113488359A (en) * | 2021-06-08 | 2021-10-08 | 电子科技大学 | Preparation method of refrigeration type GaN electron source used in ultrahigh vacuum system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060170324A1 (en) * | 2004-10-13 | 2006-08-03 | The Board Of Trustees Of The Leland Stanford Junior University | Fabrication of group III-nitride photocathode having Cs activation layer |
| CN101866977A (en) * | 2010-06-25 | 2010-10-20 | 重庆大学 | Transmissive GaN UV Photocathode Based on Gradient Buffer Layer |
-
2014
- 2014-07-23 CN CN201410351946.2A patent/CN104112634A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060170324A1 (en) * | 2004-10-13 | 2006-08-03 | The Board Of Trustees Of The Leland Stanford Junior University | Fabrication of group III-nitride photocathode having Cs activation layer |
| CN101866977A (en) * | 2010-06-25 | 2010-10-20 | 重庆大学 | Transmissive GaN UV Photocathode Based on Gradient Buffer Layer |
Non-Patent Citations (1)
| Title |
|---|
| 杜晓晴 等: "GaN紫外光阴极材料的高低温两步制备实验研究", 《光学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113488359A (en) * | 2021-06-08 | 2021-10-08 | 电子科技大学 | Preparation method of refrigeration type GaN electron source used in ultrahigh vacuum system |
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Application publication date: 20141022 |