CN103215543B - Method for preparing film system with secondary electron emission function - Google Patents
Method for preparing film system with secondary electron emission function Download PDFInfo
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- CN103215543B CN103215543B CN201310140813.6A CN201310140813A CN103215543B CN 103215543 B CN103215543 B CN 103215543B CN 201310140813 A CN201310140813 A CN 201310140813A CN 103215543 B CN103215543 B CN 103215543B
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Abstract
The invention discloses a method for preparing a film system with a secondary electron emission function, belonging to the field of functional film preparation. The method comprises the following steps of: (1) cleaning a vacuum chamber; (2) cleaning a substrate; (3) loading the substrate; (4) vacuumizing the vacuum chamber; (5) cleaning a target material by using plasma; and (6) depositing secondary electron emission films. According to the method, the traditional oxidation process is replaced with a preparation method that multiple layers of composite functional films are deposited, so that the prepared film has the advantages of good compactness, strong adhesion, high secondary electron emission rate and the like.
Description
Technical field
The present invention relates to a kind of film system preparation method with secondary electron emission function, be specifically related to a kind of preparation method taking stainless steel as substrate and adopt magnetron sputtering technique deposition secondary electron emission film, belong to field of functional film preparation.
Background technology
Atomic clock is that keep time in current various countries, the Core equipment of time service, in a large number for military navigation station-keeping system, time-frequency test satellite location and time-frequency website and satellite civil navigation, is one of core load of satellite-navigation global positioning system (GPS).The atomic clock of current development comparative maturity mainly contains rubidium clock, hydrogen clock and caesium clock.Comparatively speaking, caesium clock precision is higher, and long-term stability is best, and reliability is very high, and in space, application has very clear and definite background demand, and as navigation and survey of deep space etc., small-sized caesium clock is also widely applied at navigation system ground station simultaneously.
The caesium clock that China's time and frequency system uses mainly relies on imported from America, and the production of small-sized caesium clock is monopolized by the U.S. at present substantially, is difficult to import especially to high Property in America cesium-beam atomic clock in Military Application.The shortage of domestic hiperspace cesium-beam atomic clock technology constrains the development of Chinese Space airmanship to a great extent.
One of them major reason does not solve the problems such as the cesium-beam atomic clock life-span is short.The factor affecting cesium-beam atomic clock working life is a lot, wherein the electron-multiplier life-span short is a major cause, the work-ing life of the reason causing the electron-multiplier life-span short mainly electron-multiplier dynode secondary electron emission function film is too short, and high gain and high stable coordination aspect have problems.Therefore, whether current domestic high-performance cesium-beam atomic clock can be succeeded in developing, and depend on the development progress of long lifetime high gain electron-multiplier to a great extent, and the development of long lifetime high gain secondary electron emission function film is depended in the development of electron-multiplier.
Summary of the invention
The object of the present invention is to provide a kind of film system preparation method with secondary electron emission function, be specially a kind of preparation method taking stainless steel as substrate and adopt magnetron sputtering technique deposition secondary electron emission film, described method utilizes the preparation method of deposit multilayer complex function thin film to replace conventional oxidation process, and prepared film compactness is good, strong adhesion and secondary electron emission rate advantages of higher.
Object of the present invention is realized by following technical scheme:
Have a film system preparation method for secondary electron emission function, described method steps is as follows:
(1) clean vacuum room: open vacuum chamber, not contaminated for protection target aluminium film is placed into directly over target, remove the pollutent in the rete and air come off in vacuum chamber, then dip in volatile organic solution wiped clean vacuum chamber inwall with absorbent gauze; Described target has three kinds, is respectively metal titanium targets, metallic silver target, ceramic alumina magnesium target; The purity of described target is more than 99.99%;
(2) substrate is cleaned: stainless steel substrate is put into clean vessel, rinse well with water, again stainless steel substrate is used respectively analytical pure acetone and each ultrasonic cleaning 10 ~ 30min of analytical pure alcohol, then rinse well by the volatile organic solution of analytical pure, with the wiping of chipless cleansing tissue to surperficial no marking, scratch and drop remaining trace;
(3) substrate is filled: the stainless steel substrate after step (2) being cleaned is put in the substrate frame of vacuum chamber, and removes for the protection of the not contaminated aluminium film of target;
(4) vacuum chamber: open mechanical pump and take out in advance, vacuum tightness is evacuated to 1Pa, then drives molecular pump, opens the high threshold of molecular pump, is evacuated to 3.0 × 10 after molecular pump smooth running
-5pa, then heats stainless steel substrate to temperature required rear insulation;
(5) plasma clean target: pass into Ar gas to vacuum chamber, and control flow and make pressure in vacuum tank be 0.3Pa, treat that Ar airshed is stablized, now Ar airshed is 21.7 ~ 22.5sccm, open grid bias power supply, power is adjusted to 150W, glow discharge produces plasma body, surface cleaning is carried out to stainless steel substrate, after cleaning 10 ~ 30min, closes grid bias power supply; Again respectively to metal titanium targets, metallic silver target, ceramic alumina magnesium target pre-sputtering 10 minutes cleaning targets, sputtering power is 200W;
(6) secondary electron emission thin film deposition: after the cleaning of step (5) target terminates, first opening metal titanium target baffle plate, titanium deposition film, deposition power is 100 ~ 400W, and depositing time is 5 ~ 9min; Close metal titanium targets baffle plate, then opening metal silver target baffle plate, depositing silver film, deposition power is 100 ~ 400W, and depositing time is 25 ~ 45min, closes metallic silver target baffle plate; Open argent and ceramic alumina magnesium two target baffle plate, adjustment ceramic alumina magnesium target radio frequency source power is within the scope of 200W ~ 600W, and meanwhile, adjustment metallic silver target radio frequency power is within the scope of 10W ~ 300W, depositing time is 30 ~ 90min, closes argent and ceramic alumina magnesium two target baffle plate; Open ceramic alumina magnesium target baffle plate, deposited oxide magnesium film, deposition power is 200 ~ 500W, depositing time is 30 ~ 90min, close ceramic alumina magnesium baffle plate, close source of the gas, terminate sample and be coated with, be namely respectively the film system of secondary electron emission function of the hybrid films of metal titanium membrane, metal silverskin, magnesium oxide and argent, pure zirconia magnesium film from down to up.
Step (1), (2) described volatile organic solution are all preferably dehydrated alcohol;
Described stainless steel substrate is No. 304 stainless steel substrates preferably;
In step (2), water used is deionized water purity and above water;
Step (2) the described ultrasonic cleaning time is preferably 15min;
Step (4) is temperature required relevant with the processing parameter of film forming.
Beneficial effect
(1) the film system preparation method with secondary electron emission function of the present invention, utilizes the preparation method of deposit multilayer complex function thin film to replace conventional oxidation process.Prepared film compactness is good, strong adhesion and secondary electron emission rate advantages of higher.
(2) the present invention can deposit secondary electron emission performance and the good secondary electron emission film of anti-sputtering performance on the stainless steel-based end.Can be used in the microelectronic device such as plasma panel, secondary emission multiplier.
Accompanying drawing explanation
Fig. 1 is the secondary electron emission functional film system schematic diagram adopting the method for the invention to prepare.
Embodiment
Below in conjunction with the drawings and specific embodiments in detail the present invention is described in detail, but is not limited thereto.
Embodiment 1
Have a film system preparation method for secondary electron emission function, described method steps is as follows:
(1) clean vacuum room: open vacuum chamber, is placed into directly over target by not contaminated for protection target aluminium film, removes the pollutent in the rete and air come off in vacuum chamber, then dips in dehydrated alcohol wiped clean vacuum chamber inwall with absorbent gauze; Described target has three kinds, is respectively metal titanium targets, metallic silver target, ceramic alumina magnesium target; The purity of described target is more than 99.99%;
(2) substrate is cleaned: No. 304 stainless steel substrates are put into clean vessel, clean with deionized water rinsing, again No. 304 stainless steel substrates are used analytical pure acetone and each ultrasonic cleaning 15min of analytical pure alcohol respectively, then rinse well with analytical pure dehydrated alcohol, with the wiping of chipless cleansing tissue to surperficial no marking, scratch and drop remaining trace;
(3) substrate is filled: No. 304 stainless steel substrates after step (2) being cleaned are put in the substrate frame of vacuum chamber, and remove for the protection of the not contaminated aluminium film of target;
(4) vacuum chamber: open mechanical pump and take out in advance, vacuum tightness is evacuated to 1Pa, then drives molecular pump, opens the high threshold of molecular pump, is evacuated to 3.0 × 10 after molecular pump smooth running
-5pa, then insulation 1 hour after heated substrate to 400 DEG C;
(5) plasma clean target: pass into Ar gas to vacuum chamber, and control flow and make pressure in vacuum tank be 0.3Pa, treat that Ar airshed is stablized, now Ar airshed is 21.7 ~ 22.5sccm, open grid bias power supply, power is adjusted to 150W, glow discharge produces plasma body, surface cleaning is carried out to No. 304 stainless steel substrates, after cleaning 15min, closes grid bias power supply; Again respectively to metal titanium targets, metallic silver target, ceramic alumina magnesium target pre-sputtering 10 minutes cleaning targets, sputtering power is 200W;
(6) secondary electron emission thin film deposition: after the cleaning of step (5) target terminates, first opening metal titanium target baffle plate, titanium deposition film, deposit thickness is 80nm; Close metal titanium targets baffle plate, then opening metal silver target baffle plate, depositing silver film, deposit thickness is 500nm, closes metallic silver target baffle plate; Open argent and ceramic alumina magnesium two target baffle plate, adjustment ceramic alumina magnesium target radio frequency source power is within the scope of 400W, and meanwhile, adjustment metallic silver target radio frequency power is within the scope of 50W, and deposit thickness is 100+50nm, closes argent and ceramic alumina magnesium two target baffle plate; Open ceramic alumina magnesium target baffle plate, deposited oxide magnesium film, thickness is 100nm, close ceramic alumina magnesium baffle plate, close source of the gas, terminate sample to be coated with, be namely respectively the film system of secondary electron emission function of the hybrid films of metal titanium membrane, metal silverskin, magnesium oxide and argent, pure zirconia magnesium film from down to up, as shown in Figure 1;
The present invention includes but be not limited to above embodiment, every any equivalent replacement of carrying out under the principle of spirit of the present invention or local improvement, all will be considered as within protection scope of the present invention.
Claims (5)
1. there is a film system preparation method for secondary electron emission function, it is characterized in that: described method steps is as follows:
(1) clean vacuum room: open vacuum chamber, not contaminated for protection target aluminium film is placed into directly over target, remove the pollutent in the rete and air come off in vacuum chamber, then dip in volatile organic solution wiped clean vacuum chamber inwall with absorbent gauze; Described target has three kinds, is respectively metal titanium targets, metallic silver target, ceramic alumina magnesium target; The purity of described target is more than 99.99%;
(2) substrate is cleaned: stainless steel substrate is put into clean vessel, rinse well with water, again stainless steel substrate is used respectively analytical pure acetone and each ultrasonic cleaning 10 ~ 30min of analytical pure alcohol, then rinse well by the volatile organic solution of analytical pure, with the wiping of chipless cleansing tissue to surperficial no marking, scratch and drop remaining trace;
(3) substrate is filled: the stainless steel substrate after step (2) being cleaned is put in the substrate frame of vacuum chamber, and removes for the protection of the not contaminated aluminium film of target;
(4) vacuum chamber: open mechanical pump and take out in advance, vacuum tightness is evacuated to 1Pa, then drives molecular pump, opens the high threshold of molecular pump, is evacuated to 3.0 × 10 after molecular pump smooth running
-5pa, then heats stainless steel substrate to temperature required rear insulation;
(5) plasma clean target: pass into Ar gas to vacuum chamber, and control flow and make pressure in vacuum tank be 0.3Pa, treat that Ar airshed is stablized, now Ar airshed is 21.7 ~ 22.5sccm, open grid bias power supply, power is adjusted to 150W, glow discharge produces plasma body, surface cleaning is carried out to stainless steel substrate, after cleaning 10 ~ 30min, closes grid bias power supply; Again respectively to metal titanium targets, metallic silver target, ceramic alumina magnesium target pre-sputtering 10 minutes cleaning targets, sputtering power is 200W;
(6) secondary electron emission thin film deposition: after the cleaning of step (5) target terminates, first opening metal titanium target baffle plate, titanium deposition film, deposition power is 100 ~ 400W, and depositing time is 5 ~ 9min; Close metal titanium targets baffle plate, then opening metal silver target baffle plate, depositing silver film, deposition power is 100 ~ 400W, and depositing time is 25 ~ 45min, closes metallic silver target baffle plate; Open argent and ceramic alumina magnesium two target baffle plate, adjustment ceramic alumina magnesium target radio frequency source power is within the scope of 200W ~ 600W, and meanwhile, adjustment metallic silver target radio frequency power is within the scope of 10W ~ 300W, depositing time is 30 ~ 90min, closes argent and ceramic alumina magnesium two target baffle plate; Open ceramic alumina magnesium target baffle plate, deposited oxide magnesium film, deposition power is 200 ~ 500W, depositing time is 30 ~ 90min, close ceramic alumina magnesium baffle plate, close source of the gas, terminate sample and be coated with, be namely respectively the film system of secondary electron emission function of the hybrid films of metal titanium membrane, metal silverskin, magnesium oxide and argent, pure zirconia magnesium film from down to up.
2. a kind of film system preparation method with secondary electron emission function according to claim 1, is characterized in that: step (1), (2) described volatile organic solution are dehydrated alcohol.
3. a kind of film system preparation method with secondary electron emission function according to claim 1, is characterized in that: described stainless steel substrate is No. 304 stainless steel substrates.
4. a kind of film system preparation method with secondary electron emission function according to claim 1, is characterized in that: the water described in step (2) is deionized water purity and above water.
5. a kind of film system preparation method with secondary electron emission function according to claim 1, is characterized in that: step (2) the described ultrasonic cleaning time is 15min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103789730B (en) * | 2014-01-16 | 2015-10-28 | 西安交通大学 | A kind of preparation method of secondary electron emission film |
| CN104362058A (en) * | 2014-10-15 | 2015-02-18 | 兰州空间技术物理研究所 | Curved surface film forming method for dynode of electron multiplier |
| CN105206486A (en) * | 2015-09-11 | 2015-12-30 | 兰州空间技术物理研究所 | Production technology for dynode shell |
| CN105349968A (en) * | 2015-11-19 | 2016-02-24 | 西安交通大学 | Dynode film structure and electron multiplier based on dynode film structure |
| CN105470092A (en) * | 2015-11-19 | 2016-04-06 | 西安交通大学 | Dynode structure and arc dynode electron multiplier based on the same |
| CN107740044B (en) * | 2017-10-11 | 2019-08-23 | 西安交通大学 | Doping metals and the magnesia secondary film of aluminium oxide and preparation method thereof |
| CN107988576A (en) * | 2017-11-30 | 2018-05-04 | 西安交通大学 | A kind of magnesia cermet secondary film and preparation method thereof |
| CN108085651B (en) * | 2017-12-14 | 2020-09-25 | 北京工业大学 | Electron beam bombardment resistant secondary electron emission composite film and preparation method thereof |
| CN109786951A (en) * | 2018-12-20 | 2019-05-21 | 兰州空间技术物理研究所 | A kind of thermoelectricity protection integrated membrane structure |
| CN111748769B (en) * | 2020-06-03 | 2022-08-12 | 西安空间无线电技术研究所 | Method for reducing secondary electron emission coefficient of silver surface high-energy area |
| CN114395747B (en) * | 2021-12-24 | 2023-10-24 | 兰州空间技术物理研究所 | High-emissivity bombardment-resistant secondary electron emission film structure and preparation method |
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| CN102087944B (en) * | 2010-09-30 | 2012-09-05 | 四川虹欧显示器件有限公司 | Composite dielectric protective film of plasma display panel (PDP) and preparation method thereof |
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