CN106637116A - Simple preparation of secondary electron emission film - Google Patents
Simple preparation of secondary electron emission film Download PDFInfo
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- CN106637116A CN106637116A CN201611166493.1A CN201611166493A CN106637116A CN 106637116 A CN106637116 A CN 106637116A CN 201611166493 A CN201611166493 A CN 201611166493A CN 106637116 A CN106637116 A CN 106637116A
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- sputtering
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- simple method
- secondary film
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0089—Reactive sputtering in metallic mode
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
Abstract
The invention discloses a simple preparation of a secondary electron emission film and belongs to the technical field of preparation of secondary electron emission cathode materials. According to the simple preparation of the secondary electron emission film, pure metal of silver/aluminum/titanium serves as a substrate, pure metal of magnesium serves as a sputtering source, pure argon services as working gas and pure oxygen serves as reactant gas; through resistance heating on the substrate and a direct current reaction magnetron sputtering, a MgO film can be prepared from the silver/aluminum titanium substrate and reach a secondary emission coefficient of delta of up to 4.88. MgO film cathodes prepared through the method have the advantages of being simple in preparation, controlled in thickness, uniform in component, good in crystallization, high in secondary emission coefficient, stable in emission performance, resistant to electron bombardment and is promising for the fields such photomultipliers, caesium atomic blocks and magnetrons.
Description
Technical field
The present invention relates to a kind of simple method for preparing of secondary film, and in particular to one kind is with silver/aluminium/titanium
It is that base material adopts magnetron sputtering technique deposition to have the preparation method of the MgO film of excellent secondary electron emissions performance to belong to, and is belonged to
The preparing technical field of secondary cathode material.
Background technology
With the development of electronic information technology, secondary electron emissions material plays more and more important in vacuum electron device
Effect, such as photomultiplier, cesium-beam atomic clock, magnetron be military, Domestic vacuum electronic device.Relative to other secondary emissions
Material, MgO film possesses excellent secondary emission performance, under the conditions of relatively low accelerating potential (200-600eV), secondary emission
Coefficient can maintain more than 3, meet the actual operation requirements of various vacuum electron devices.At present, the side of magnesia film is prepared
Method has various, such as traditional thermal activation treatment, sol-gel process, magnetron sputtering deposition, electron beam evaporation plating.Method for manufacturing thin film
And technique has a direct impact to the pattern of MgO film, structure, surface roughness and film thickness, and then affect its secondary emission
Performance.For example, the secondary emission coefficient of amorphous state MgO film is relatively low, and the crystalline substance of acquisition is deposited under certain substrate temperature conditions
State MgO film then has higher secondary emission coefficient；Relatively thin MgO film easily penetrates into base material by electron beam, and compared with
Thick MgO film is unfavorable for the secondary electron effusion surface of film internal excitation and is unfavorable for benefit of the electronics in cathode surface again
Fill, thus secondary emission coefficient is poor, and only the moderate MgO film of thickness just has comparatively ideal secondary electron emissions system
Number.The traditional preparation methods of MgO film are thermal activation treatment Ag-Mg alloy, and the method can not realize the accurate control of film thickness
System, the secondary emission less stable of the cathode emitter of preparation, the life-span is shorter.MgO film composition prepared by sol-gel process
Complex structure, second-rate, the impact secondary emission coefficient of MgO layer.Using MgO target, magnetic control splashes on metal or glass substrate
Direct precipitation MgO film is penetrated, MgO is usually amorphous state, and secondary emission coefficient is undesirable；And in sputter procedure heat substrate or
Subsequent heat treatment, needs higher temperature to make MgO that crystalline state transformation to occur, and temperature is too high easily makes film separation and fail, into
Film uniformity is poor.
The content of the invention
For traditional bianry alloy thermal activation treatment prepare MgO second emission cathode film thicknesses it is wayward, secondary
The unstable grade deficiency of coefficient is penetrated, the present invention adopts magnetron sputtering technique, using magnesium metal as sputtering source material, be passed through argon gas for work
Make gas, oxygen is reacting gas, and metallic substrates are heated using resistance heating manner, d.c. sputtering magnesium target, in gold
Reactive deposition MgO film on category base material.By adjusting base reservoir temperature and oxygen argon gas stream flow ratio, successfully prepare thickness it is controllable,
Composition is uniform, the MgO film that good crystallinity, secondary emission coefficient are good and stable.The invention provides a kind of preparation technology letter
Singly, film thickness is controllable, secondary emission coefficient is high, emitting performance is stable and the preparation side of the cathode film material of resistance to electron bombardment
Method.
The preparation method of secondary MgO film provided by the present invention is accomplished by：
A. with pure metallic silver, aluminium, titanium as substrate material, Jing surfaces mill, polishing are clear with acetone and alcohol ultrasonic wave afterwards
Wash.With the sputtering source material that simple metal magnesium serves as thin-film material；
B. the base material obtained by Jing steps A is fixed on sample stage, sample stage is put into into magnetic control sputtering device Sample Room, base material
In the once purged feeding rotatable metallic substrate of Sample Room.
C. confined reaction room is vacuumized, metallic substrates is heated；
D. treat that magnetic control sputtering device reative cell back end vacuum is evacuated to a certain degree and metallic substrates in room temperature or are heated to one
Under the conditions of constant temperature degree, the high pure oxygen and argon mixture gas of certain flow ratio are passed through, are gone up to reaction pressure in reative cell vacuum
When start pre-sputtering, pre-sputtering is processed and start after certain hour the sputtering of direct current magnesium target, the magnesium and chamber obtained by argon ion bombardment target
Oxygen reaction in room, finally obtains MgO film in substrate surface deposition.
In said method step A, the purity of the substrate material argent, aluminium, titanium and magnesium metal target is
99.99%.
In said method step A, the surface mill, glossing are：Difference Jing 2000#, 3000#, 5000#SiC sand paper
Polishing Ag/Al/Ti substrate samples are conducive to the adventitious deposit of magnetron sputtering material to obtain smooth planar surface.After Jing third
Ketone and alcohol difference ultrasonic wave cleaning 5min, after vacuum drying chamber drying, to remove sample surfaces adsorbing contaminant.
In said method step B, the cleaning is under an argon atmosphere by radio-frequency power supply in 50～100W power conditions
The argon ion aura cleaning 300s of lower generation.
In said method step C, the vacuum pumping method is vacuumized for molecular pump, and reative cell back end vacuum is 5 × 10-4
～8 × 10-4Pa, the mode of heating of metallic substrates is resistance-type heating, and the rate of heat addition is 20 DEG C/min.
In said method step D, the base reservoir temperature be room temperature sputtering the sample later stage in vacuum tube furnace Jing 400～
600 DEG C, carry out 10～30min activation process under the conditions of the high pure oxygens of 10～20Pa.
In said method step D, the base reservoir temperature is set between 200～500 DEG C, and sputtering source gas high purity oxygen gas are pure
Spend for 99.999%, high-purity argon gas purity is 99.999%.
In said method step D, the gas flow ratio O2/ Ar is 1/90～10/90 (flux unit：Sccm), react
Air pressure is controlled between 0.8～1.0Pa.
In said method step D, the pre-sputtering under conditions of flapper closure, using sputtering 5 under 50～200W power
～10min, to remove target material surface adsorbate and impurity.
In said method step D, the magnetically controlled DC sputtering power is 50～200W.
The present invention finally gives high (the maximum emission ratio δ of secondary emission coefficientmax=4.88), resistance to electron bombardment (once
Electron energy be 400eV constant bombardments after 72 hours maximum secondary emission ratio δ still greater than 3.0), secondary emission stable performance
MgO film negative electrode.Film surface microstructure is in flake shaped particle, and particle is uniformly distributed, size about 50nm～1.5 μm, section
For obvious column crystal.
Description of the drawings
The present invention has 9 accompanying drawings, is now respectively described below：
Fig. 1 is the surface SEM patterns of the made MgO film of embodiment 1；
Fig. 2 is the section SEM patterns of the made MgO film of embodiment 1；
Fig. 3 is the surface SEM patterns of the made MgO film of embodiment 2；
Fig. 4 is the section SEM patterns of the made MgO film of embodiment 2；
Fig. 5 is the primary electron energy-secondary emission coefficient graph of a relation of embodiment 1；
Fig. 6 is the primary electron energy-secondary emission coefficient graph of a relation of embodiment 2；
Fig. 7 is the primary electron energy-secondary emission coefficient graph of a relation of embodiment 3；
Fig. 8 is the primary electron energy-secondary emission coefficient graph of a relation of embodiment 4；
Fig. 9 is that secondary of the embodiment 3 at primary electron constant bombardment MgO film surface of the electron energy for 400eV is sent out
Penetrate life curve figure.
Specific embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following examples.
In following examples argent/aluminium/titanium sheet Jing 2000#, 3000#, 5000#SiC sand paper pretreatment after, Jing acetone and
Alcohol difference ultrasonic wave cleaning 5min, dries stand-by.The size of following substrate material is：10mm×10mm×0.2mm.
Embodiment 1
By grinding and polishing light, simultaneously the cleaned argent base material of ultrasonic wave is put into magnetron sputtering Sample Room, is fixed on high temperature gummed tape
In metallic substrates.The argon ion aura for being produced under 50W power conditions by radio-frequency power supply under an argon atmosphere cleans 300s.It
Afterwards sample is sent into reative cell and is vacuumized, and treats that back end vacuum is reduced to 5 × 10-4Pa, starts to be passed through O2/ Ar mixed gas, O2/ Ar gas
Body flow-rate ratio is 1/90.Question response room vacuum is 1Pa, keeps magnesium target lower section flapper closure, starts direct current pre-sputtering, sputters work(
Rate is 150W, time 300s.Open baffle plate afterwards, formal d.c. sputtering Mg, the time is 60min.Substrate is not heated, and is room temperature 25
℃.Air is filled in sputtering to vacuum chamber after terminating, take out sample.By vacuum tube furnace under 400 DEG C, 20Pa high purity oxygen gas atmosphere
Further activation, treats that furnace temperature drop but takes out sample to less than 60 DEG C.Primary electron energy-secondary emission coefficient figure is shown in Fig. 5, and one
Secondary electron energy be 400eV constant bombardments after 72 hours maximum secondary emission ratio δ still greater than 3.
Embodiment 2
By grinding and polishing light, simultaneously the cleaned argent base material of ultrasonic wave is put into magnetron sputtering Sample Room, is fixed on high temperature gummed tape
In metallic substrates.The argon ion aura for being produced under 50W power conditions by radio-frequency power supply under an argon atmosphere cleans 300s.It
Afterwards sample is sent into reative cell and is vacuumized, and is heated to 400 DEG C to substrate.Treat that back end vacuum is reduced to 5 × 10-4Pa, starts to be passed through
O2/ Ar mixed gas, O2/ Ar gas flow ratios are 1/90.Question response room vacuum is 1Pa, keeps magnesium target lower section flapper closure,
Start direct current pre-sputtering, sputtering power is 150W, time 300s.Baffle plate, formal d.c. sputtering Mg are opened afterwards, and the time is
60min.Air is filled in sputtering after base reservoir temperature is cooled to below 60 DEG C to vacuum chamber after terminating, take out sample.Primary electron energy
Amount-secondary emission coefficient figure is shown in Fig. 6, and primary electron energy is 400eV constant bombardments maximum secondary emission ratio δ after 72 hours
Still greater than 3.
Embodiment 3
By grinding and polishing light, simultaneously the cleaned metal aluminium base of ultrasonic wave is put into magnetron sputtering Sample Room, is fixed on high temperature gummed tape
In metallic substrates.The argon ion aura for being produced under 50W power conditions by radio-frequency power supply under an argon atmosphere cleans 300s.It
Afterwards sample is sent into reative cell and is vacuumized, and is heated to 400 DEG C to substrate.Treat that back end vacuum is reduced to 5 × 10-4Pa, starts to be passed through
O2/ Ar mixed gas, O2/ Ar gas flow ratios are 1/90.Question response room vacuum is 1Pa, keeps magnesium target lower section flapper closure,
Start direct current pre-sputtering, sputtering power is 150W, time 300s.Baffle plate, formal d.c. sputtering Mg are opened afterwards, and the time is
60min.Air is filled in sputtering after base reservoir temperature is cooled to below 60 DEG C to vacuum chamber after terminating, take out sample.Primary electron energy
Amount-secondary emission coefficient figure is shown in Fig. 7, and primary electron energy is 400eV constant bombardments maximum secondary emission ratio δ after 72 hours
Still greater than 3.
Embodiment 4
By grinding and polishing light, simultaneously the cleaned Titanium base material of ultrasonic wave is put into magnetron sputtering Sample Room, is fixed on high temperature gummed tape
In metallic substrates.The argon ion aura for being produced under 50W power conditions by radio-frequency power supply under an argon atmosphere cleans 300s.It
Afterwards sample is sent into reative cell and is vacuumized, and is heated to 400 DEG C to substrate.Treat that back end vacuum is reduced to 5 × 10-4Pa, starts to be passed through
O2/ Ar mixed gas, O2/ Ar gas flow ratios are 1/90.Question response room vacuum is 1Pa, keeps magnesium target lower section flapper closure,
Start direct current pre-sputtering, sputtering power is 150W, time 300s.Baffle plate, formal d.c. sputtering Mg are opened afterwards, and the time is
60min.Air is filled in sputtering after base reservoir temperature is cooled to below 60 DEG C to vacuum chamber after terminating, take out sample.Primary electron energy
Amount-secondary emission coefficient figure is shown in Fig. 8, and primary electron energy is 400eV constant bombardments maximum secondary emission ratio δ after 72 hours
Still greater than 3.
The main scheme for implementing said method of the present invention is the foregoing is only, but the present invention is not limited to this, it is all without departing from this
Any modification, equivalent or improvement for being made in the case of invention core etc., should be included in protection scope of the present invention.
Claims (10)
1. a kind of simple method for preparing of secondary film, it is characterised in that prepare essentially according to the following steps：
A. with pure metallic silver, aluminium, titanium as substrate material, Jing surfaces mill, polishing are cleaned afterwards with acetone and alcohol ultrasonic wave.With
Simple metal magnesium serves as the sputtering source material of thin-film material；
B. the base material obtained by Jing steps A is fixed on sample stage, sample stage is put into into magnetic control sputtering device Sample Room, base material is entering
Specimen chamber is once purged to be sent in rotatable metallic substrate；
C. confined reaction room is vacuumized, metallic substrates is heated；
D. treat that magnetic control sputtering device reative cell back end vacuum is evacuated to a certain degree and metallic substrates in room temperature or are heated to a constant temperature
Under the conditions of degree, the high pure oxygen and argon mixture gas of certain flow ratio are passed through, are opened when reative cell vacuum is gone up to reaction pressure
Beginning pre-sputtering, pre-sputtering is processed and start after certain hour the sputtering of direct current magnesium target, in the magnesium obtained by argon ion bombardment target and chamber
Oxygen reaction, finally substrate surface deposition obtain MgO film.
2. according to claim 1 a kind of secondary film simple method for preparing, it is characterised in that in step A, institute
The purity for stating substrate material argent, aluminium, titanium and magnesium metal target is 99.99%.Surface mill, glossing are：Difference Jing
2000#, 3000#, 5000#SiC sand papering Ag/Al/Ti substrate samples are conducive to magnetron sputtering to obtain smooth planar surface
The adventitious deposit of material.After Jing acetone and alcohol difference ultrasonic wave cleaning 5min, after vacuum drying chamber drying, to remove sample
Product adsorption impurity.
3. according to claim 1 a kind of secondary film simple method for preparing, it is characterised in that in step B, institute
It is that the argon ion aura for being produced under 50～100W power conditions by radio-frequency power supply under an argon atmosphere cleans 300s to state cleaning.
4. according to claim 1 a kind of secondary film simple method for preparing, it is characterised in that in step C, institute
State vacuum pumping method to vacuumize for molecular pump, reative cell back end vacuum is 5 × 10-4～8 × 10-4Pa, the heating of metallic substrates
Mode is resistance-type heating, and the rate of heat addition is 20 DEG C/min.
5. according to claim 1 a kind of secondary film simple method for preparing, it is characterised in that in step D, institute
State base reservoir temperature for room temperature sputtering the sample later stage in vacuum tube furnace under the conditions of 400～600 DEG C of Jing, the high pure oxygens of 10～20Pa
Carry out 10～30min activation process.
6. according to claim 1 a kind of secondary film simple method for preparing, it is characterised in that in step D, institute
State base reservoir temperature to be set between 200～500 DEG C, sputtering source gas high purity oxygen gas purity is 99.999%, high-purity argon gas purity
For 99.999%.
7. according to claim 1 a kind of secondary film simple method for preparing, it is characterised in that in step D, institute
State gas flow ratio O2/ Ar is 1/90～10/90 (flux unit：Sccm), reaction pressure is controlled between 0.8～1.0Pa.
8. according to claim 1 a kind of secondary film simple method for preparing, it is characterised in that in step D, institute
Pre-sputtering is stated under conditions of flapper closure, using 5～10min is sputtered under 50～200W power, to remove target material surface absorption
Thing and impurity.
9. according to claim 1 a kind of secondary film simple method for preparing, it is characterised in that in step D, institute
Magnetically controlled DC sputtering power is stated for 50～200W.
10. secondary film is prepared according to claim 1-9 any one preparation method.
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| CN201611166493.1A CN106637116B (en) | 2016-12-16 | 2016-12-16 | A kind of simple preparation method of secondary film |
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| CN201611166493.1A CN106637116B (en) | 2016-12-16 | 2016-12-16 | A kind of simple preparation method of secondary film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085651A (en) * | 2017-12-14 | 2018-05-29 | 北京工业大学 | A kind of secondary laminated film of resistance to beam bombardment and preparation method thereof |
| CN113471034A (en) * | 2021-05-29 | 2021-10-01 | 南京三乐集团有限公司 | Preparation method of magnesium oxide secondary emitter |
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| CN103243305A (en) * | 2013-04-22 | 2013-08-14 | 兰州空间技术物理研究所 | Secondary electron emission film preparation method |
| CN103726026A (en) * | 2014-01-10 | 2014-04-16 | 中国科学院长春光学精密机械与物理研究所 | Method of preparing thin film by magnetron sputtering of oxide ceramic target |
| CN103924205A (en) * | 2014-04-28 | 2014-07-16 | 中国人民解放军国防科学技术大学 | High temperature-resistant low-infrared emittance composite coating and preparation method thereof |
| CN104593742A (en) * | 2015-01-20 | 2015-05-06 | 清华大学深圳研究生院 | Equipment and method for preparing oxide film with biaxial texture |
-
2016
- 2016-12-16 CN CN201611166493.1A patent/CN106637116B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103243305A (en) * | 2013-04-22 | 2013-08-14 | 兰州空间技术物理研究所 | Secondary electron emission film preparation method |
| CN103726026A (en) * | 2014-01-10 | 2014-04-16 | 中国科学院长春光学精密机械与物理研究所 | Method of preparing thin film by magnetron sputtering of oxide ceramic target |
| CN103924205A (en) * | 2014-04-28 | 2014-07-16 | 中国人民解放军国防科学技术大学 | High temperature-resistant low-infrared emittance composite coating and preparation method thereof |
| CN104593742A (en) * | 2015-01-20 | 2015-05-06 | 清华大学深圳研究生院 | Equipment and method for preparing oxide film with biaxial texture |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085651A (en) * | 2017-12-14 | 2018-05-29 | 北京工业大学 | A kind of secondary laminated film of resistance to beam bombardment and preparation method thereof |
| CN113471034A (en) * | 2021-05-29 | 2021-10-01 | 南京三乐集团有限公司 | Preparation method of magnesium oxide secondary emitter |
| CN113471034B (en) * | 2021-05-29 | 2023-11-14 | 南京三乐集团有限公司 | Preparation method of magnesium oxide secondary emitter |
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