CN107546100A - Xenon lamp Excimer UV photooxidation vacuum equipment and its application method - Google Patents
Xenon lamp Excimer UV photooxidation vacuum equipment and its application method Download PDFInfo
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- CN107546100A CN107546100A CN201610473918.7A CN201610473918A CN107546100A CN 107546100 A CN107546100 A CN 107546100A CN 201610473918 A CN201610473918 A CN 201610473918A CN 107546100 A CN107546100 A CN 107546100A
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Abstract
A kind of xenon lamp Excimer UV photooxidation vacuum equipment provided by the invention and its application method, including：Vacuum chamber, controlling organization is provided with vacuum chamber；Xenon lamp quasi-molecule discharging tube, xenon lamp quasi-molecule discharging tube are arranged on inside vacuum chamber, and water cooling plant is provided with xenon lamp quasi-molecule discharging tube, and xenon lamp quasi-molecule discharging tube is connected with controlling organization；Specimen holder, bottom of the specimen holder from outside through vacuum chamber enters inside vacuum chamber, and specimen holder is parallel with xenon lamp quasi-molecule discharging tube；Oxygen intake, nitrogen inlet and exhaust outlet, oxygen intake, nitrogen inlet and exhaust outlet are arranged in the side wall of vacuum chamber, and oxygen intake, nitrogen inlet and exhaust outlet connect with the inner chamber of vacuum chamber；Set-up of control system is on vacuum chamber.Compared with prior art, beneficial effects of the present invention are as follows：Using xenon lamp quasi-molecule discharging tube, it launches the ultraviolet light of 172nm wavelength, by regulating and controlling oxygen content in vacuum chamber, you can realize high intensity ultraviolet photooxidation to material surface at normal temperatures.
Description
Technical field
Surface clean or oxide etch that a kind of new ultra-violet Photoxidation Methods improve material are the present invention relates to the use of, more
Specifically, it is related to a kind of xenon lamp Excimer UV photooxidation vacuum equipment and its application method.
Background technology
During using low pressure mercury lamp as the ultraviolet oxidation of light source, 184.9nm and 253.7nm ultraviolet radiation
Oxygen can be decomposed into generation oxygen exciton and ozone molecule, oxygen atom has very strong oxidisability, can effectively remove big
The organic pollution of most metals, semiconductor and insulating materials, prepared in Material growth, surface modification and device etc.
Basic research and industry application field play an important role.Ultraviolet oxidation method not only there is cleaning to imitate substrate
Should, the strong oxidizing property of oxygen atom can also be by the oxidation of some metal materials (for example silver, aluminium etc.) or by carbon family material
Expect (such as graphene, CNT) etching, realize material modification and functionalization.In the past few years, Wo Menfa
The ultraviolet oxidation vacuum equipment technology (patent No. using low pressure mercury lamp as light source is opened up：ZL201310242512.4,
ZL201210462171.7, ZL201210442424.4).For single chamber hardware (patent No.：
ZL201310242512.4), when oxygen content is 1atm in chamber, it is relative to ultraviolet light in air ambient
Oxide etch intensity significantly increases, and 200W luminous powers, which can etch, removes bilayer graphene film.By using dual cavity
Structure, light source and sample stage are located at exocoel and inner cavity chamber respectively, and ultraviolet light is transmitted to inner chamber by quartz window
Room, when base reservoir temperature is increased into 150 DEG C, its photooxidation etching intensity drastically strengthens.When oxygen pressure is 1atm
When, can etching removes more than ten layers graphene films after ultraviolet light 8min.The ultraviolet oxidation process
With accurate controllability, and realize and merged with electrical properties in-situ test and chemical gaseous phase annealing technology.However,
Due to the presence of quartz window, ultraviolet light can be partially absorbed by the subject when through quartz window, will result at room temperature
Photochemical reaction intensity is extremely faint, and the change of single-layer graphene film is not seen from light microscope.Moreover,
Ultraviolet oxidation equipment using low pressure mercury lamp as light source (200W), it is at most only capable of etching away list in air ambient
Layer graphene film, and can be with serious temperature-rise effect；Although by further improving oxygen content, Ke Yizeng
Big photooxidation etching degree, but it is difficult to etch away more than three layers of graphene.
The content of the invention
For in the prior art the defects of, it is an object of the invention to provide one kind to overcome material surface cleaning, oxidation
The xenon lamp Excimer UV photooxidation vacuum equipment and its application method of problem present in modified and etching.
In order to solve the above technical problems, a kind of xenon lamp Excimer UV photooxidation vacuum equipment provided by the invention, bag
Include：Vacuum chamber, controlling organization is provided with vacuum chamber；Xenon lamp quasi-molecule discharging tube, xenon lamp quasi-molecule discharging tube
It is arranged on inside vacuum chamber, water cooling plant, xenon lamp quasi-molecule discharging tube and control is provided with xenon lamp quasi-molecule discharging tube
Mechanism connects；Specimen holder, bottom of the specimen holder from outside through vacuum chamber enters inside vacuum chamber, and sample
Frame is parallel with xenon lamp quasi-molecule discharging tube；Oxygen intake, nitrogen inlet and exhaust outlet, oxygen intake, nitrogen inlet and
Exhaust outlet is arranged in the side wall of vacuum chamber, and the inner chamber of oxygen intake, nitrogen inlet and exhaust outlet and vacuum chamber connects
It is logical；Set-up of control system is on vacuum chamber.
Preferably, a length of 172nm of ultraviolet light wave of xenon lamp quasi-molecule discharging tube transmitting.
Preferably, control system includes mechanical pump, vacuum meter and the barometer being separately positioned on vacuum chamber.
Preferably, in addition to electrical interface, electrical interface are arranged in the side wall of vacuum chamber.
Preferably, in addition to spare interface, spare interface are arranged in the side wall of vacuum chamber.
Preferably, temperature control system is set in specimen holder.
Preferably, specimen holder includes control-rod and is arranged on the sample stage of control boom end；Wherein sample stage and xenon lamp
Quasi-molecule discharging tube is parallel；Control-rod moves along vertical direction in the range of 5mm~100mm.
Preferably, the material of vacuum chamber is stainless steel.
A kind of application method of xenon lamp Excimer UV photooxidation vacuum equipment, comprises the following steps：
Step 1, nitrogen is filled with vacuum chamber until vacuum chamber room pressure stops being filled with nitrogen after being more than an atmospheric pressure
Gas, open vacuum chamber door；
Step 2, sample is positioned on specimen holder, adjusts sample and the distance of xenon lamp quasi-molecule discharging tube lower surface is
11mm, close vacuum chamber door；
Step 3, mechanical pump is opened until the gas pressure intensity in vacuum chamber reaches 3Pa；
Step 4, it is passed through the oxygen of predetermined value pressure；
Step 5, nitrogen is passed through until the air pressure in vacuum chamber is 1atm；
Step 6, xenon lamp quasi-molecule discharging tube irradiation 15min is opened；
Step 7, mechanical pump and exhaust outlet are opened until the gas pressure intensity in vacuum chamber drops to 3Pa；
Step 8, mechanical pump is closed.
Preferably, in step 4, predetermined value 0.2atm, 4kPa or 7Pa.
Compared with prior art, beneficial effects of the present invention are as follows：Using xenon lamp quasi-molecule discharging tube, it is launched
The ultraviolet light of 172nm wavelength, by regulating and controlling oxygen content in vacuum chamber, you can real to material surface at normal temperatures
Existing high intensity ultraviolet photooxidation.
There is the ultraviolet oxidation performance of high intensity at normal temperatures, change on the cleaning of the dry method of material and device, surface
Property and graphical etching field have important value, have important application in material, electronic technology field.
Brief description of the drawings
By reading the detailed description made with reference to the following drawings to non-limiting example, further feature of the invention
Objects and advantages will become more apparent upon.
Fig. 1 is xenon lamp Excimer UV photooxidation vacuum device structure schematic diagram of the present invention；
Fig. 2 is that the application method of xenon lamp Excimer UV photooxidation vacuum equipment of the present invention is filled respectively in nitrogen atmosphere
Enter under 4kPa Oxygen Conditions pattern before (1atm) xenon lamp Excimer UV photooxidation etches graphenic surface to show
It is intended to；
Fig. 3 is that the application method of xenon lamp Excimer UV photooxidation vacuum equipment of the present invention is filled respectively in nitrogen atmosphere
Enter under 4kPa Oxygen Conditions pattern after (1atm) xenon lamp Excimer UV photooxidation etches graphenic surface to show
It is intended to；
Fig. 4 is that the application method of xenon lamp Excimer UV photooxidation vacuum equipment of the present invention is filled respectively in nitrogen atmosphere
Enter under 7Pa Oxygen Conditions pattern before (1atm) xenon lamp Excimer UV photooxidation etches graphenic surface to illustrate
Figure；
Fig. 5 is that the application method of xenon lamp Excimer UV photooxidation vacuum equipment of the present invention is filled respectively in nitrogen atmosphere
Enter under 7Pa Oxygen Conditions pattern after (1atm) xenon lamp Excimer UV photooxidation etches graphenic surface to illustrate
Figure.
In figure：
1- vacuum chamber 2- xenon lamp quasi-molecule discharging tube 3- oxygen intakes
4- nitrogen inlet 5- exhaust outlet 6- mechanical pumps
7- vacuum meter 8- barometer 9- spare interfaces
10- control-rod 11- sample stage 12- electrical interfaces
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the skill of this area
Art personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that to this area
Those of ordinary skill for, without departing from the inventive concept of the premise, some changes and improvements can also be made.
These belong to protection scope of the present invention.
Research is found：In air atmosphere, due to strong absorption of the oxygen to 172nm photons, power is 1kW's
Xenon lamp excimer light source does not produce etching substantially to the graphene film at 5mm distances.Research also found：With low
Pressure mercury lamp is the ultraviolet oxidation equipment of light source (200W), and it is at most only capable of etching away individual layer stone in air ambient
Black alkene film, and can be with serious temperature-rise effect；Although by further improving oxygen content, light can be increased
Oxide etch degree, but it is difficult to etch away more than three layers of graphene.
And xenon lamp quasi-molecule discharging tube can launch wavelength be 172nm ultraviolet light, this high-energy photons can not only
Oxygen is decomposed into generation oxygen exciton and ozone molecule, additionally it is possible to excite more organic molecule materials, have stronger
Oxidisability.Thus, the side etched using the Strong oxdiative of xenon lamp Excimer UV photooxidation vacuum equipment realization at room temperature
Method, its efficiency in traditional material surface clean will be effectively improved, and open up and change in new material and device surface
The application in property field.
As shown in figure 1, a kind of xenon lamp Excimer UV photooxidation vacuum equipment provided by the invention is mainly by vacuum chamber
Room 1, ultraviolet light source system and vacuum equipment monitoring system composition.Wherein, vacuum chamber 1 has stainless steel material to be made,
Inner tip placement xenon lamp quasi-molecule discharging tube 2, sample stage 11 is located at below light source, and it is with sample distance by control-rod
10 are adjusted in the range of 5mm~100mm, and inside is equipped with temperature control system, and temperature control system includes heating (up to 200 DEG C)
And water-cooling system；There are oxygen intake 3, nitrogen inlet 4 and exhaust outlet 5 in the two side of vacuum chamber 1.Ultraviolet light source system
Including xenon lamp quasi-molecule discharging tube 2 and controlling organization, ultraviolet light source system has water cooling plant, and its launch wavelength is mainly
172nm ultraviolet light.When the oxygen that certain pressure intensity is filled with vacuum chamber 1, it generates ozone after ultraviolet light
And oxygen atom, and photochemical reaction occurs with sample surfaces, reach the purpose of cleaning or oxide etch.Vacuum equipment controls
System includes vacuum meter 7, barometer 8 and vacuum mechanical pump 6, and vacuum mechanical pump 6 can realize 2.5Pa vacuum,
Vacuum chamber 1 can also be filled with the gas no more than 1.5atm, can the effective content of control chamber indoor oxygen and nitrogen.
Vacuum chamber 1 is single-chamber cell structure, made by stainless steel material that vacuum chamber 1 is rectangular parallelepiped structure, and front side has
Closure.Its inner cavity chamber's overall width is 350mm, depth 250mm, is highly 320mm, wall thickness 8mm.Its
Xenon lamp quasi-molecule discharging tube 2 is fixed in upper surface, and lower surface is equipped with liftable sample stage 11, side be equipped with oxygen intake 3,
Nitrogen inlet 4 and exhaust outlet 5.Sample stage 11 has temperature control system, and it can be from ultraviolet oxidation equipment body bottom
Into vacuum chamber 1, and it is manipulated in the range of vertical direction 95mm by control-rod 10 and moved.Sample stage 11
For rectangle, it is grown and wide respectively 200mm and 100mm, built-in electric wire, heating coil and water cooling plant, passes through control
The inner chamber of bar 10 processed is connected with external vacuum control system and electronic equipment.The length of control-rod 10 is 350mm, and external diameter is
There are corresponding with quill shaft screw thread and stuck point in 12mm, side end face, can lifted in the range of 95mm.
Ultraviolet light source system includes controlling organization and xenon lamp quasi-molecule discharging tube 2.Controlling organization can control ultraviolet source
Switch, radiation intensity, radiated time etc..Xenon lamp quasi-molecule discharging tube 2 can launch wavelength be mainly the ultraviolet of 172nm
Light, its power tube diameter 30mm, are shaped as tubular structure from 0 to 4kW continuously adjustabes.Ultraviolet lamp tube both ends lead to
Cross the two sides that insulated enclosure set is fixed on vacuum chamber 1.The inside of xenon lamp quasi-molecule discharging tube 2 has water cooling plant, main
It is used to prevent from bursting caused by the constantly rise of ultraviolet lamp tube temperature.
Control system mainly includes vacuum mechanical pump 6, vacuum meter 7 and barometer 8.Chamber is filled with by gas valve control
Interior gas, vacuum and gas content are monitored by vacuum meter 7 and barometer 8 respectively in chamber, base vacuum in chamber
Degree can reach 3Pa, and chamber interior maximum functional pressure is 1.5atm.Can effectively it be let out with discharge gas gas outlet
Pressure.
The rear end face of vacuum chamber 1 has the electrical interface 12 and gas for carrying out the electrical testing function of electronic component in chamber
Spare interface 9.
For the above-mentioned ultraviolet oxidation vacuum equipment using quasi-molecule discharging tube as light source, below by taking graphene film as an example,
Illustrate by controlling oxygen content to significantly improve its oxide etch performance, its key step and result are as follows：
Step 1, main power source and vacuum meter 7 are opened successively, open the valve of nitrogen inlet 4, nitrogen is filled with vacuum chamber
In room 1.The valve of nitrogen inlet 4 is closed after air pressure is slightly above an atmospheric pressure, opens vacuum chamber 1.
Step 2, the SiO for having mechanical stripping graphene will be shifted2/ Si substrates are positioned on sample stage 11, regulation sample with
The distance of ultraviolet lamp tube lower surface is 11mm, closes vacuum chamber 1.
Step 3, the water-cool control and temperature control system and the power supply of mechanical pump 6 of vacuum chamber 1 are opened successively, treat that vacuum reaches
To after 3Pa, vacuum extraction valve is closed.
Step 4, the charge valve and gas flow meter of oxygen intake 3 is opened, when air pressure in cavity is 1atm, is closed
Oxygen intake 3 fills valve.
Step 5, ultraviolet lamp tube main power source is opened, the power (1kW) of xenon lamp quasi-molecule discharging tube 2 is set, starts ultraviolet light
Irradiation switch.
Step 6, after ultraviolet light 15min, xenon lamp control power supply is closed.
Step 7, mechanical pump 6 and vacuum valve are opened successively, after air pressure is down to 3Pa in vacuum chamber 1, are closed true
Empty valve and mechanical pump 6.
Step 8, repeat step (1)-(3), sample is taken out, and places fresh sample.
Step 9, oxygen aerating valve and gas flow meter is opened, when air pressure in cavity is predetermined value (0.2atm is followed successively by,
4kPa and 7Pa) oxygen input valve is closed, opening nitrogen input valve makes chamber pressure be 1atm.As Fig. 2, Fig. 3,
Shown in Fig. 4 and Fig. 5, it can be seen that by the optical morphology figure under more different air pressure：Under room temperature condition, oxygen
Content can etch away eight layer graphene films when being 7Pa, oxygen content is only capable of etching away individual layer when increasing to 4kPa
Graphene film.If oxygen content continues to increase to 0.2atm, graphene, which can not substantially be etched, (is not put into etching
Front and rear shape appearance figure).
Step 10, repeat step (5)-(7).
Step 11, mechanical pump 6 is closed, closes barometer 8, water-cool control and temperature control system successively.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in upper
Particular implementation is stated, those skilled in the art can make a variety of changes or change within the scope of the claims,
This has no effect on the substantive content of the present invention.In the case where not conflicting, in embodiments herein and embodiment
Feature can be arbitrarily mutually combined.
Claims (10)
- A kind of 1. xenon lamp Excimer UV photooxidation vacuum equipment, it is characterised in that including：Vacuum chamber, controlling organization is provided with vacuum chamber；Xenon lamp quasi-molecule discharging tube, xenon lamp quasi-molecule discharging tube are arranged on inside vacuum chamber, in xenon lamp quasi-molecule discharging tube Interior to be provided with water cooling plant, xenon lamp quasi-molecule discharging tube is connected with controlling organization；Specimen holder, bottom of the specimen holder from outside through vacuum chamber enters inside vacuum chamber, and specimen holder and xenon Lamp quasi-molecule discharging tube is parallel；Oxygen intake, nitrogen inlet and exhaust outlet, oxygen intake, nitrogen inlet and exhaust outlet are arranged on vacuum chamber In side wall, oxygen intake, nitrogen inlet and exhaust outlet connect with the inner chamber of vacuum chamber；Set-up of control system is on vacuum chamber.
- 2. xenon lamp Excimer UV photooxidation vacuum equipment according to claim 1, it is characterised in that accurate point of xenon lamp The a length of 172nm of ultraviolet light wave of electron-discharge tube transmitting.
- 3. xenon lamp Excimer UV photooxidation vacuum equipment according to claim 1, it is characterised in that control System includes mechanical pump, vacuum meter and the barometer being separately positioned on vacuum chamber.
- 4. xenon lamp Excimer UV photooxidation vacuum equipment according to claim 1, it is characterised in that also wrap Electrical interface is included, electrical interface is arranged in the side wall of vacuum chamber.
- 5. xenon lamp Excimer UV photooxidation vacuum equipment according to claim 1, it is characterised in that also wrap Spare interface is included, spare interface is arranged in the side wall of vacuum chamber.
- 6. xenon lamp Excimer UV photooxidation vacuum equipment according to claim 1, it is characterised in that in sample Temperature control system is set in product frame.
- 7. xenon lamp Excimer UV photooxidation vacuum equipment according to claim 1, it is characterised in that sample Frame includes control-rod and is arranged on the sample stage of control boom end；Wherein sample stage is parallel with xenon lamp quasi-molecule discharging tube； Control-rod moves along vertical direction in the range of 5mm~100mm.
- 8. xenon lamp Excimer UV photooxidation vacuum equipment according to claim 1, it is characterised in that vacuum The material of chamber is stainless steel.
- 9. a kind of application method of xenon lamp Excimer UV photooxidation vacuum equipment, it is characterised in that including following step Suddenly：Step 1, nitrogen is filled with vacuum chamber until vacuum chamber room pressure stops being filled with nitrogen after being more than an atmospheric pressure Gas, open vacuum chamber door；Step 2, sample is positioned on specimen holder, adjusts sample and the distance of xenon lamp quasi-molecule discharging tube lower surface is 11mm, close vacuum chamber door；Step 3, mechanical pump is opened until the gas pressure intensity in vacuum chamber reaches 3Pa；Step 4, it is passed through the oxygen of predetermined value pressure；Step 5, nitrogen is passed through until the air pressure in vacuum chamber is 1atm；Step 6, xenon lamp quasi-molecule discharging tube irradiation 15min is opened；Step 7, mechanical pump and exhaust outlet are opened until the gas pressure intensity in vacuum chamber drops to 3Pa；Step 8, mechanical pump is closed.
- 10. the application method of xenon lamp Excimer UV photooxidation vacuum equipment according to claim 9, its feature exist In, in step 4, predetermined value 0.2atm, 4kPa or 7Pa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113367268A (en) * | 2021-03-18 | 2021-09-10 | 郑州圣华药物食品技术开发有限公司 | Pulsed ozone disinfection and washing food cabinet excited by xenon excimer light source |
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| JPH01183809A (en) * | 1988-01-19 | 1989-07-21 | Babcock Hitachi Kk | Photo assisted cvd system |
| CN1511339A (en) * | 2001-04-06 | 2004-07-07 | ���������ƴ���ʽ���� | Ultraviolet ray assisted processing deivce for semiconductor processing |
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| CN113367268A (en) * | 2021-03-18 | 2021-09-10 | 郑州圣华药物食品技术开发有限公司 | Pulsed ozone disinfection and washing food cabinet excited by xenon excimer light source |
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