CN102983064A - Vacuum equipment with ultraviolet light/ ozone surface treatment and electrical property in-situ test integrated - Google Patents
Vacuum equipment with ultraviolet light/ ozone surface treatment and electrical property in-situ test integrated Download PDFInfo
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- CN102983064A CN102983064A CN2012104424244A CN201210442424A CN102983064A CN 102983064 A CN102983064 A CN 102983064A CN 2012104424244 A CN2012104424244 A CN 2012104424244A CN 201210442424 A CN201210442424 A CN 201210442424A CN 102983064 A CN102983064 A CN 102983064A
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Abstract
The invention discloses vacuum equipment with ultraviolet light/ ozone surface treatment and an electrical property in-situ test integrated. The vacuum equipment with the ultraviolet light/ ozone surface treatment and the electrical property in-situ test integrated mainly comprises a vacuum chamber, an ultraviolet source system, a vacuum pump system, vacuum equipment control system and an electronic component test system. The vacuum chamber is composed of an upper vacuum inner chamber and a lower vacuum outer chamber. An ultraviolet lamp source is fixed at the top end of the outer chamber. An adjustable sample table is arranged in the inner chamber and a heating and water cooling system is arranged inside the inner chamber. The vacuum equipment with the ultraviolet light/ ozone surface treatment and the electrical property in-situ test integrated is capable of precisely controlling a surface treatment process of materials, such as grapheme, by ultraviolet light/ ozone. In situ measurement and characterization of electrical properties of a micro-nano electronic component are achieved. Application value in surface cleaning and modification of the materials and electrical property in situ characterization of the electronic component is important.
Description
Technical field
The present invention relates to the UV/ozone process for treating surface, in particular, relate to a kind of vacuum equipment that collects UV/ozone surface treatment and electrical properties in-situ test.
Background technology
The UV/ozone process for treating surface can effectively be removed the organic pollution of most metals, semiconductor and insulating material, plays an important role in the basic scientific research such as Material growth, surface modification and device preparation and industry application.This technique functions comes from nineteen seventies, and it is initially the UV-irradiation air or oxygen, and progressively develop into the vacuum ultraviolet (VUV) cleaning technique with gases such as further reduction water in air vapour, nitrogen dioxide on photochemically reactive impact; On scale, also develop to high-power automatic transmission cleaning equipment from initial small-power substrate cleaning equipment.This ultraviolet lighting cleaning equipment mainly is based on low pressure mercury lamp can launch the ultraviolet light that main wavelength is positioned at 184.9nm and 253.7nm, oxygen generates oxygen atom and ozone under the irradiation of these two kinds of ultraviolet lights, and with the organic molecule generation photochemical reaction that is in excitation state, generate the materials such as water and carbon dioxide, reach the purpose of surface clean.
The UV/ozone process for treating surface not only has the cleaning effect to substrate, the strong oxidizing property of oxygen atom can also with some metal materials (for example silver, aluminium etc.) oxidation or etching carbon group material (such as Graphene, carbon nano-tube etc.) surface, realize material modification.In this photochemical treatment process, the impact that reduces as far as possible non-oxygen molecule in the environment is most important to obtaining high-quality sample.For the vacuum ultraviolet (VUV) cleaning technique, be about to uviol lamp and specimen holder and place same vacuum chamber, input the oxygen of certain pressure intensity again and open UV-irradiation after reaching certain base vacuum degree when indoor, this technology can effectively be removed the impact of steam and other non-carrier of oxygen of absorption in the chamber.
Also there is significant limitation the UV/ozone modification technology in itself: at first, ultraviolet lamp tube and sample are placed same chamber, the volume of meeting augmenting response chamber is unfavorable for accurately controlling photochemically reactive process and precision.Secondly, UV-irradiation can cause the fluctuating of ambient temperature, and then can cause ozone decomposed to become the speed of oxygen atom to rise and fall, thereby affects the process of uviol lamp/ozone surface modification.
UV/ozone photochemical reaction technology is for the surface treatment process of carbon group element, not only have surface clean and charge carrier doping effect, and when surface organic matter disappeared totally, they can produce etching effect to it again, and its sheet resistance is sharply increased.Take the research of Graphene as example, after we knew that carbon group element is through the UV/ozone modification, if be exposed in the atmospheric environment, its surface is gas and the impurity in (a few minutes) absorbed air rapidly, and this is unfavorable for the accurate sign of modifying process.If the electric property of energy in-situ test electronic component in the UV/ozone modifying process, we just can control accurately and characterize modifying process.For this reason, we must consider the compatibility of this original position electrical properties measuring technology and UV/ozone technology, thereby our design has been proposed higher or more special requirement.
Summary of the invention
The present invention is directed to the technical problem that exists in the above-mentioned prior art, a kind of vacuum equipment that collects UV/ozone surface treatment and electrical properties in-situ test is provided, overcome the problem that exists in the existing sample surfaces modification technology, realize a kind of vacuum equipment that UV/ozone modification and electronic component performance are tested that integrates, it can accurately control photochemically reactive process, and conduction property (comprising high temperature) that can the in-situ investigation electronic component, have important value aspect dry method cleaning, surface modification and the electrical properties sign of materials and devices.
For achieving the above object, the technical solution adopted in the present invention is as follows:
A kind of vacuum equipment that collects UV/ozone surface treatment and electrical properties in-situ test, mainly by vacuum chamber, ultraviolet light source system, vacuum pump system and vacuum equipment control system and electronic components test system form, wherein, described ultraviolet light source system comprises control power supply and ultraviolet lamp tube, described vacuum chamber comprises outer chamber and inner cavity chamber, the described ultraviolet lamp tube of described exocoel indoor location, sample stage and heating and water cooling plant are set in the described inner cavity chamber, and has a gas input, output port, the light of described ultraviolet lamp tube emission is by the quartz window of inner cavity chamber, shine on the sample stage, described inner cavity chamber has the oxygen of certain pressure intensity, it cleans and modification the sample surfaces on the sample stage through generating ozone and oxygen atom after the UV-irradiation; Described vacuum pump system and vacuum equipment control system for generation of and control vacuum degree in the vacuum chamber, described electronic components test system can carry out to the electrical properties of electronic component in-situ test and characterize.
Described ultraviolet lamp tube emission is mainly the ultraviolet light of 184.9nm and 253.7nm.
Described inner cavity chamber is mainly made by quartz material on top, the bottom is mainly stainless steel material and makes, the inner cavity chamber top has the quartz window at wavelength 184.9nm and 253.7nm place high permeability, the size of described quartz window is not less than the aperture, inside of inner cavity chamber, effectively to avoid the generation of inner cavity chamber's oxygen photochemical reaction dark space under UV-irradiation, described gas input, output port are arranged on inner cavity chamber's bottom stainless steel parts.
The height of described sample stage can be regulated within the specific limits by control lever, to realize and effectively control UV/ozone surface treatment.
Described vacuum pump is by two-stage (two-speed) pump, and namely mechanical pump and molecular pump form.
Described vacuum equipment control system mainly comprises: gas flowmeter, vacuum gauge, temperature control system and water-cooling system.
Described electronic components test system mainly comprises: lock-in amplifier, voltage source and galvanometer, can carry out in-situ characterization to the electrical properties of electronic component.
Compared with the prior art, the present invention has following beneficial effect:
Technical scheme provided by the present invention, integrate UV/ozone surface treatment and electronic component in-situ testing technique, the process for treating surface of this UV/ozone not only can accurately be controlled modifying process, but also can realize in-situ investigation and the sign of electrical properties under normal temperature and the high temperature, have important application at material, electronic technology field.
The present invention adopts the vacuum system of dual cavity, is about to ultraviolet lamp tube and sample stage and places respectively outer chamber and inner cavity chamber, and give effective control by heating and water-cooling system to the sample stage temperature, thereby can better control photochemical reaction process.
Description of drawings
Fig. 1 represents vacuum device structure schematic diagram of the present invention.
Fig. 2 is the ceramic base structural representation that is installed with on the sample stage.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail:
Designed vacuum device structure mainly is comprised of vacuum chamber, ultraviolet light source system, vacuum pump system and vacuum equipment control system, electronic components test system as shown in Figure 1 among the present invention.
1. ultraviolet light source system comprises control power supply and ultraviolet lamp tube 1.
Control power supply and can control the switch of uviol lamp, radiation intensity, radiated time etc.Ultraviolet lamp tube is low pressure mercury lamp, it at first is fixed on the aluminum reflector, and then reflector is fixed in the outer chamber top, and light source can be launched the ultraviolet light that is mainly 184.9nm and 253.7nm.
2. vacuum chamber comprises outer chamber 2 and inner cavity chamber 3.
Quartz window 4 clear light sizes are not less than inner cavity chamber's internal diameter, are fixed on the steel flange, can see through 184.9nm and 253.7nm ultraviolet light, reduce the inhomogeneities of inner cavity chamber's ozone generating.
Inner cavity chamber's sample stage 5 is mainly made by stainless steel material, is connected with external control system by control lever 6, and its built-in circuit lead-in wire and heating and water-cooling system can liftings in the 60mm scope, are 10mm apart from quartz window lower surface minimum distance.
Inner cavity chamber's 3 bottom stainless steel parts have gas input port, output port.
3. vacuum pump system 7:
By two-stage (two-speed) pump, namely mechanical pump and molecular pump form, and the base vacuum degree can reach 2*10
-4Pa.
4. the vacuum equipment control system 8:
Mainly comprise gas flowmeter, vacuum gauge, temperature control system and water-cooling system.
When inner cavity chamber was filled with certain gas, gas flowmeter can be controlled the flow of inflow gas, and the vacuum degree of inner cavity chamber can be detected by high and low vacuum gauge.
5. electronic components test system 9:
The electronic components test system mainly provides lock-in amplifier, voltage source and galvanometer, can carry out in-situ characterization to the electrical properties of electronic component.
For the above-mentioned equipment that integrates UV/ozone surface modification and electronic components test system, the below specifies the key step to its surface modification and test take the graphene nano electronic component as example:
1) open main power source and vacuum gauge, open the nitrogen valve, nitrogen is filled with in the vacuum chamber, air pressure is closed the nitrogen valve after surpassing an atmospheric pressure, opens successively outer chamber and inner cavity chamber.
2) the Graphene electronic component is connected on the chip carrier (chipcarrier), then inserts on the ceramic bases socket, by control lever sample stage is placed inner cavity chamber, close successively inside and outside Pit cover.
3) open successively water-cooling system and the mechanical pump power supply of inner cavity chamber's sample stage, after vacuum degree is higher than 1Pa, open molecular pump.
4) inner cavity chamber's base vacuum degree reaches 2*10
-4Behind the Pa, open the electronic components test system power supply, the conductivity at room temperature performance before test Graphene nanoelectronic element surface is processed in the high vacuum environment.
5) closure molecule pump and inner cavity chamber's gas output valve are opened the oxygen gas flowmeter.Inner cavity chamber closes the gas input valve door after reaching 1 atmospheric pressure, opens the ultraviolet lamp tube main power source, and intensity of illumination and time are set, and starts the ultraviolet irradiation switch.
6) after the ultraviolet lamp tube irradiation finishes, close the ultraviolet lamp tube main power source, open inner cavity chamber's gas output valve, open molecular pump after vacuum degree reaches 1Pa, vacuum degree reaches 2*10
-4Again test the electric conductivity of Graphene electronic component behind the Pa, characterize the UV/ozone modification to the impact of Graphene element electric conductivity.
7) successively closure molecule pump and mechanical pump.Repeating step 1), take out sample.
8) open successively mechanical pump and molecular pump, keep the chamber vacuum state.
9) close the vacuum chamber valve, and then successively closure molecule pumping source, mechanical pump power supply, barometer, thermometer, water-cooling system and main power source.
Outer chamber and ultraviolet lamp tube designing and making process are specific as follows among the present invention:
Outer chamber is cylinder-like structure, made by stainless steel material, on seal cover is arranged.Its total height is 400mm, and internal diameter is 300mm, and wall and upper cover thickness are 6mm.
Ultraviolet lamp tube is by company's processing and fabricating, and its power is 150W, and tube diameter is 18mm, is shaped as the hairpin structure, bends to the 120mm*120mm swept area.Ultraviolet lamp tube at first is fixed on the aluminum reflecting plate, and then the aluminum reflecting plate is fixed in outer chamber seal cover inner tip.
The power control part of ultraviolet lamp tube comprises main switch, uviol lamp opening switch, Timing button.For avoiding ultra violet lamp to the human body injury, when opening vacuum chamber, the ultraviolet lamp tube auto-breaking.
The designing and making process of inner cavity chamber, quartz window, heating and water-cooling system is as follows among the present invention:
Inner cavity chamber is cylinder-like structure mainly by quartz material, and total height is 130mm, and internal diameter is 80mm, and the chamber wall thickness is 8mm.Inner cavity chamber's top ultraviolet transmission window adopts high-quality quartz material, and external diameter is 100mm, and its transmission diameter is 80mm, and thickness is 10mm, and sealing is embedded in the steel flange.Be equipped with fixing hole and sealing ring on the flange.
Inner cavity chamber's quartz window upper surface is apart from fluorescent tube 10mm bottom.
The design of inner cavity chamber's control lever and sample stage and the course of processing are specific as follows among the present invention:
Sample stage is connected with control lever, and it can enter inner cavity chamber from the vacuum equipment bottom, and handles sample stage lifting in the 60mm scope by control lever.
The sample stage diameter is 60mm, built-in electric wire, heater coil and water cooling plant, and the inner chamber by control lever is connected with electronic equipment with the external vacuum control system.
At first fixing a diameter on the sample stage is 60mm, and thickness is the insulating heat-conductive earthenware slab of 2mm, then the fixing ceramic base 11 of particular design and processing on it.Ceramic base 11 built-in 24 footnotes 12, concrete such as Fig. 2 structural representation.Its footnote 12 lower ends are connected with built-in electric wire, and the upper end just can realize that electronic component is connected with external electronic device after inserting the chip carrier that is connected with electronic component.
Control lever length is 350mm, and external diameter is 12mm, and there are the screw thread corresponding with quill shaft and stuck point in the side end face, can lifting in the 60mm scope.
It should be noted last that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although with reference to embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, technical scheme of the present invention is made amendment or is equal to replacement, do not break away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (7)
1. vacuum equipment that collects UV/ozone surface treatment and electrical properties in-situ test, it is characterized in that, mainly by vacuum chamber, ultraviolet light source system, vacuum pump system and vacuum equipment control system and electronic components test system form, wherein, described ultraviolet light source system comprises control power supply and ultraviolet lamp tube, described vacuum chamber comprises outer chamber and inner cavity chamber, the described ultraviolet lamp tube of described exocoel indoor location, sample stage and heating and water cooling plant are set in the described inner cavity chamber, and has a gas input, output port, the light of described ultraviolet lamp tube emission is by the quartz window of inner cavity chamber, shine on the sample stage, described inner cavity chamber has the oxygen of certain pressure intensity, and it cleans and modification the sample surfaces on the sample stage through generating ozone and oxygen atom after the UV-irradiation; Described vacuum pump system and vacuum equipment control system for generation of and control vacuum degree in the vacuum chamber, described electronic components test system can carry out to the electrical properties of electronic component in-situ test and characterize.
2. the vacuum equipment of collection UV/ozone according to claim 1 surface treatment and electrical properties in-situ test is characterized in that, described ultraviolet lamp tube emission is mainly the ultraviolet light of 184.9nm and 253.7nm.
3. the vacuum equipment of collection UV/ozone according to claim 2 surface treatment and electrical properties in-situ test, it is characterized in that, described inner cavity chamber is mainly made by quartz material on top, the bottom is mainly stainless steel material and makes, the inner cavity chamber top has the quartz window at wavelength 184.9nm and 253.7nm place high permeability, the size of described quartz window is not less than the aperture, inside of inner cavity chamber, effectively to avoid the generation of inner cavity chamber's oxygen photochemical reaction dark space under UV-irradiation, described gas input, output port are arranged on inner cavity chamber's bottom stainless steel parts.
4. the vacuum equipment of collection UV/ozone according to claim 1 surface treatment and electrical properties in-situ test, it is characterized in that, the height of described sample stage can be regulated within the specific limits by control lever, to realize and effectively control UV/ozone surface treatment.
5. the vacuum equipment of collection UV/ozone according to claim 1 surface treatment and electrical properties in-situ test is characterized in that, described vacuum pump is by two-stage (two-speed) pump, and namely mechanical pump and molecular pump form.
6. the vacuum equipment of collection UV/ozone according to claim 1 surface treatment and electrical properties in-situ test is characterized in that, described vacuum equipment control system mainly comprises: gas flowmeter, vacuum gauge, temperature control system and water-cooling system.
7. the vacuum equipment of collection UV/ozone according to claim 1 surface treatment and electrical properties in-situ test, it is characterized in that, described electronic components test system mainly comprises: lock-in amplifier, voltage source and galvanometer, can carry out in-situ characterization to the electrical properties of electronic component.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210442424.4A CN102983064B (en) | 2012-11-07 | 2012-11-07 | The vacuum equipment of collection UV/ozone surface treatment and electrical properties in-situ test |
| PCT/CN2013/082969 WO2014071769A1 (en) | 2012-11-07 | 2013-09-05 | Vacuum equipment system for surface cleaning and oxidative modification by ultraviolet light/ozone |
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| CN201210442424.4A CN102983064B (en) | 2012-11-07 | 2012-11-07 | The vacuum equipment of collection UV/ozone surface treatment and electrical properties in-situ test |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014071769A1 (en) * | 2012-11-07 | 2014-05-15 | 上海交通大学 | Vacuum equipment system for surface cleaning and oxidative modification by ultraviolet light/ozone |
| CN104752156A (en) * | 2013-12-30 | 2015-07-01 | 昆山国显光电有限公司 | Method and device for pattering nano carbon material film |
| CN104931825A (en) * | 2015-06-13 | 2015-09-23 | 复旦大学 | Integrated apparatus used for optical and electrical measurement and vacuum monitoring of device |
| CN107068598A (en) * | 2017-05-04 | 2017-08-18 | 哈尔滨工业大学 | A kind of utilization vacuum-ultraviolet light cleaning and the device on activated material surface |
| CN107546100A (en) * | 2016-06-24 | 2018-01-05 | 上海交通大学 | Xenon lamp Excimer UV photooxidation vacuum equipment and its application method |
| CN109580717A (en) * | 2018-11-17 | 2019-04-05 | 金华职业技术学院 | The electric measurement method of sample after a kind of vacuum chemical reaction |
| WO2019164454A1 (en) * | 2018-02-26 | 2019-08-29 | National University Of Singapore | In situ electrical properties characterization system towards surface/interface engineered functional devices |
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| JP2008075179A (en) * | 2006-09-19 | 2008-04-03 | Asm Japan Kk | Method of cleaning uv irradiation chamber |
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| CN1449872A (en) * | 2003-04-10 | 2003-10-22 | 上海复旦辰光科技有限公司 | Method and device for cleaning material surface by microwave |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014071769A1 (en) * | 2012-11-07 | 2014-05-15 | 上海交通大学 | Vacuum equipment system for surface cleaning and oxidative modification by ultraviolet light/ozone |
| CN104752156A (en) * | 2013-12-30 | 2015-07-01 | 昆山国显光电有限公司 | Method and device for pattering nano carbon material film |
| CN104752156B (en) * | 2013-12-30 | 2018-06-22 | 昆山国显光电有限公司 | A kind of thin-film patterning method and apparatus of nanometer carbon material |
| CN104931825A (en) * | 2015-06-13 | 2015-09-23 | 复旦大学 | Integrated apparatus used for optical and electrical measurement and vacuum monitoring of device |
| CN107546100A (en) * | 2016-06-24 | 2018-01-05 | 上海交通大学 | Xenon lamp Excimer UV photooxidation vacuum equipment and its application method |
| CN107068598A (en) * | 2017-05-04 | 2017-08-18 | 哈尔滨工业大学 | A kind of utilization vacuum-ultraviolet light cleaning and the device on activated material surface |
| WO2019164454A1 (en) * | 2018-02-26 | 2019-08-29 | National University Of Singapore | In situ electrical properties characterization system towards surface/interface engineered functional devices |
| CN109580717A (en) * | 2018-11-17 | 2019-04-05 | 金华职业技术学院 | The electric measurement method of sample after a kind of vacuum chemical reaction |
| CN109580717B (en) * | 2018-11-17 | 2023-09-12 | 金华职业技术学院 | Electrical measurement method for sample after vacuum chemical reaction |
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