CN100594254C - Film preparation device and observation method for film growth - Google Patents
Film preparation device and observation method for film growth Download PDFInfo
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- CN100594254C CN100594254C CN200810108517A CN200810108517A CN100594254C CN 100594254 C CN100594254 C CN 100594254C CN 200810108517 A CN200810108517 A CN 200810108517A CN 200810108517 A CN200810108517 A CN 200810108517A CN 100594254 C CN100594254 C CN 100594254C
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Abstract
The invention discloses a device adopting a physical method to prepare films on substrate material, and a method of observing film growth condition in the preparation process. A plating chamber in thedevice of the invention is consisted of a plating chamber shell and a bottom plate under the plating chamber shell. A charge valve and an observation window are arranged on a vacuum shell. A resistance heating evaporator, a radiar crucible evaporator, a sputtering target, an interference light source and a webcam are separately arranged on the bottom plate. A rotating tray driven by a rotation axis, a sample annealing heater and a device for fixing a making film sample arranged by the bottom of the sample annealing heater are arranged on a fixing frame. The method of the invention is that aninterference phenomenon formed on the film is observed when the film grows.
Description
Technical field
The present invention relates to a kind of equipment that adopts physical method on base material, to prepare film, and the method for in preparation process, observing the film growing state.More exactly, the present invention relates to adopt the vacuum moulding machine evaporation, perhaps adopt the vacuum sputtering depositional mode to form the equipment of thin film and adopt this equipment in preparation process on the surface of base material, the method for indirect observation film formation surface film formation process.
Background technology
Thin-film material has purposes widely in the sub-device research of novel photoelectric with in making.Adopt the vacuum sputtering depositional mode comparatively common in present stage in the technology that the surface of base material forms thin film.Film described here comprises film, the nonmetal film of metal, and organic film.Existing equipment for producing thin film has vacuum evaporation equipment, vacuum sputtering equipment two classes, this two kind equipment all is to be made of coating chamber, vacuum system and electrical system, coating chamber wherein is used to place the system membrane sample and carries out the preparation of film, vacuum system generally is made up of mechanical pump and diffusion pump, to provide and to keep vacuum tightness in the coating chamber, electrical system is used for providing corresponding supply of electric power to equipment.The vacuum evaporation equipment of prior art can only prepare vacuum evaporation coating, and vacuum sputtering equipment can only be prepared vacuum sputtering membrane.Therefore study or the teaching situation under some special occasions under, for example some special system film requirement, during the requirement film that refabrication one deck forms with vacuum sputtering on evaporating film, can only in different equipment, prepare different films respectively, to satisfy special requirement.And when in distinct device, preparing different film respectively, need rebulid the vacuum work condition, so its energy consumption is higher, efficient is lower.Another deficiency of existing installation is when carrying out anneal after film preparation is good, need film sample is taken out from coating chamber, be placed in the other annealing heating installation and carry out anneal, not only efficient is low, energy consumption is big, but also can influence the performance of film to a certain extent; Because same requirement of film anneal carried out under vacuum condition in some cases, therefore also needs to set up again the vacuum work condition again.In addition, existing membrane equipment can't be observed the situation of film growth in process implementing, the film forming thickness of GPRS generally is rule of thumb to be worth the film forming processing parameter of control, as when vacuum evaporation deposits film forming, be vaporization temperature and the speed of growth of time controlling diaphragm thickness and the thickness that film may form by rule of thumb controlling evaporation source, take out sample then and carry out actual measurement, obtain film forming vacuum thickness.As seen, adopt the thickness of prior art control film growth in the utilization of reality, to be difficult to grasp, and efficient is very low.
Summary of the invention
The invention provides a kind of prior art deficiency that overcomes, can on an equipment, timesharing realize vacuum evaporation and the film forming device of vacuum sputtering, and can in time carry out the equipment of sample anneal, device of the present invention also can be at film forming indirect observation simultaneously film growing state; The invention provides a kind of method of indirect observation film growing state simultaneously.
Film preparation device of the present invention is made up of coating chamber, vacuum system and electrical system, and except that coating chamber, vacuum system is identical with electrical system with the equipment of prior art.Coating chamber of the present invention is made of vacuum chamber housing and the base plate that is positioned under the coating chamber housing, the coating chamber housing is provided with inflation valve and viewing window, on base, be respectively arranged with the resistance heating evaporation device, radiation formula crucible evaporation heater, the target that is used for sputter, interfere light source, camera, and the mechanism that is used to be provided with fixing dismountable radiation formula crucible evaporation heater, on base plate, also be provided with an anchor, anchor is provided with the shaft-driven rotatable tray of rotation, on rotatable tray, be useful on the mechanism that fixing print substrate heater or dismountable radiation formula crucible vaporizer are set, the shell that dismountable radiation formula crucible evaporation heater is made by stainless steel, be arranged at the ring-like quartz heating-pipe in the stainless steel casing, be arranged at the cover plate that pushes up on the stainless steel casing, and the crucible that is arranged on the cover plate constitutes, on the cover board also be provided with the print folder, going to the bottom of print annealing well heater is provided with the device that is used for fixing system film print, also be provided with on the shell of dismountable radiation formula crucible evaporation heater and the print annealing well heater and be used for the device that connects with base plate or rotatable tray, be on the shell of crucible evaporation heater and print annealing well heater, screw to be set in the present invention, cooperate with screw with threaded connecting rod, again screw rod is fixed in the hole on rotatable tray or the base plate, realizes the shell of crucible evaporation heater and fixing of print annealing well heater.The print annealing well heater device that is used for fixing system film print that is provided with of going to the bottom can be a draw-in groove, also can be with fastening piece fixed intermediate plate, or be directly used in the fastening fastening piece.
Used interference light source is the lighting transistor that can send UV-light in the film preparation device of the present invention, and lighting transistor is arranged at the camera next door.
Also be provided with rotating shaft on the coating chamber base plate of film preparation device of the present invention, rotating shaft is provided with rotating shifting board.
The observational technique of film growth is to be radiated at equably with UV-light to form on the film in the film of the present invention, forming film thickness with film formation surface increases, film formation surface engenders the interference hot spot that has color, increase with institute's film former thickness, the interference hot spot color and luster that film forming is sent changes gradually and deepens gradually, interferes the change of hot spot color and colourity can indirectly observe the situation of film generation and the variation of film thickness thereof according to finding.
The present invention carries out film forming when interfere observing, and makes to observe that angle becomes 20 to 30 degree to have best observing effect between sight line and thin film planar.
Be provided with resistance heating evaporation device, radiation formula crucible vaporizer in the coating chamber of apparatus of the present invention simultaneously, be used for the sputtering target of sputtering sedimentation, obviously, can carry out the operation of vacuum evaporation coating and vacuum sputtering system film respectively with device of the present invention; In addition owing to make the film print in the device of the present invention, substrate just, be to be set at the print substrate heater to go to the bottom upward being used for fixing in the device of making membrane sample of setting, therefore after film preparation is good, can directly carry out sample annealing operation, do not need as prior art when therefore preparing film with device of the present invention, need in different equipment, to carry out operation respectively, and will in different equipment, repeatedly set up the vacuum work condition respectively again.
The resistance heating evaporation device that is provided with among the present invention is to be made into evaporation source with tungsten filament or molybdenum boat, makes by the deposition material heat fused to reach evaporation, realizes the plated film operation, and its advantage is simple in structure, and is cheap, easy to operate; Also be provided with radiation formula crucible vaporizer among the present invention simultaneously, this evaporation mode, be particularly suitable for the evaporation of powdered material or organic materials, and can avoid the particle evaporating materials to spatter the waste that produces because of spring, also can be by in crucible, successively putting into the multilayer film that different materials is implemented in evaporation on the print or sputter different material layer, as electrode-organic film-electrode-organic film.
Radiation formula crucible evaporation structure of the present invention has following advantage:
1) when evaporation coating, well heater can be used as the evaporation heating source; And when sputter, it can be used as well heater again and is used as the print heating source, and design can the sticking power of enhanced film on print like this.
2) adopt crucible as heating container, its volume can be less, and its opening is also little, can effectively reduce the waste of material in the evaporative process.
What 3) place in the heating mantles is the quartzy radiation heating lamp that goes in ring, and the organic materials that is positioned under the irradiation of heating lamp in the crucible can be heated uniformly, can effectively avoid splashing of powdered material, makes the velocity of evaporation of material stable, and film forming is even.
4) in radiation formula crucible vaporizer, temperature element can be set, can control the vaporization temperature of differing materials like this, optimize filming technology.
5) when sputter, radiation formula crucible vaporizer is mounted on the rotatable tray, and it is moved to the sputtering target top, so can be suitable for extraordinary print pyritous heating and annealing to non-glass.
Coating chamber base plate of the present invention is provided with rotating shaft, rotating shaft is provided with can be with the shifting board of its rotation, before formal plated film, baffle plate can be gone to above the evaporation source, the material that is gone out by evaporator evaporation before impurity and the normal evaporation condition foundation is stopped by baffle plate, avoid these materials on film formation surface, to deposit, begin the back flap shutter at formal plated film,, can begin film growth away from evaporation source, up to needed film thickness, so just can guarantee the quality of plated film.
Description of drawings
Fig. 1 is a coating chamber diagrammatic cross-section of the present invention, Fig. 2 is a radiation formula crucible evaporation structure synoptic diagram, Fig. 3 is print annealing well heater synoptic diagram, Fig. 4 is the sputtering target structural representation, Fig. 5 has the camera structure synoptic diagram of interfering light source, Fig. 6 to Fig. 9 interference ring that the print surface presents during for different film forming thickness.
Embodiment
The present invention is below in conjunction with embodiment and accompanying drawing explanation.
Vacuum system is identical with electrical system and prior art in the film preparation device of the present invention, repeats no more, and only the present invention's coating chamber is unlike the prior art explained orally at this.
Fig. 2 is the structural representation of radiation formula crucible vaporizer 13 of the present invention, its concrete structure is at the outer cover 24 of making well heater with stainless steel plate through turning, a cover plate 20 is set above outer cover 24, the center of cover plate 20 has a circular hole and is used to place quartz crucible 21, around cover plate 20, also be fixed with four print folders 22, in order to clamp the high temperature annealing print or the sputtered samples of different sizes.At belt quartzy radiation heating tube 19 of outer cover 24 internal fixing.Outer cover 24 is provided with the draw-in groove 25 that matches with steady brace 23 on the cover plate 22.Among the figure 17 is the power connection of heating tube 19.The leg 26 that also is provided with temperature thermocouple 18 in addition and is used for fixing.Adopt the design of radiant heater that following advantage is arranged:
A this well heater when evaporation coating can be used for evaporating heating source;
B pulls down radiation heater 13 when sputter from base plate 1, change the outfit to be fixed on the movable pallet 9, and Rotary tray 9 makes its top of aiming at sputtering target again, can reach the extraordinary print sputter heating of non-glass and the required temperature of annealing;
C can be used as the print heating source, and design can the sticking power of enhanced film on print like this;
D adopts special quartz crucible as heating container, and it is not only than the firm good heat conductivity of small beaker, and the also little waste that can effectively reduce material in the evaporative process of the little opening of volume;
What place in the e heating mantles is the quartzy radiation heating lamp that goes in ring, and the organic materials that is contained under the irradiation of heating lamp in the vitreous silica crucible can be heated uniformly, can effectively avoid splashing of powdered material, so the velocity of evaporation of material is stable, and film forming is even;
The f well heater adopts transformer and the isolated power supply mode of high pressure, so during the regulating voltage controlled temperature, can avoid the glow discharge of high pressure generation to make the well heater short circuit.
The structure of print substrate heater of the present invention as shown in Figure 3.The print substrate heater also is to adopt stainless steel structure, and its top is surrounded the structure that has internal cavities as shown by stainless steel plate.It is heating tube fixed bit hole that four quartz heating- pipes 28,27 are installed in the inside of cavity structure, is the substrate 30 that stainless steel is made in the bottom of silica tube, and its edge has draw-in groove 29 and is used to place print, just prepares the substrate of film.The print surface of being fixed in the draw-in groove 29 when the operation of system film can deposit film, after finishing, evaporation can under the vacuum environment of system film, carry out anneal to print, so not only saved the energy, the over oxidation of also having avoided the traditional technology process that print is caused.
31 is permanent magnet materials among Fig. 4, the 32nd, and sputter anode, the 33rd, negative electrode, the 34th, the dead ring of making by insulating material, the 35th, anode.
Camera of the present invention and interference light source are seen Fig. 5, and this structure can be in the situation of thin film growth process indirect observation film growth.36 is ultraviolet light-emitting diode among the figure, the 37th, and convex lens, the 38th, can send the photodiode of visible light, the 39th, assemble aperture, 40 is the inner chamber of camera lens, the 41st, video picture chip, the 42nd, pick-up lens.Owing to also be provided with the diode 38 of visible light among the present invention, therefore also can be suitable for observing some can produce interference under visible light film.The elevation angle that it should be noted that pick-up lens can be adjusted, and observes with the convenient interference ring that the print surface is produced.
Film-forming process of device of the present invention is summarized as follows:
A is positioned over the substrate of handling well on the print substrate heater 12, and with draw-in groove 29 with substrate constraint, substrate is gone to be positioned at the top of resistance-type evaporation source 2, when vacuum tightness reaches 10
-3During pa,, measure evaporation end when reaching needed thickness with film thickness gauge 5 with resistance-type evaporation aluminium electrode.
B rotates turning axle 10 by servomotor, and driven rotary pallet 9 rotates, when making the substrate aligning magnetron sputtering target top on the substrate heater 12 that is fixed on the rotary-tray 9, begin ventilation, by valve 6 control charge flow rates, boosted voltage makes electronics be accelerated to anode, produces new dissociating in the way.Ion is accelerated to negative electrode bump target, and target particle and secondary Electricity are hit, and the former arrives substrate surface formation of deposits film and becomes Long, and the latter is accelerated to facilitate more in the anode way and dissociates.When film thickness gauge records thickness and reaches, stop sputter.Rotary-tray is rotated once more and aim at resistance-type evaporation by servomotor, second aluminium electrode rete prepared in evaporation, when vacuum tightness reaches 10
-3During pa, evaporate and finish after 1 minute.
C rotates rotary-tray by servomotor once more, until aiming at the radiation formula vaporizer, carries out the operation of another time evaporation film forming.
So just can finish the preparation of multilayer film.In above process, when evaporation heater or radiation heater etc. does not reach working temperature as yet, baffle plate is blocked thereon, deposit at substrate surface with the ion of avoiding in temperature-rise period, steaming, influence film forming quality.And after evaporation heater or radiation heater etc. reaches working temperature, baffle plate can be removed, carry out normal film forming deposition.
When the extraordinary print to non-glass carries out sputter coating, radiation formula crucible evaporation heater 13 should be retrofitted on the rotatable tray 9.
Available camera is observed the inteferometer coating that forms on the film surface under light source (ultraviolet source or visible light source) irradiation in this said process.
The example of a preparation organometallic complex below is provided, and explains orally the way of viewing film growing state by this example.
The film for preparing in the present embodiment is the 8-hydroxy-quinoline metal complexes, and this organic semiconductor thin film has film forming characteristics preferably.The 8-hydroxy-quinoline metal complexes is the very important electroluminescent material material of a class, has both had higher second-order transition temperature, and itself has electron-transporting again, can generate the good film of quality with vacuum vapour deposition.8-hydroxy-quinoline cadmium (8-hydroxylquin-line cadmium, Cdq
2) be a kind of important one pole type electron transport material, the present invention is a raw material with the 8-hydroxy-quinoline cadmium, has prepared the different Cdq of underlayer temperature by vacuum vapour deposition
2Film.Its concrete way is: at first glass substrate was respectively cleaned 30 minutes with Ultrasonic Cleaners in deionized water, ethanol, acetone, just obtained clean glass substrate after the oven dry.Method with vacuum thermal evaporation plates one deck Cdq on such substrate then
2Film, the vacuum tightness in this process in the vacuum chamber remains at (4～5) * 10
-3Pa, Cdq
2The temperature of medicine remains on about 170 ℃ of vaporization temperatures, and the evaporation time is 20min.In above-mentioned vacuum and temperature environment, we have made the organic nano film that underlayer temperature is 45 ℃, 65 ℃ and 85 ℃ respectively.After evaporation was finished, substrate heater kept 150 ℃ and carries out anneal.Cdq
2Material adopts Cdq
2The high-purity C dq of crude product through repeatedly distilling and purify and obtain
2Powder, purity reaches more than 99.9%.Evaporate the circular special quartz crucible that used crucible adopts diameter 5cm.
In the process of above-mentioned evaporation, adjust camera, make that angle becomes 20 to 30 degree between its sight line (optical axis of camera just) and print thin film planar, simultaneously with the other ultraviolet light source oblique illumination of camera to print, with observation film forming situation.Experiment shows, when angle between sight line and print thin film planar beyond 20 to 30 degree time, the poor effect of its observation.
When crucible is heated to the luminous organic material temperature when reaching vaporization temperature, earlier baffle plate is removed from crucible, open radiating light source simultaneously, make ultraviolet lighting be mapped to the print film formation surface, because be invisible light, so the surface is as dark as a stack of black cats.When start vaporizer, the sample surfaces film gives off pale green coloured light.Along with the continuous increase of thickness, the light that film sends becomes faint yellow gradually, but its light-emitting area is little.When film thicker (more than about 20nm), film surface is beige.For the estimation to surperficial film thickness, we have prepared the different film of a series of thickness and have been recorded in observed surface light emitting situation under the uviolizing, have measured thickness respectively with the laser polarization thickness tester then, and have made form.When evaporation coating, just can be according to observed under the ultraviolet ray, the luminous situation of film surface is estimated the thickness of film.If above observation is when shining with ordinary ray, because rete is very thin, only is 20nm, can can't see the existence of superficial film, be that limit of error has also surpassed 10nm with the THICKNESS GAUGE FOR THE MEASUREMENT OF THIN FOILS monitoring.Viewed situation when Fig. 6 to 9 has provided different thickness.Along with the continuous increase of thickness, the light that film sends becomes faint yellow gradually, but its light-emitting area is little.When film thicker (more than about 20nm), film surface is beige.According to these characteristics, can estimate the thickness of film according to the luminous situation of observed film surface under the ultraviolet ray.As can be seen, film thickness at this moment is even from the luminescent film figure of Fig. 6, middle send out brown in part because rate of warming too fast due to, film thickness measured value at this moment is about 20nm.It is green that Fig. 7 centre of figure is, and just in time covers among the 1st layer film when it is the formation of the 2nd level film, and this moment, the film thickness of actual measurement was about 30nm.Be again that Yin Wendu control is too urgent in the figure of Fig. 8, make three-layer thin-film be brownish black, the film thickness measured value of this moment is about 40nm.It is well arranged to form the multilayer film superposition in the figure of Fig. 9, the clear interference ring of light-emitting area, and its thickness, center reaches 800A °, and it is the thinnest to keep to the side, and the film thickness measured value of this moment is about 80nm.Can obtain the information of film thickness indirectly by the visible this method of the present invention of this result.
Claims (3)
1. film preparation device, comprise coating chamber, vacuum system and electrical system, it is characterized in that coating chamber is made of vacuum chamber housing and the base plate that is positioned under the coating chamber housing, the coating chamber housing is provided with inflation valve and viewing window, on base, be respectively arranged with the resistance heating evaporation device, radiation formula crucible evaporation heater, the target that is used for sputter, interfere light source, camera, and the leg that is used for fixing dismountable radiation formula crucible evaporation heater, on base plate, also be provided with an anchor, anchor is provided with the shaft-driven rotatable tray of rotation, on rotatable tray, be useful on the mechanism that fixing print substrate heater or dismountable radiation formula crucible vaporizer are set, the shell that dismountable radiation formula crucible evaporation heater is made by stainless steel, be arranged at the ring-like quartz heating-pipe in the stainless steel casing, be arranged at the cover plate that pushes up on the stainless steel casing, and the crucible that is arranged on the cover plate constitutes, on the cover board also be provided with the print folder, going to the bottom of print substrate heater is provided with the device that is used for fixing system film print, also be provided with on the shell of dismountable radiation formula crucible evaporation heater and the print annealing well heater and be used for the device that connects with base plate or rotatable tray, used interference light source is the lighting transistor that can send UV-light.
2. film preparation device according to claim 1 it is characterized in that used interference light source is the lighting transistor that can send UV-light, and lighting transistor is arranged at the camera next door.
3. film preparation device according to claim 1 and 2 is characterized in that also being provided with rotating shaft on the base plate of coating chamber, and rotating shaft is provided with rotating shifting board.
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| CN200810108517A CN100594254C (en) | 2008-05-21 | 2008-05-21 | Film preparation device and observation method for film growth |
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| CN200810108517A CN100594254C (en) | 2008-05-21 | 2008-05-21 | Film preparation device and observation method for film growth |
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| CN100594254C true CN100594254C (en) | 2010-03-17 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102337503A (en) * | 2010-07-19 | 2012-02-01 | 鸿富锦精密工业（深圳）有限公司 | Film material processing device and evaporating device with film material processing device |
| CN102877029B (en) * | 2012-09-11 | 2014-03-05 | 中国科学技术大学 | Nano film evaporation external member for solar cell |
| CN103805956B (en) * | 2014-02-27 | 2015-10-21 | 苏州大学 | A kind of original position pattern and optical performance monitor evaporation source and vacuum sediment equipment |
| CN104073764B (en) * | 2014-06-17 | 2016-05-18 | 京东方科技集团股份有限公司 | A kind of rotary evaporation source apparatus for OLED evaporation |
| CN104928640B (en) * | 2015-07-05 | 2017-11-07 | 林志苹 | A kind of method that porous activated carbon particle is combined with titanium deoxid film |
| JP6600519B2 (en) * | 2015-09-28 | 2019-10-30 | 株式会社Ｓｃｒｅｅｎホールディングス | Film forming apparatus and data creation method |
| CN106978587B (en) * | 2016-01-15 | 2019-11-08 | 张家港康得新光电材料有限公司 | The plating method of vacuum coating equipment and simple substance membrane |
| CN107841722A (en) * | 2017-11-15 | 2018-03-27 | 中山市创科科研技术服务有限公司 | A kind of optical coating directly monitors the protector of control evaporation |
| CN108796450A (en) * | 2018-08-17 | 2018-11-13 | 北京铂阳顶荣光伏科技有限公司 | A kind of attachment device and heating device is steamed altogether |
| CN109609915B (en) * | 2019-01-09 | 2020-12-01 | 张晓军 | Disordered engineering semiconductor nano material preparation system |
| CN111826628B (en) * | 2020-06-24 | 2022-07-29 | 合肥科晶材料技术有限公司 | Device for controlling quartz crucible by using magnet |
| CN111850496A (en) * | 2020-07-28 | 2020-10-30 | 合肥科晶材料技术有限公司 | RF and PVD system for manufacturing solid-state thin film battery |
| CN112195443A (en) * | 2020-09-14 | 2021-01-08 | 武汉电信器件有限公司 | Film deposition system and film coating method |
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2008
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