CN101834233A - Method for rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature - Google Patents
Method for rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature Download PDFInfo
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- CN101834233A CN101834233A CN201010137326A CN201010137326A CN101834233A CN 101834233 A CN101834233 A CN 101834233A CN 201010137326 A CN201010137326 A CN 201010137326A CN 201010137326 A CN201010137326 A CN 201010137326A CN 101834233 A CN101834233 A CN 101834233A
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Abstract
The invention discloses a method for rapidly depositing a hydrogenated amorphous silicon solar battery thin film at low temperature, which comprises the following steps of: firstly, placing a cleaned substrate on a substrate platform of an opposite target magnetron sputtering device; then vacuumizing a reaction chamber of the opposite target magnetron sputtering device and cleaning the substrate platform of the opposite target magnetron sputtering device and the wall of the reaction chamber by argon plasma; heating the substrate platform; charging a reaction gas into the reaction chamber and adjusting air pressure; starting a sputtering power supply and depositing the amorphous silicon thin film till an amorphous silicon thin film sample is obtained; finally cooling to room temperature under the protection of hydrogen, taking out the sample and finishing the deposition of the hydrogenated amorphous silicon thin film. The invention can rapidly deposit the hydrogenated amorphous silicon thin film at low temperature by utilizing an opposite target magnetron reaction sputtering deposition technology.
Description
Technical field
The present invention relates to the film preparation field, relate in particular to a kind of method of rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature.
Background technology
The hydrogenation non crystal silicon film technology of preparing has become the problem that receives much concern, because its outstanding photoelectric characteristic makes it have great Practical significance and wide application prospect at microelectronics technology and technical field of solar.In its traditional preparation technology, have following at least two defectives: 1. underlayer temperature is very high, causes the doping of film easily; 2. thin layer poor growth, the commercialization cost is very high.For this reason, people have proposed the novel preparation method of multiple hydrogenation non crystal silicon film, but still fail well to solve the problems of the technologies described above, and realize that the low temperature of hydrogenation non crystal silicon film is grown fast.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method of rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature, utilizes target reactive magnetron sputtering deposition technique fast deposition hydrogenation non crystal silicon film at low temperatures.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of method of rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature is used target reactive magnetron sputtering deposition technique, and it comprises following steps:
A, clean substrate, and substrate is placed on the chip bench to target reactive magnetron sputtering precipitation equipment, this substrate is monocrystalline silicon piece or quartz plate or corning glass or plastic;
B, utilization vacuumize its reative cell the vacuum-pumping system of target reactive magnetron sputtering precipitation equipment, make reative cell air pressure be lower than 5 * 10
-4Pa;
C, argon plasma clean target and reative cell wall to target reactive magnetron sputtering precipitation equipment, the steps include: at first to hide substrate with baffle plate, with the flow feeding reative cell of argon gas with 5-15sccm, open shielding power supply, begin to clean, continue 20-40 minute, close shielding power supply then;
D, heated substrate platform feed reacting gas to 20-300 ℃ to reative cell, and reacting gas comprises H
2And Ar, flow-rate ratio H
2: Ar=3: 1, air pressure adjustment is 0.1-5Pa, opens shielding power supply, and power remains between the 45-55W, and the deposition of beginning amorphous silicon membrane is to obtaining the hydrogenation non crystal silicon film sample;
After E, deposition are finished; at first close shielding power supply; again argon flow amount is set to zero; keep hydrogen flowing quantity constant; close the chip bench heater then; under hydrogen shield, lower the temperature; after the chip bench temperature drops to room temperature; hydrogen flowing quantity is set to zero, and closed vacuum-pumping system, in reative cell, charge into drying nitrogen pressure to reative cell then when being an atmospheric pressure; open the reative cell sampling window; taking-up deposits the substrate of hydrogenation non crystal silicon film, and the sampling window of off-response chamber is finished the deposition of hydrogenation non crystal silicon film.
The described substrate of step 1-A can be monocrystalline silicon piece, and the step of this monocrystalline silicon piece being carried out chemical cleaning is as follows: soaked 3 minutes with acetone and methyl alcohol mixed liquor earlier, take out oven dry, use volume ratio NH again
4OH: H
2O
2: H
2O=1: 2: 5 mixed solution soaked 5 minutes, took out and used deionized water rinsing, put into volume ratio HF: H again
2O=1: soaked 1 minute in 10 the mixed solution, take out and use deionized water rinsing, oven dry.
The described substrate of step 1-A can also be quartz plate or corning glass, the step of this quartz plate or corning glass being carried out chemical cleaning is: it was cleaned 8-12 minute in ultrasonic washing instrument with acetone earlier, with dipping in spirituous rayon balls it is cleaned again, at last oven dry.
The described substrate of step 1-A can also be plastic, and the step of this plastic being carried out chemical cleaning is: it was cleaned 8-12 minute in ultrasonic washing instrument with alcohol, then oven dry.
Described target to target reactive magnetron sputtering precipitation equipment is the high resistant pure silicon target.
Adopt the beneficial effect that technique scheme produced to be: the present invention can prepare hydrogenation non crystal silicon film fast under 150-300 ℃ low temperature, utilization prepares hydrogenation non crystal silicon film to target reactive magnetron sputtering deposition technique, plasma is constrained between two relative sputtering targets, causes Ar and H
2Have the characteristic that efficiently excites and dissociate Deng reacting gas, thereby be implemented in the efficient target sputter under the higher ion volume density, not only required underlayer temperature is low, and deposition velocity is fast; Simultaneously,, avoided the bombardment of high energy particle, more helped the microcosmic ordering deposition of film film because film-substrate is positioned at outside the plasma slab.
Description of drawings
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
Fig. 1 is the atomic force shape appearance figure of the hydrogenation non crystal silicon film that deposited under various substrate of embodiment 1-5, among the figure, and A, 20 ℃ of B, 150 ℃ of C, 200 ℃ of D, 250 ℃ of E, 300;
Fig. 2 is the raman scattering spectrum of the hydrogenation non crystal silicon film that deposited under various substrate of embodiment 1-5;
Fig. 3 is the hydrogenation non crystal silicon film that deposited under various substrate of embodiment 1-5 (α * Ephoton)
1/2Curve and band gap parameter.
Embodiment
Following examples describe technical scheme of the present invention in detail.
Used in the present invention to target reactive magnetron sputtering precipitation equipment, can be United States Patent (USP) " to target sputtering equipment ", its patent No. is " US 2003/0094365A1 "; This device comprises shielding power supply, is used to regulate the regulating circuit of shielding power supply power, reative cell, be positioned at reative cell to target and chip bench and chip bench heater, be arranged on Intaker controller, vacuum-pumping system on the reative cell.
The method of the rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature of first embodiment of the invention comprises following steps:
A, get a monocrystalline silicon piece substrate, soaked 3 minutes with acetone and methyl alcohol mixed liquor earlier, take out oven dry, use volume ratio NH again
4OH: H
2O
2: H
2O=1: 2: 5 mixed solution soaked 5 minutes, took out and used deionized water rinsing, put into volume ratio HF: H again
2O=1: soaked 1 minute in 10 the mixed solution, take out and use deionized water rinsing, oven dry is placed into substrate on the chip bench to target reactive magnetron sputtering precipitation equipment then;
B, utilize vacuum-pumping system that the reative cell to target reactive magnetron sputtering precipitation equipment is vacuumized, make reative cell air pressure be lower than 5 * 10
-4Pa;
C, elder generation hide substrate with baffle plate, with the flow feeding reative cell of argon gas with 10sccm, open shielding power supply then, and power remains on 100W, utilizes argon plasma that high resistant pure silicon target and reative cell wall are cleaned, and continues 30 minutes, closes shielding power supply then;
D, heated substrate platform to 20 ℃, the hydrogen of 30sccm flow and the argon gas of 10sccm flow are fed reative cell, regulate vacuum-pumping system, make the reative cell internal gas pressure remain on 0.5Pa, open shielding power supply, power remains on 50W, the deposition of beginning hydrogenation non crystal silicon film;
E; measure film thickness with the step instrument; treat that thin film deposition is to desired thickness; at first close shielding power supply; again argon flow amount is set to zero; keep hydrogen flowing quantity constant; close the chip bench heater then; under hydrogen shield, lower the temperature, after the chip bench temperature drops to room temperature, hydrogen flowing quantity is set to zero; and close vacuum-pumping system; in reative cell, charge into drying nitrogen pressure to reative cell then when being an atmospheric pressure, open the reative cell sampling window, take out the substrate that deposits hydrogenation non crystal silicon film; the sampling window of off-response chamber is finished the deposition of hydrogenation non crystal silicon film.
Embodiment 2
The method of the rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature of second embodiment of the invention, its step is identical with embodiment 1, just heated substrate platform to 150 ℃ in step 1-D.
The method of the rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature of third embodiment of the invention, its step is identical with embodiment 1, just heated substrate platform to 200 ℃ in step 1-D.
Embodiment 4
The method of the rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature of fourth embodiment of the invention, its step is identical with embodiment 1, just heated substrate platform to 250 ℃ in step 1-D.
Embodiment 5
The method of the rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature of fifth embodiment of the invention, its step is identical with embodiment 1, just heated substrate platform to 300 ℃ in step 1-D.
Embodiment 1-5 has adopted different underlayer temperatures, and Fig. 1 has provided the atomic force shape appearance figure of the resulting amorphous silicon hydride solar battery thin film of embodiment 1-5, by figure obviously as seen, film becomes graininess to distribute, along with the rising of underlayer temperature, roughness of film, be RMS, reduce gradually.Compare with common magnetron sputtered deposition technology, preparation technology in low temperature of the present invention is owing to suppressed the bombardment effect of high energy particle in the plasma, and the film that is obtained has the higher surface particles uniformity and littler surface roughness.
Fig. 2 has provided the raman scattering spectrum of embodiment 1-5 institute deposited samples, show among the figure, rising along with underlayer temperature, characterize the parameter of the membrane structure degree of order: " the full width at half maximum value of transverse optical mode " and " the pairing bands of a spectrum integrated intensity of transverse acoustic mode and transverse optical mode ", the two all has the trend of reducing, this explanation is along with the rising of underlayer temperature, and the degree of order of thin-membrane short-range and intermediate range is enhanced.This has further proved and has adopted the facing-target magnetron sputtering system technology to prepare the feasibility of constitutionally stable amorphous silicon hydride solar battery thin film at low temperatures.
Fig. 3 has provided the optical characteristics of embodiment 1-5 institute deposited samples, as seen from the figure, hydrogenation non crystal silicon film reacts integrally-built associating density of states B parameter (the big more then overall structure of the B value degree of order is high more) and then shows rising trend along with its optical band gap of rising of underlayer temperature reduces gradually.The variation of above optical parametric has proved the hydrogenation non crystal silicon film that uses method of the present invention can prepare Stability Analysis of Structures, superb optical performance.
In addition, utilize technical scheme of the present invention, can in the hydrogenation non crystal silicon film of deposition, mix elements such as B or P by changing target, thereby realize the preparation of large-area P type or N type hydrogenation non crystal silicon film.
Listed examples of the present invention is intended to further illustrate the methods and applications direction of this rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature, and scope of the present invention is not constituted any restriction.
Claims (5)
1. the method for a rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature is used target reactive magnetron sputtering deposition technique, it is characterized in that: comprise following steps:
A, clean substrate, and substrate is placed on the chip bench to target reactive magnetron sputtering precipitation equipment, this substrate is monocrystalline silicon piece or quartz plate or corning glass or plastic;
B, utilization vacuumize its reative cell the vacuum-pumping system of target reactive magnetron sputtering precipitation equipment, make reative cell air pressure be lower than 5 * 10
-4Pa;
C, argon plasma clean target and reative cell wall to target reactive magnetron sputtering precipitation equipment, the steps include: at first to hide substrate with baffle plate, with the flow feeding reative cell of argon gas with 5-15sccm, open shielding power supply, begin to clean, continue 20-40 minute, close shielding power supply then;
D, heated substrate platform feed reacting gas to 20-300 ℃ to reative cell, and reacting gas comprises H
2And Ar, flow-rate ratio H
2: Ar=3: 1, air pressure adjustment is 0.1-5Pa, opens shielding power supply, and power remains between the 45-55W, and the deposition of beginning amorphous silicon membrane is to obtaining the hydrogenation non crystal silicon film sample;
After E, deposition are finished; at first close shielding power supply; again argon flow amount is set to zero; keep hydrogen flowing quantity constant; close the chip bench heater then; under hydrogen shield, lower the temperature; after the chip bench temperature drops to room temperature; hydrogen flowing quantity is set to zero, and closed vacuum-pumping system, in reative cell, charge into drying nitrogen pressure to reative cell then when being an atmospheric pressure; open the reative cell sampling window; taking-up deposits the substrate of hydrogenation non crystal silicon film, and the sampling window of off-response chamber is finished the deposition of hydrogenation non crystal silicon film.
2. the method for rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature according to claim 1, it is characterized in that: the described substrate of step 1-A is a monocrystalline silicon piece, the step of this monocrystalline silicon piece being carried out chemical cleaning is as follows: soaked 3 minutes with acetone and methyl alcohol mixed liquor earlier, take out oven dry, use volume ratio NH again
4OH: H
2O
2: H
2O=1: 2: 5 mixed solution soaked 5 minutes, took out and used deionized water rinsing, put into volume ratio HF: H again
2O=1: soaked 1 minute in 10 the mixed solution, take out and use deionized water rinsing, oven dry.
3. the method for rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature according to claim 1, it is characterized in that: the described substrate of step 1-A is quartz plate or corning glass, the step of this quartz plate or corning glass being carried out chemical cleaning is: it was cleaned 8-12 minute in ultrasonic washing instrument with acetone earlier, with dipping in spirituous rayon balls it is cleaned again, at last oven dry.
4. the method for rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature according to claim 1, it is characterized in that: the described substrate of step 1-A is a plastic, the step of this plastic being carried out chemical cleaning is: it was cleaned 8-12 minute in ultrasonic washing instrument with alcohol, then oven dry.
5. the method for rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature according to claim 1, it is characterized in that: described target to target reactive magnetron sputtering precipitation equipment is the high resistant pure silicon target.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260853A (en) * | 2011-07-07 | 2011-11-30 | 西安理工大学 | Method for depositing silicon membrane for solar cell on basis of magnetic control sputtering technology |
| CN103560180A (en) * | 2013-11-15 | 2014-02-05 | 上海电机学院 | Hydrogenated amorphous silicon nanowire array preparation method |
| CN104488094A (en) * | 2012-05-21 | 2015-04-01 | 新南创新私人有限公司 | Advanced hydrogenation of silicon solar cells |
| CN108914071A (en) * | 2018-08-10 | 2018-11-30 | 深圳市都乐精密制造有限公司 | Amorphous silicon hydride method for preparing optical thin film |
| CN109239827A (en) * | 2018-11-10 | 2019-01-18 | 深圳市都乐精密制造有限公司 | Low angle off-set optical Thin Film Filter for face identification system |
| CN109964303A (en) * | 2016-11-18 | 2019-07-02 | 应用材料公司 | Via the method for physical vapour deposition (PVD) deposition of amorphous silicon layers or silicon oxycarbide layer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1445821A (en) * | 2002-03-15 | 2003-10-01 | 三洋电机株式会社 | Forming method of ZnO film and ZnO semiconductor layer, semiconductor element and manufacturing method thereof |
| CN100527448C (en) * | 2007-02-12 | 2009-08-12 | 江苏林洋新能源有限公司 | Hydrogenation non crystal silicon film solar battery and its preparing method |
-
2010
- 2010-04-01 CN CN2010101373260A patent/CN101834233B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1445821A (en) * | 2002-03-15 | 2003-10-01 | 三洋电机株式会社 | Forming method of ZnO film and ZnO semiconductor layer, semiconductor element and manufacturing method thereof |
| CN100527448C (en) * | 2007-02-12 | 2009-08-12 | 江苏林洋新能源有限公司 | Hydrogenation non crystal silicon film solar battery and its preparing method |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260853A (en) * | 2011-07-07 | 2011-11-30 | 西安理工大学 | Method for depositing silicon membrane for solar cell on basis of magnetic control sputtering technology |
| CN102260853B (en) * | 2011-07-07 | 2013-01-02 | 西安理工大学 | Method for depositing silicon membrane for solar cell on basis of magnetic control sputtering technology |
| CN104488094A (en) * | 2012-05-21 | 2015-04-01 | 新南创新私人有限公司 | Advanced hydrogenation of silicon solar cells |
| CN104488094B (en) * | 2012-05-21 | 2017-03-08 | 新南创新私人有限公司 | The improved hydrogenation of silicon solar cell |
| CN103560180A (en) * | 2013-11-15 | 2014-02-05 | 上海电机学院 | Hydrogenated amorphous silicon nanowire array preparation method |
| CN109964303A (en) * | 2016-11-18 | 2019-07-02 | 应用材料公司 | Via the method for physical vapour deposition (PVD) deposition of amorphous silicon layers or silicon oxycarbide layer |
| CN109964303B (en) * | 2016-11-18 | 2023-08-29 | 应用材料公司 | Method for depositing amorphous silicon layer or silicon oxycarbide layer by physical vapor deposition |
| CN108914071A (en) * | 2018-08-10 | 2018-11-30 | 深圳市都乐精密制造有限公司 | Amorphous silicon hydride method for preparing optical thin film |
| CN109239827A (en) * | 2018-11-10 | 2019-01-18 | 深圳市都乐精密制造有限公司 | Low angle off-set optical Thin Film Filter for face identification system |
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