CN104328493A - Preparation method of polycrystalline silicon thin film - Google Patents
Preparation method of polycrystalline silicon thin film Download PDFInfo
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- CN104328493A CN104328493A CN201410598219.6A CN201410598219A CN104328493A CN 104328493 A CN104328493 A CN 104328493A CN 201410598219 A CN201410598219 A CN 201410598219A CN 104328493 A CN104328493 A CN 104328493A
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Abstract
The invention relates to a preparation method of a large-area polycrystalline silicon thin film under a condition of low temperature. The method comprises the following steps: conventionally cleaning a substrate, placing the cleaned substrate into a vacuum coating system, performing plasma in-situ cleaning on the substrate with hydrogen gas; performing pre-depositing on the substrate to obtain a thin film by utilizing silane and hydrogen gas as reacting gases, performing plasma etching on the obtained thin film by utilizing hydrogen gas, and depositing the etched thin film again to obtain the polycrystalline silicon thin film. According to the technical scheme of the invention, cheap high-quality large-area polycrystalline silicon thin film can be prepared, the polycrystalline silicon thin film has less crystal boundaries of the crystal particle, high crystallization degree and large crystal particle, is expect to improve the performance of a polycrystalline silicon thin film solar battery when used in the solar battery, and can be applied to the photoelectronic device field and the like.
Description
Technical field
The invention belongs to polysilicon membrane technical field, specifically relate to the preparation method of the large-area polycrystalline silicon film under a kind of cold condition.
Background technology
Plasma enhanced chemical vapor deposition method (PECVD) is the ionization of gas making containing film composed atom by microwave or radio frequency etc., be partially formed plasma body, and plasma chemistry activity is very strong, be easy to react, desired film is gone out at deposition on substrate, in order to make chemical reaction carry out at a lower temperature, the activity that make use of plasma body promotes reaction.
Multi-crystal silicon film solar battery be integrate long, the stable performance of the efficiency of conversion of crystal silicon solar energy battery, life-span and with low cost, preparation technology simple, can the solar cell of new generation of the advantage such as big area production, the photovoltaic market in future will occupy critical role, this year, along with the development of polysilicon membrane technology of preparing, multi-crystal silicon film solar battery is hopeful the s-generation hull cell of alternative crystal silicon solar energy battery most, has become one of international field of solar energy study hotspot.
The growth quality of polysilicon membrane directly affects polysilicon membrane efficiency of conversion and other performances, polysilicon membrane crystallization degree is incomplete, crystal grain is little is the major cause limiting battery performance with defect concentration height, the substrate preparing polysilicon membrane conventional has silicon single crystal, non-crystalline silicon, conductive glass, the simple glass of polyimide and cheapness and stainless steel etc., but be difficult to form larger crystal grain on the non-silicon substrate of cheapness.In inexpensive substrate, prepare high crystallization degree thus, the polysilicon membrane of fabricating low-defect-density and large grain size is problem demanding prompt solution.
Summary of the invention
The crystallization degree that the object of the invention is to solve polycrystalline silicon thin films is low, crystal grain is little, the difficult problem that defect concentration is large, plasma enhanced chemical vapor deposition method (PECVD) is utilized to deposit, polysilicon grain crystal boundary prepared by solution PECVD is many, the problem that crystal grain is little, makes cheap high quality, and uniform large area polysilicon thin film low temperature preparation becomes possibility.
For achieving the above object, the present invention is to be realized by following technical scheme:
A preparation method for polysilicon membrane, after first carrying out routine cleaning, is positioned in vacuum coating system, uses hydrogen to carry out plasma body situ cleaning again to substrate to substrate; Adopt silane and hydrogen to be reactant gases, substrate carries out pre-deposition and obtains film, adopt hydrogen to carry out plasma etching the film obtained, the film after etching is deposited again and obtains polysilicon membrane.
Its principle is, the defects such as a lot of dislocations, surface state and dangling bonds are contained at the polysilicon membrane deposited by PECVD method, greatly reduce minority carrier lifetime in polysilicon membrane, and then have impact on the raising of solar cell short-circuit current and cell conversion efficiency.At polysilicon membrane early growth period, first grow one deck amorphous hatching layer, the dislocation that hatching layer contains, surface state directly can affect the Enhancing Nucleation Density of polysilicon membrane with the defect concentration such as dangling bonds and core is grown up, reduce the defect concentration of amorphous hatching layer thus, increasing surfactivity and reducing surface energy is improve the important step of polysilicon membrane quality.In deposition process, increase hydrogen plasma etching link, at the polycrystalline silicon growth initial stage, utilize the corrasion of hydrogen plasma, while filling up silicon dangling bonds, weak Si-Si bond is broken, and again forms stable Si-Si bond, film surface activity can be increased simultaneously, reduce forming core energy, few in the hope of preparing crystal particle crystal boundary, crystal grain is large, the high quality polysilicon membrane that defect concentration is little.Can be implemented in low temperature depositing in inexpensive substrate by PECVD method, and sample table area is large, and rotatable, can high quality be prepared thus, uniform large-area polycrystalline silicon film.
In above-described technical scheme, plasma etching adopt the flow of hydrogen to be 10sccm ~ 100sccm, etching time is 1 ~ 12min.
In above-described technical scheme, in pre-deposition and again deposition process, silane flow rate is 1sccm ~ 50sccm, and hydrogen flowing quantity is 10sccm ~ 100sccm.
In above-described technical scheme, the depositing time of pre-deposition is 2 ~ 10min, and the depositing time again deposited is 1h ~ 5h.
In above-described technical scheme, described vacuum coating system is the coating system adopting microwave plasma to strengthen chemical Vapor deposition process.
In above-described technical scheme, described substrate is silicon chip, simple glass or conductive glass.The routine of substrate is cleaned as to use acetone successively, dehydrated alcohol and deionized water ultrasonic cleaning 10min, and adopt nitrogen to dry up.
Plasma body situ cleaning adopts the flow of hydrogen to be 10sccm ~ 100sccm, and plasma body situ clean times is 10mim ~ 20min.
Described substrate temperature scope is 25 DEG C ~ 500 DEG C, and the microwave power of vacuum coating system is 500W ~ 1200W.
Technical scheme of the present invention can prepare the cheap large-area polysilicon membrane of high quality, its crystal particle crystal boundary is few, and crystallization degree is high, and crystal grain is large, on solar cell, be expected the performance improving multi-crystal silicon film solar battery, be applied at other fields such as opto-electronic devices simultaneously.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1:
Select substrate to be simple glass originally executing in example, substrate size is 2cm × 2cm, and be positioned over the sample table central authorities of vacuum coating system, sample table speed of rotation is 10r/min, silicon deposited film time t
1for 5min, etching time is 2min, and after etching, the silicon deposited film time is 1.5h.
On common glass substrate, the concrete steps of deposited polycrystalline silicon thin film are as follows:
1) after using acetone, dehydrated alcohol and deionized water ultrasonic cleaning substrate 10min successively, dry up with nitrogen, common glass substrate is put into WM-PECVD (Microwave Plasma Torch Atomic Emission Spect rometry method) system;
2) underlayer temperature is risen to 250 DEG C;
3) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is that 1000W carries out discharging and carries out in-situ hydrogen plasma clean 15min to substrate;
4) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W carries out deposit thin films of silicon 5min;
5) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is 1000 carry out discharge step 4) in deposit film carry out hydrogen plasma etching 2min;
6) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W is in step 5) deposit thin films of silicon 1.5h is continued on basis;
7) treat that substrate is down to room temperature, reach deposited polycrystalline silicon thin film on simple glass.
The present embodiment take simple glass as the polysilicon membrane of substrate, preparation, inexpensive, and quality is high, can prepare large-area polysilicon membrane, and its crystal particle crystal boundary is few, and crystallization degree is high, and crystal grain is large.
Embodiment 2:
Select substrate to be simple glass originally executing in example, substrate size is 2cm × 2cm, and be positioned over the sample table central authorities of vacuum coating system, sample table speed of rotation is 10r/min, silicon deposited film time t
1for 5min, etching time is 2min, and after etching, the silicon deposited film time is 4h.
On common glass substrate, the concrete steps of deposited polycrystalline silicon thin film are as follows:
1), after using acetone, dehydrated alcohol and deionized water ultrasonic cleaning substrate 10min successively, dry up with nitrogen, common glass substrate is put into WM-PECVD system;
2) underlayer temperature is risen to 250 DEG C;
3) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is that 1000W carries out discharging and carries out in-situ hydrogen plasma clean 15min to substrate;
4) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W carries out deposit thin films of silicon 5min;
5) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is 1000 carry out discharge step 4) in deposit film carry out hydrogen plasma etching 2min;
6) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W is in step 5) deposit thin films of silicon 4h is continued on basis;
7) treat that substrate is down to room temperature, reach deposited polycrystalline silicon thin film on simple glass.
The present embodiment take simple glass as the polysilicon membrane of substrate, preparation, inexpensive, and quality is high, can prepare large-area polysilicon membrane, and its crystal particle crystal boundary is few, and crystallization degree is high, and crystal grain is large.
Embodiment 3:
The present embodiment selects substrate to be conductive glass, and substrate size is 2cm × 2cm, and be positioned over the sample table central authorities of vacuum coating system, sample table speed of rotation is 10r/min, silicon deposited film time t
1for 10min, etching time is 5min, and after etching, the silicon deposited film time is 4h.
In Conducting Glass, the concrete steps of deposited polycrystalline silicon thin film are as follows:
1), after using acetone, dehydrated alcohol and deionized water ultrasonic cleaning substrate 10min successively, dry up with nitrogen, Conducting Glass is put into WM-PECVD system;
2) underlayer temperature is risen to 250 DEG C;
3) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is that 1000W carries out discharging and carries out in-situ hydrogen plasma clean 15min to substrate;
4) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W carries out deposit thin films of silicon 10min;
5) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is 1000 carry out discharge step 4) in deposit film carry out hydrogen plasma etching 5min;
6) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W is in step 5) deposit thin films of silicon 4h is continued on basis;
7) treat that substrate is down to room temperature, reach deposited polycrystalline silicon thin film on conductive glass.
The present embodiment take conductive glass as the polysilicon membrane of substrate, preparation, inexpensive, and quality is high, can prepare large-area polysilicon membrane, and its crystal particle crystal boundary is few, and crystallization degree is high, and crystal grain is large.
Embodiment 4:
The present embodiment selects substrate to be simple glass, and substrate size is 2cm × 2cm, and be positioned over the sample table central authorities of vacuum coating system, sample table speed of rotation is 10r/min, silicon deposited film time t
1for 10min, etching time is 10min, and after etching, the silicon deposited film time is 4h.
On common glass substrate, the concrete steps of deposited polycrystalline silicon thin film are as follows:
1), after using acetone, dehydrated alcohol and deionized water ultrasonic cleaning substrate 10min successively, dry up with nitrogen, common glass substrate is put into WM-PECVD system;
2) underlayer temperature is risen to 250 DEG C;
3) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is that 1000W carries out discharging and carries out in-situ hydrogen plasma clean 15min to substrate;
4) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W carries out deposit thin films of silicon 10min;
5) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is 1000 carry out discharge step 4) in deposit film carry out hydrogen plasma etching 10min;
6) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W is in step 5) deposit thin films of silicon 4h is continued on basis;
7) treat that substrate is down to room temperature, reach deposited polycrystalline silicon thin film on simple glass.
The present embodiment take simple glass as the polysilicon membrane of substrate, preparation, inexpensive, and quality is high, can prepare large-area polysilicon membrane, and its crystal particle crystal boundary is few, and crystallization degree is high, and crystal grain is large.
Embodiment 5:
The present embodiment selects substrate to be silicon chip, and substrate size is 2cm × 2cm, and be positioned over the sample table central authorities of vacuum coating system, sample table speed of rotation is 6r/min, silicon deposited film time t
1for 10min, etching time is 5min, and after etching, the silicon deposited film time is 4h.
In silicon chip substrate, the concrete steps of deposited polycrystalline silicon thin film are as follows:
1), after using acetone, dehydrated alcohol and deionized water ultrasonic cleaning 10min successively, dry up with nitrogen, silicon chip substrate is put into WM-PECVD system;
2) underlayer temperature is risen to 250 DEG C;
3) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is that 1000W carries out discharging and carries out in-situ hydrogen plasma clean 15min to substrate;
4) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W carries out deposit thin films of silicon 10min;
5) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is 1000 carry out discharge step 4) in deposit film carry out hydrogen plasma etching 5min;
6) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W is in step 5) deposit thin films of silicon 4h is continued on basis;
7) treat that substrate is down to room temperature, reach deposited polycrystalline silicon thin film on silicon chip.
The present embodiment take simple glass as the polysilicon membrane of substrate, preparation, inexpensive, and quality is high, can prepare large-area polysilicon membrane, and its crystal particle crystal boundary is few, and crystallization degree is high, and crystal grain is large.
Embodiment 6:
Select substrate to be simple glass, substrate size is 20cm × 20cm, and be positioned over the sample table central authorities of vacuum coating system, sample table speed of rotation is 6r/min, silicon deposited film time t
1for 10min, etching time is 5min, and after etching, the silicon deposited film time is 4h.
On common glass substrate, the concrete steps of deposited polycrystalline silicon thin film are as follows:
1), after using acetone, dehydrated alcohol and deionized water ultrasonic cleaning 10min successively, common glass substrate, with drying up, is put into WM-PECVD system by nitrogen;
2) underlayer temperature is risen to 250 DEG C;
3) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is that 1000W carries out discharging and carries out in-situ hydrogen plasma clean 15min to substrate;
4) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W carries out deposit thin films of silicon 10min;
5) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 40sccm, and microwave power is 1000 carry out discharge step 4) in deposit film carry out hydrogen plasma etching 5min;
6) at the same temperature (250 DEG C), adjustment hydrogen flowing quantity is 50sccm, and silane flow rate is 10sccm, and microwave power is that 1000W is in step 5) deposit thin films of silicon 4h is continued on basis;
7) treat that substrate is down to room temperature, reach deposited polycrystalline silicon thin film on simple glass.
The present embodiment take simple glass as the polysilicon membrane of substrate, preparation, inexpensive, and quality is high, can prepare large-area polysilicon membrane, and its crystal particle crystal boundary is few, and crystallization degree is high, and crystal grain is large.
The foregoing describe the preferred embodiments of the present invention, not thereby limit to interest field of the present invention.Those skilled in the art do not depart from the scope and spirit of the present invention interior done any amendment, equivalent replacement and improve, all should within interest field of the present invention.
Claims (10)
1. a preparation method for polysilicon membrane, is characterized in that, after first carrying out routine cleaning, is positioned in vacuum coating system, uses hydrogen to carry out plasma body situ cleaning again to substrate to substrate; Adopt silane and hydrogen to be reactant gases, substrate carries out pre-deposition and obtains film, adopt hydrogen to carry out plasma etching the film obtained, the film after etching is deposited again and obtains polysilicon membrane.
2. the preparation method of polysilicon membrane according to claim 1, is characterized in that, plasma etching adopt the flow of hydrogen to be 10sccm ~ 100sccm, etching time is 1 ~ 12min.
3. the preparation method of polysilicon membrane according to claim 1, is characterized in that, in pre-deposition and again deposition process, silane flow rate is 1sccm ~ 50sccm, and hydrogen flowing quantity is 10sccm ~ 100sccm.
4. the preparation method of polysilicon membrane according to claim 1, is characterized in that, the depositing time of pre-deposition is 2 ~ 10min, and the depositing time again deposited is 1h ~ 5h.
5. the preparation method of polysilicon membrane according to claim 1, is characterized in that, described vacuum coating system is the coating system adopting microwave plasma to strengthen chemical Vapor deposition process.
6. the preparation method of polysilicon membrane according to claim 1, is characterized in that, described substrate is silicon chip, simple glass or conductive glass.
7. the preparation method of polysilicon membrane according to claim 1, is characterized in that, the routine of described substrate is cleaned as to use acetone successively, dehydrated alcohol and deionized water ultrasonic cleaning 10min, and adopts nitrogen to dry up.
8. the preparation method of polysilicon membrane according to claim 1, is characterized in that, plasma body situ cleaning adopts the flow of hydrogen to be 10sccm ~ 100sccm, and plasma body situ clean times is 10mim ~ 20min.
9. the preparation method of polysilicon membrane according to claim 1, is characterized in that, described substrate temperature scope is 25 DEG C ~ 500 DEG C, and the microwave power of vacuum coating system is 500W ~ 1200W.
10. the polysilicon membrane prepared of the method as described in any one of claim 1 ~ 9.
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| CN103270578A (en) * | 2010-12-30 | 2013-08-28 | 应用材料公司 | Thin film deposition using microwave plasma |
| CN103266352A (en) * | 2013-05-06 | 2013-08-28 | 北京工业大学 | Low cost high-performance polycrystalline silicon base film preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20010028100A1 (en) * | 1997-07-25 | 2001-10-11 | Hughes Electronics Corporation. | Passivation layer and process for semiconductor devices |
| US6239034B1 (en) * | 1998-11-02 | 2001-05-29 | Vanguard International Semiconductor Corporation | Method of manufacturing inter-metal dielectric layers for semiconductor devices |
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