CN100517572C - Polycrystalline silicon thin film and preparation method of component thereof - Google Patents
Polycrystalline silicon thin film and preparation method of component thereof Download PDFInfo
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- CN100517572C CN100517572C CNB2007100188877A CN200710018887A CN100517572C CN 100517572 C CN100517572 C CN 100517572C CN B2007100188877 A CNB2007100188877 A CN B2007100188877A CN 200710018887 A CN200710018887 A CN 200710018887A CN 100517572 C CN100517572 C CN 100517572C
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Abstract
The invention relates to a method for the preparation of polycrystalline silicon thin film and the forming of its components used in solar battery. The said method for the preparation of polycrystalline silicon thin film comprises steps as follows: A. fundus cleaning B. preparation of polycrystalline silicon thin film, which is to inflate argon into the vacuum chamber with high purity silicane as the target when the pressure of the vacuum chamber is pumped to 2 is multipled by 10 to 4 Pa. Apply bias voltage of 200 to 1,000 V between the workpiece support and the vacuum chamber of 45% to 80% in dutyfactor and 300 to 500Gs in magnetic density when the pressure in the vacuum chamber achieves 0.5 to 5 Pa, and make magnetic control sputter coating to form polycrystalline silicon thin film on the aluminium film of the chip surface; When making metallic-membrane plating when the chip temperature is between 25 to 30 degrees centigrade, the temperature of the vacuum chamber is between 25 to 30 degrees centigrade. The invention has advantages of directly obtaining polycrystalline silicon thin film under normal temperature, which makes the preparation and crystallization of the silicon bulk thin film accomplished simultaneously and lower the cost of large-scale preparation of the polycrystalline silicon thin film with simple process in batch production.
Description
Technical field:
The present invention relates to the formation method of the assembly of the preparation of polysilicon membrane and the polysilicon membrane that solar cell uses thereof.
Background technology:
The silicon wafer solar cell costs an arm and a leg, and the silicon cost of material has occupied 50%～60% of silicon wafer solar cell cost.Therefore reduce the solar cell cost, effective way is exactly to reduce the consumption of silicon materials.Photovoltaic industry is just being tried to explore a series of research approaches, wherein the most effectively is exactly to adopt thin silicon substrate.At present, owing to be subjected to the restriction of cutting technique, the silicon wafer substrate thickness of solar cell is approximately 200～300 μ m, and thickness is in the research and development less than 100 μ m silicon substrate technologies of preparing.Up-to-date result of study shows that thickness is that monocrystalline or the polysilicon film of 1 μ m just has photoelectric conversion efficiency preferably.Therefore thin-film solar cells becomes one of the most potential direction of solar cell development.Owing to be subjected to the restriction of material, efficient and stability, multi-crystal silicon film solar battery becomes present one of the developing direction of practical value and market potential that has most.Consider industrial actual needs, research at present mainly concentrates on seeks the meeting point that should raise the efficiency in the large-scale production process on the problem that reduces cost again.At present high temperature chemical vapor deposition methods that adopt more, it is fast that this method has film growth rate, advantages such as the thin film crystallization quality is good, yet this method need be selected heat-resisting backing material, generally require above 1400 ℃, so need the good substrate of thermal stability, these resistant to elevated temperatures backing materials mostly are nonmetallic materials; Because thin film deposition and crystallization need be carried out step by step, therefore the danger of contaminating impurity arranged again, simultaneously because the high temperature substrate that suitable this method prepares polysilicon solar cell is an insulator, the Metal Contact that needs research to make new advances.Therefore existing multi-crystal silicon film solar battery preparation method does not fit into the industrial needs of extensive high efficiency.
Summary of the invention:
The objective of the invention is to avoid the deficiencies in the prior art part and a kind of preparation method that can prepare polysilicon membrane and assembly thereof at normal temperatures is provided, make the preparation and the crystallization of silicon substrate film under vacuum condition, finish synchronously, need not conventional annealing handles, reduce the cost of multi-crystal silicon film solar battery mass preparation when guaranteeing the quality of polysilicon membrane, improved the thin-film solar cells transformation efficiency.
Purpose of the present invention can be by realizing by the following technical solutions: a kind of polysilicon membrane preparation method, and its main feature includes following steps:
A. substrate is cleaned, and the mixed liquor with cleaning fluid and pure water in the ultrasonic cleaning machine carries out surface clean to substrate;
B. polysilicon membrane preparation, as target, pressure is extracted into 2 * 10 in the vacuum chamber body with HIGH-PURITY SILICON
-4Behind the Pa, charge into argon gas to the vacuum chamber body, when pressure reaches 0.5～5Pa in the vacuum chamber body, add the bias voltage of 200～1000V between workpiece car that substrate is installed and vacuum chamber body, duty ratio is 45～80%; Magnetic field intensity 300～500Gs, the beginning magnetron sputtering plating forms polysilicon membrane at the substrate aluminium film surface; Substrate temperature is 25～30 ℃, and during plated film, vacuum chamber body temperature degree is 25～30 ℃.
The material of described polysilicon membrane preparation method's substrate is glass, metal material or plastics flexible material.
When the material of described substrate is non-aluminum, the aluminum film electrode preparation process is arranged between steps A and B, vacuum chamber AM aluminum metallization film is put in cleaned substrate.Described aluminum film electrode preparation process, the method for employing vacuum thermal evaporation, vacuum degree is 5 * 10
-4～9 * 10
-4Pa, deposit thickness are 0.8～5 μ m; For guaranteeing high speed deposition aluminium electrode in low melting point substrates such as plastics, evaporation current is 4000～4500A, and deposition rate is 10～300nm/s.
Described polysilicon membrane preparation method's polysilicon membrane preparation process, described target are Czochralski-Si, polysilicon or amorphous silicon, and the purity of target silicon must be more than 99.99%.
Magnetron sputtering in the described polysilicon membrane preparation process is the DC pulse magnetron sputtering, and the power of magnetron sputtering is 12000～16000W, and power density is 10～13W/cm2.
The distance that described polysilicon membrane preparation process hits with substrate is 50～500mm.
Described polysilicon membrane deposit thickness is 1～5 μ m.
The assembly of described polysilicon membrane, it mainly contains following steps:
A. substrate is cleaned, and the mixed liquor with cleaning fluid and pure water in the ultrasonic cleaning machine carries out surface clean to substrate;
B. aluminum film electrode preparation will be put into vacuum chamber AM aluminum metallization film at the bottom of the cleaned substrate.Described aluminum film electrode preparation process, the method for employing vacuum thermal evaporation, vacuum degree is 5 * 10
-4～9 * 10
-4Pa, deposit thickness are 0.8～5 μ m; For guaranteeing high speed deposition aluminium electrode in low melting point substrates such as plastics, evaporation current is 4000～4500A, and deposition rate is 10～300nm/s;
C. polysilicon membrane preparation as target, is extracted into 2 * 10 with pressure in the vacuum chamber body with HIGH-PURITY SILICON
-4Behind the Pa, charge into argon gas to the vacuum chamber body, when pressure reaches 0.5～5Pa in the vacuum chamber body, add the bias voltage of 200～1000V between workpiece car that substrate is installed and vacuum chamber body, duty ratio is 45～80%; Magnetic field intensity 300～500Gs, the beginning magnetron sputtering plating forms polysilicon membrane at the substrate aluminium film surface; Substrate temperature is 25～30 ℃, and during plated film, vacuum chamber body temperature degree is 25～30 ℃;
D. transparent conductive electrode or comb electrode preparation is coated with transparent conductive electrode or comb electrode on the polysilicon membrane surface; To select purity for use be 99.99% zinc oxide with purity is that 99.99% aluminium oxide mixed sintering becomes the direct current sputtering target, and wherein alumina content is 6～10% mass fractions, and two targets are staggered relatively, and the target spacing is about 40～70mm; The polysilicon membrane rete that plating is good is placed on the position that is higher than two target top edges, 3～10cm towards two targets; Base vacuum is 2～5 * 10 before the sputter
-2Pa is that 99.999% argon gas charges into the operating room by valve with purity, reaches 1～5Pa until air pressure, opens shielding power supply, and the power that raises gradually continues to feed argon gas to system's build-up of luminance; Deposit thickness is 200～500nm;
E. antireflective diaphragm preparation prepares antireflective coating on transparent conductive electrode or polysilicon membrane and comb electrode.Thermal resistance evaporation magnesium fluoride, evaporation current are 1500～1800A, and voltage is 6～10V, and the time is 50～100S.
The invention has the beneficial effects as follows, polysilicon membrane of the present invention and assembly preparation thereof are target with the HIGH-PURITY SILICON, adopt the method for magnetron sputtering applying bias to prepare polysilicon membrane, can directly obtain the polysilicon membrane of high-crystallinity at normal temperatures, make the preparation and the crystallization of silicon substrate film under vacuum condition, finish synchronously, need not subsequent anneal and handle, therefore avoided the danger of contaminating impurity, guarantee the quality of polysilicon membrane, greatly reduced the cost of polysilicon membrane mass preparation simultaneously.Its technology is simple, can produce in batches.
Description of drawings:
Fig. 1: the structural representation sketch of many silicon polycrystalline films of the present invention assembly;
Fig. 2: the polysilicon membrane XRD figure of the embodiment of the invention 1 (the stainless steel-based end);
Fig. 3: the polysilicon membrane XRD figure (aluminum alloy substrate) of the embodiment of the invention 2.
Embodiment:
Below in conjunction with embodiment the present invention is done further concrete description, but embodiments of the present invention are not limited thereto.
The device of the present invention's preparation is seen the list/polysilicon membrane preparation facilities of application on the same day.
Embodiment 1: a kind of polysilicon membrane preparation method.
With the stainless steel is substrate.
A. substrate is cleaned, and the mixed liquor with cleaning fluid and pure water in the ultrasonic cleaning machine carries out surface clean to substrate; Through ultrasonic cleaning 5 minutes, the electrostatic precipitation rifle dried up.
B. aluminum film electrode preparation will be put into vacuum chamber AM aluminum metallization film at the bottom of the cleaned substrate.Described aluminum film electrode preparation process, the method for employing vacuum thermal evaporation, vacuum degree is 5 * 10
-4, deposit thickness is 3 μ m; Evaporation current is 4000～4500A, and deposition rate is 10～300nm/s.
C. adopt the DC pulse magnetron sputtering to prepare polysilicon membrane in same vacuum chamber, target is 99.99% polysilicon block, and pressure in the vacuum chamber body is extracted into 2 * 10
-4Behind the Pa, charge into argon gas to the vacuum chamber body, when pressure reached 0.5～5Pa in the vacuum chamber body, power density was 10W/cm during sputter
2The distance of target and substrate is 300mm, substrate temperature is 25～30 ℃, during plated film, the vacuum chamber body need not heat, and temperature is 25～30 ℃, between workpiece car and vacuum chamber body, add duty ratio and be the Dc bias of 60% 800V, deposit thickness is 2 μ m, observes the crystallization situation of polysilicon membrane under XRD, sees Fig. 2.
As can be seen, except Al (111) and Al (220) Si (111) has appearred also among the figure, Si (220), Si (311) obvious diffraction peak from Fig. 2 XRD diffraction pattern.
Embodiment 2: a kind of polysilicon membrane preparation method.
With aluminium alloy A380 is substrate, and positive after mechanical polishing, ultrasonic cleaning is after 5 minutes, the electrostatic precipitation rifle dries up, and puts on the vacuum chamber work rest, adopts the DC pulse magnetron sputtering to prepare polysilicon membrane, target is 99.99% polysilicon block, and power density is 12W/cm during sputter
2The distance of target and substrate is 500mm, substrate temperature is 25～30 ℃, during plated film, the vacuum chamber body need not heat, and temperature is 25～30 ℃, between workpiece car and vacuum chamber body, add duty ratio and be the Dc bias of 50% 500V, deposit thickness is 2.5m, observes the crystallization situation of polysilicon membrane under XRD, sees Fig. 3.
As can be seen, except Al (111) and Al (220) Si (111) has appearred also among the figure, Si (220), Si (311) obvious diffraction peak from Fig. 3 XRD diffraction pattern.
Embodiment 3: a kind of preparation method of polysilicon film component.
Fig. 1 has provided a kind of concrete structure schematic diagram of polysilicon film component of the present invention.As seen from Figure 1, the structure at the bottom of this non-aluminum base is substrate (A); Aluminum film electrode (B); Polysilicon membrane (C); Transparent conductive electrode or comb electrode (D); Antireflective diaphragm (E).
A. substrate is cleaned, and the mixed liquor with cleaning fluid and pure water in the ultrasonic cleaning machine carries out surface clean to substrate.
B. aluminum film electrode preparation is put into vacuum chamber AM aluminum metallization film with cleaned substrate.
C. polysilicon membrane preparation, with HIGH-PURITY SILICON as target, after pressure is extracted into 2 * 10-4Pa in the vacuum chamber body, charge into argon gas to the vacuum chamber body, when pressure reaches 0.5～5Pa in the vacuum chamber body, add the bias voltage of 200～1000V between workpiece car and vacuum chamber body, duty ratio is 45～80%; Magnetic field intensity 300～500Gs, the beginning magnetron sputtering plating forms polysilicon membrane at the substrate aluminium film surface; Substrate temperature is 25～30 ℃, and during plated film, vacuum chamber body temperature degree is 25～30 ℃.
D. transparent conductive electrode or comb electrode preparation is coated with transparent conductive electrode or comb electrode on the polysilicon membrane surface; To select purity for use be 99.99% zinc oxide with purity is that 99.99% aluminium oxide mixed sintering becomes the direct current sputtering target, and wherein alumina content is 6～10% mass fractions, and two targets are staggered relatively, and the target spacing is about 40～70mm; The polysilicon membrane rete that plating is good is placed on the position that is higher than two target top edges, 3～10cm towards two targets; Base vacuum is 2～5 * 10 before the sputter
-2Pa is that 99.999% argon gas charges into the operating room by valve with purity, reaches 1～5Pa until air pressure, opens shielding power supply, and the power that raises gradually continues to feed argon gas to system's build-up of luminance; Deposit thickness is 200～500nm.
E. antireflective diaphragm preparation prepares antireflective coating on transparent conductive electrode or polysilicon membrane and comb electrode.Open magnesium fluoride evaporation power supply, evaporation current is 1500～1800A, and voltage is 6～10V, and the time is 50～100S.
Embodiment 4: a kind of preparation method of polysilicon film component.
With aluminium alloy A380 is substrate.
Its steps A, C are identical with embodiment 2, and step D, E are identical with embodiment 4.
Claims (7)
1. polysilicon membrane preparation method, its feature includes following steps:
A. substrate is cleaned, and the mixed liquor with cleaning fluid and pure water in the ultrasonic cleaning machine carries out surface clean to substrate;
B. polysilicon membrane preparation, as target, pressure is extracted into 2 * 10 in the vacuum chamber body with HIGH-PURITY SILICON
-4Behind the Pa, charge into argon gas to the vacuum chamber body, when pressure reaches 0.5～5Pa in the vacuum chamber body, add the bias voltage of 200～1000V between workpiece car that substrate is installed and vacuum chamber body, duty ratio is 45～80%; Magnetic field intensity 300～500Gs; The beginning magnetron sputtering plating forms polysilicon membrane at substrate surface; Base reservoir temperature is 25～30 ℃, and during plated film, vacuum chamber body temperature degree is 25～30 ℃.
2. polysilicon membrane preparation method as claimed in claim 1, the material that it is characterized in that described substrate is glass, metal material or plastics flexible material.
3. polysilicon membrane preparation method as claimed in claim 2, when the material that it is characterized in that described substrate is non-aluminum, the aluminum film electrode preparation process is arranged between steps A and B, vacuum chamber AM aluminum metallization film is put in cleaned substrate, described aluminum film electrode preparation process, adopt the method for vacuum thermal evaporation, vacuum degree is 5 * 10
-4～9 * 10
-4Pa, deposit thickness are 0.8～5 μ m; Evaporation current is 4000～4500A, and deposition rate is 10～300nm/s.
4. polysilicon membrane preparation method as claimed in claim 1 is characterized in that in the described polysilicon membrane preparation process, described target is Czochralski-Si, polysilicon or amorphous silicon, and the purity of target silicon must be more than 99.99%.
5. as claim 1 or 2 or 3 or 4 described polysilicon membrane preparation methods, it is characterized in that the magnetron sputtering in the described polysilicon membrane preparation process is the DC pulse magnetron sputtering, the power of magnetron sputtering is 12000～16000W, and power density is 10～13W/cm
2
6. polysilicon membrane preparation method as claimed in claim 5 is characterized in that the distance that described polysilicon membrane preparation process hits with substrate is 50～500mm.
7. polysilicon membrane preparation method as claimed in claim 1 is characterized in that described polysilicon membrane deposit thickness is 1～5 μ m.
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| CNB2007100188877A CN100517572C (en) | 2007-10-09 | 2007-10-09 | Polycrystalline silicon thin film and preparation method of component thereof |
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| CNB2007100188877A CN100517572C (en) | 2007-10-09 | 2007-10-09 | Polycrystalline silicon thin film and preparation method of component thereof |
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| CN2008102100526A Division CN101404304B (en) | 2007-10-09 | 2007-10-09 | Production method for polysilicon film component |
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| CN101781794B (en) * | 2008-12-30 | 2012-05-23 | 兰州大成科技股份有限公司 | Method for preparing low-doping rate polycrystalline silicon films |
| CN101660208B (en) * | 2009-06-25 | 2011-07-27 | 南安市三晶阳光电力有限公司 | Method for reducing polysilicon cast ingot stress |
| CN102787295A (en) * | 2012-07-27 | 2012-11-21 | 中国科学院电工研究所 | Method for preparing CdTe polycrystalline film |
| CN102881563B (en) * | 2012-10-16 | 2015-07-08 | 浙江工商职业技术学院 | Preparation method of polycrystalline silicon film component |
| CN104975260B (en) * | 2015-08-05 | 2018-05-01 | 大连大学 | A kind of preparation method of high crystallization rate polysilicon membrane |
| CN109904392A (en) * | 2017-12-07 | 2019-06-18 | 中国科学院上海硅酸盐研究所 | A kind of lithium air battery positive electrode composite material and preparation method |
| CN115020543B (en) * | 2022-05-30 | 2024-07-26 | 重庆理工大学 | ReS2(1-x)Se2xManufacturing method of Schottky junction type photoelectric detector and detector |
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