CN101838794A - Method for preparing titania film by using gas flow reaction sputtering under middle gas pressure and method for preparing solar cell - Google Patents
Method for preparing titania film by using gas flow reaction sputtering under middle gas pressure and method for preparing solar cell Download PDFInfo
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- CN101838794A CN101838794A CN201010186538A CN201010186538A CN101838794A CN 101838794 A CN101838794 A CN 101838794A CN 201010186538 A CN201010186538 A CN 201010186538A CN 201010186538 A CN201010186538 A CN 201010186538A CN 101838794 A CN101838794 A CN 101838794A
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Abstract
The invention discloses a method for preparing a titania film by using gas flow reaction sputtering under a middle gas pressure and a method for preparing a solar cell. The preparation method for the titania film comprises the following steps of: A), placing a glass substrate plated with a transparent conducting film into a reaction chamber of vacuum sputtering coating equipment and vacuumizing the reaction chamber; and B), introducing a working gas into a target chamber between a pair of titanium targets which is oppositely arranged in a cathode device of the vacuum sputtering coating equipment, and introducing oxygen outside the target chamber, wherein the sputtering gas pressure of the working gas is 10 to 100 Pa, and a TIO2 film is formed on the transparent conducting film by sputtering deposition. The method improves the sputtering gas pressure, and prevents high-energy superoxide anions O- and neutral argon particles from bombarding the substrate so as to reduce crystal defects and improve the electrical conductivity and the thermal stability of the TIO2 film.
Description
Technical field
The present invention relates to the method for reactive sputtering plating titanium deoxid film and the technology of preparation solar cell.
Background technology
With glass is that the non-crystalline silicon of substrate or the preceding nesa coating of amorphous/microcrystalline silicon solar cell mostly are with adulterated stannic oxide of fluorine or adulterated zinc oxide.But since the specific refractory power of these transparent films be 1.9～2.0 and the specific refractory power of non-crystalline silicon to be 3.6～4.0. make light on transparent film and non-crystalline silicon interface very big reflection loss be arranged.In order to reduce reflection loss, can between nesa coating and amorphous silicon film, insert a skim.Its specific refractory power should be the geometrical mean of nesa coating and non-crystalline silicon specific refractory power.And this tunic must have certain electroconductibility.
Titanium dioxide TiO
2Film is transparent insulating film under normal conditions.Its semi-conductor energy gap is about 3.5 electron-volts.Its specific refractory power is 2.3～2.6.In making processes, to its doping,, perhaps control the content of oxygen as mixing with transition element niobium (Nb), can obtain TiO transparent and conduction
2Film.So TiO
2Become the candidate material that this anti-reflection is used.TiO
2Film can prepare by several different methods, for example: chemical vapour deposition, magnetron sputtering, sol-gel method, or pulse laser method of evaporation.The pulse laser method of evaporation needs the heat substrate, and is not suitable for large-scale industrial production.The TiO that sol-gel method can't obtain conducting electricity
2Film.
Magnetron sputtering method can obtain titanium dioxide film by adulterated TiOx ceramic target of sputter or the adulterated metal titanium targets of reactive sputtering.Usually the sputtering pressure of magnetron sputtering reaction is between 0.1Pa～10Pa, this is because magnetron sputtering method mainly is by the electronics acceleration of circling round in magnetic field, and utilize magnetic field with electron confinement near target surface, improving it participates in atomic collision and makes its ionized probability, thereby generation high density plasma, that supervenes in this process has high-energy oxonium ion and a neutral argon particle, the oxonium ion of high energy and neutral argon particle bombardment substrate, thereby cause sustaining damage in the crystal length, cause lattice defect, these defectives can become the heavily connection center in unbound electron and hole, thereby reduce the electroconductibility of film, also can reduce TiO
2Thermostability in the presence of air.From the principle of magnetron sputtering reaction we as can be seen, the magnetron sputtering reaction only suits to carry out under subatmospheric, this is because under the high sputtering pressure, the mean free path of electronics shortens, the magnetically confined effect is no longer obvious, and electronics no longer concentrates near the target surface, and electron density reduces greatly.Being used for the ion density of sputter has all reduced, and therefore can reduce deposition.
In addition, reaction magnetocontrol sputtering is easy to take place the target intoxicating phenomenon.Reactive sputtering titanium target particularly.Unless use complicated loop control system accurately to grasp the working point, just can avoid this phenomenon.Be difficult to control just because of magnetron sputtering method, and technological process poor repeatability is difficult to obtain stable and high-quality electrically conducting transparent titanium dioxide film, makes magnetron sputtering method prepare TiO
2Film is subjected to great limitation in solar cell application.
Summary of the invention
The present invention seeks to overcome the shortcoming of titanium deoxid film preparation method in the prior art, a kind of preparation method that can obtain high-quality titanium deoxid film is provided, and the method for preparing solar cell.
For achieving the above object, the technical solution used in the present invention is: air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in a kind of the application, and it comprises the steps
A), the glass substrate that will be coated with nesa coating puts into the reaction chamber of vacuum sputtering coating equipment, described reaction chamber is vacuumized;
B), the cathode assembly of described vacuum sputtering coating equipment has the titanium target of pair of opposing, feed working gas in the target chamber between described a pair of titanium target, and outside described target chamber aerating oxygen, the sputtering pressure of wherein said working gas is 10Pa～100Pa, through sputtering sedimentation, deposition obtains TiO on described nesa coating
2Film.
Say that further described nesa coating is SnO
2Or ZnO or InSnO film.
Further, the temperature of described substrate is 25～300 ℃.
Further, the working gas that feeds in the described target chamber is an argon gas, and the throughput ratio of argon gas in the target chamber and oxygen is 200: 1 to 1000: 1.
Further, the titanium content in the described titanium target accounts for more than 99% of weight percent, and the foreign matter content in the described titanium target is less than 0.5% of weight percent.
Further, also contain niobium-dopedly in the described titanium target, and the atomic ratio of titanium and niobium is 100: 2～5 in the described titanium target.
Further, a pair of described titanium target is the pair of plates that is parallel to each other.
Perhaps, a pair of described titanium target is the arc target, and the minor increment between the described arc target is positioned at the exit in described target chamber.
Preferably, be added with direct current or the rf bias less than 0V on the described substrate more than or equal to-100V.
The present invention also provides a kind of method for preparing solar cell, and it comprises the steps
A, cleaning transparent conducting glass substrate, described transparent conducting glass substrate has nesa coating;
B, the method that adopts air pressure air-flow reactive sputtering in the aforesaid application to prepare titanium dioxide nano-film are plated titanium deoxid film on the nesa coating of described transparent conducting glass substrate;
C, infrared laser are carved nesa coating;
D, utilize plasma enhanced chemical vapor deposition method deposition of amorphous silicon films;
E, green laser are carved amorphous silicon membrane;
F, deposition of aluminum electrode;
H, green laser are carved described aluminium electrode;
I, after tested, the encapsulation, obtain the solar cell finished product.
Further, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, p-i-n a-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, p-i-n a-Si, p-i-n a-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, p-i-n a-Si, p-i-n μ c-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, p-i-na-Si, p-i-n SiGe, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, CdTe, rear electrode.
Perhaps, at described TiO
2After coating thin film is finished, plate ZnO film again, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, p-i-n a-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, p-i-n a-Si, p-i-n a-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, p-i-n a-Si, p-i-n μ c-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, p-i-na-Si, p-i-n SiGe, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, CdTe, rear electrode.
The thickness of described ZnO film is smaller or equal to 5 nanometers.
Because the technique scheme utilization, the present invention compared with prior art has following advantage and effect: the sedimentary TiO of air pressure air-flow reactive sputtering during the present invention utilizes
2Film can access and has anatase structured TiO
2Film.Compared with traditional magnetron sputtering, owing to adopted the air-flow sputtering method, only adopt the about beam electrons of electric field, make electronics shake back and forth, so sputter can be operated under the comparison high atmospheric pressure along direction of an electric field.Because gas density increases, the probability of collision of gas atom increases, so the high energy particle entrained energy that can reduce by collision process, thereby has avoided the oxonium ion and the neutral particle bombardment substrate of high energy, has reduced lattice defect, and then has improved TiO
2The electroconductibility of film and TiO
2Thermostability in the presence of air.And, middle air pressure gas stream reactive sputtering depositing Ti O
2, oxygen can not touch the surface of target, does not have the target intoxicating phenomenon, makes technology have good repeatability and can significantly improve sputter rate.
The TiO that utilizes method of the present invention to prepare
2Film refractive index is 2.3～2.6, and resistivity is less than 1000ohm.cm, is that light is buried in oblivion coefficient less than 0.1 under the light-wave irradiation situation of 550 nanometers at wavelength, and sedimentation rate can reach 30nm/min.
Description of drawings
Accompanying drawing 1 is the structural representation one of solar cell;
Accompanying drawing 2 is the structural representation two of solar cell;
Accompanying drawing 3 is the structural representation three of solar cell;
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
The invention discloses the method that air pressure air-flow reactive sputtering in a kind of use prepares titanium dioxide nano-film, be by adopting the high speed argon gas of hollow cathode and big flow, prevent reactant gases contact target surface, increase working gas air pressure in the sputter reaction, the energy of minimizing particle is realized.When therefore oxonium ion and neutral particle impinge upon on the substrate, can not influence TiO
2Growth for Thin Film.
Specifically, it comprises the steps:
A), the glass substrate that will be coated with nesa coating puts into the reaction chamber of vacuum sputtering coating equipment, reaction chamber vacuum tightness is evacuated to 10
-1Pa, this nesa coating is SnO usually
2Or ZnO or InSnO film;
B), the cathode assembly of described vacuum sputtering coating equipment has the titanium target of pair of opposing, titanium content in the described titanium target accounts for more than 99% of weight percent, foreign matter content is less than 0.5% of weight percent, preferably, also be mixed with niobium (Nb) element in the described titanium target, the atomic ratio of titanium and niobium is 100: 2～5 in the described titanium target; Feed working gas in the target chamber between described a pair of titanium target, be preferably argon gas, logical oxygen outside the target chamber, the sputtering pressure of wherein said argon gas is 10Pa～100Pa, optimally, the sputtering pressure of argon gas selects 20Pa, and the throughput ratio of oxygen and argon gas is 1: 500, and substrate temperature is 200～300 ℃, carry out sputtering sedimentation, sputtering power density is 10 watts/every square centimeter, and sputtering time 0.5 minute obtains the TiO of 30 nanometer to 100 nanometer thickness through deposition
2Film.
Further, being added with DC (direct current) or RF (radio frequency) biasing on the described substrate, attracting the part ion accelerating flow, improve the energy of film forming bombardment atom to substrate, negative bias, is preferably-80V less than 0V more than or equal to-100V～-60V.
The titanium target of vacuum sputtering coating equipment of the present invention is the pair of plates target that is parallel to each other; Preferably, vacuum sputtering coating equipment has as Chinese patent application 201010144915.1 disclosed structures, a pair of described titanium target is the arc target, minor increment between the described arc target is positioned at the exit in described target chamber, it is big that the recess of described arc target forms central authorities relatively, the target chamber that two ends are narrow, this structure can better retrain the electronics of target cavity edge.
Prepare TiO below by air pressure air-flow reactive sputtering in the experimental technique test
2The effect of film, air pressure air-flow sputtering method and magnetron sputtering method plating TiO in utilizing respectively
2Film, and compare.
Experiment condition is: sputtering pressure is 30Pa, 300 ℃ of substrate temperatures, and rf bias voltage-80V, oxygen flow are 8sccm, and argon flow amount is 2000sccm, and discharge power is 500W, obtains the TiO that thickness is 300 nanometers
2Film.
Wherein, air pressure air-flow sputtering method during first group and second group adopt, sputtering time 5 minutes.
The 3rd group and the 4th group is adopted magnetron sputtering method, and sputtering time is 2 hours.
Bury in oblivion test through electric conductivity and light and relatively obtain following table, compared with prior art, utilize the TiO of the inventive method preparation
2Have good electrical conductivity and sedimentation rate.
| ? | ??TiO 2The preparation method | Specific conductivity (10 before the heating -3S/cm) | Light is buried in oblivion coefficient (550nm) | Heating back specific conductivity (10 -3S/cm) | Heating back light is buried in oblivion coefficient (550nm) | Specific conductivity/light is buried in oblivion coefficient | Sedimentation rate (nm/min) |
| First group | The air-flow sputter | ??8.333 | ?0.05 | ??2.740 | ??0.02 | ??13.7 | ??30 |
| Second group | The air-flow sputter | ??1.818 | ?0.01 | ??0.952 | ??0.005 | ??19 | ??30 |
| The 3rd group | Magnetron sputtering | ??0.313 | ?0.008 | ??0.002 | ??0.003 | ??0.06 | ??2 |
| The 4th group | Magnetron sputtering | ??12.500 | ?0.2 | ??3.846 | ??0.1 | ??3.85 | ??2 |
The method of utilizing middle air pressure air-flow reactive sputtering of the present invention to prepare titanium dioxide nano-film prepares solar cell, comprises the steps:
A, cleaning transparent conducting glass substrate, described transparent conducting glass substrate has nesa coating;
B, the method that adopts aforesaid middle air pressure air-flow reactive sputtering to prepare titanium dioxide nano-film are plated titanium deoxid film on the nesa coating of transparent conducting glass substrate;
C, infrared laser are carved nesa coating and titanium deoxid film;
D, utilize plasma enhanced chemical vapor deposition method (PECVD) deposition of amorphous silicon films;
E, green laser are carved amorphous silicon membrane;
F, deposition of aluminum electrode;
H, green laser are carved described aluminium electrode;
I, after tested, the encapsulation, obtain the solar cell finished product.
The structure of described solar cell is followed successively by glass substrate, nesa coating, TiO2, p-i-n a-Si, rear electrode, as shown in Figure 1; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO2, p-i-n a-Si, p-i-n a-Si, rear electrode, as shown in Figure 2; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO2, p-i-n a-Si, p-i-n μ c-Si, rear electrode, as shown in Figure 3; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO2, p-i-n a-Si, p-i-n SiGe, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO2, CdTe, rear electrode or the like.
Perhaps, can also be at described TiO
2After coating thin film is finished, plate ZnO film again, the thickness of ZnO film is smaller or equal to 5 nanometers.The structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, p-i-n a-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, p-i-n a-Si, p-i-n a-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, p-i-n a-Si, p-i-n μ c-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, p-i-n a-Si, p-i-n SiGe, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, ZnO, CdTe, rear electrode.
Utilize the TiO of air-flow sputtering method preparation of the present invention
2Film is as antireflective film, the unijunction that obtains and the performance of double junction non-crystal silicon solar energy battery such as following table:
| ? | Battery structure | Open circuit voltage (mV) | Saturation current density (mA/cm 2) | Packing factor (%) | Efficient (%) |
| First group | ??SnO2/TiO2/p-i-n/Al | ??850 | ??12.82 | ??70.5 | ??7.68 |
| Second group | ??SnO2/p-i-n/Al | ??830 | ??12.20 | ??69.3 | ??7.02 |
| The 3rd group | ??SnO2/TiO2/p-i-n/p-i-n/Al | ??1690 | (6.93 on average) | ??71.2 | (8.32 on average) |
| The 4th group | ??SnO2/p-i-n/p-i-n/Al | ??1660 | (6.70 on average) | ??70.1 | (7.80 on average) |
Wherein, first group and the 3rd group are for having TiO
2The solar cell of antireflective film, second group and the 4th group be not for there being TiO
2The control group of antireflective film has TiO as can be seen
2The solar cell of antireflective film all is significantly improved with respect to open circuit voltage, saturation current density, packing factor and the efficient of the solar cell that does not have antireflective film.
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (10)
1. air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in the application, and it is characterized in that: it comprises the steps
A), the glass substrate that will be coated with nesa coating puts into the reaction chamber of vacuum sputtering coating equipment, described reaction chamber is vacuumized;
B), the cathode assembly of described vacuum sputtering coating equipment has the titanium target of pair of opposing, feed working gas in the target chamber between described a pair of titanium target, and outside described target chamber aerating oxygen, the sputtering pressure of wherein said working gas is 10Pa～100Pa, through sputtering sedimentation, deposition obtains TiO on described nesa coating
2Film.
2. air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in the application according to claim 1, it is characterized in that: described nesa coating is SnO
2Or ZnO or InSnO film.
3. air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in the application according to claim 1, it is characterized in that: the temperature of described substrate is 25～300 ℃.
4. air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in the application according to claim 1, it is characterized in that: the working gas that feeds in the described target chamber is an argon gas, and the throughput ratio of argon gas in the target chamber and oxygen is 200: 1 to 1000: 1.
5. air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in the application according to claim 1, it is characterized in that: the titanium content in the described titanium target accounts for more than 99% of weight percent, and the foreign matter content in the described titanium target is less than 0.5% of weight percent.
6. air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in the application according to claim 1, it is characterized in that: a pair of described titanium target is the pair of plates that is parallel to each other.
7. air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in the application according to claim 1, it is characterized in that: a pair of described titanium target is the arc target, and the minor increment between the described arc target is positioned at the exit in described target chamber.
8. air pressure air-flow reactive sputtering prepares the method for titanium deoxid film in the application according to claim 1, it is characterized in that: be added with direct current or radio frequency negative bias on the described substrate, negative bias more than or equal to-100V less than 0V.
9. method for preparing solar cell, it is characterized in that: it comprises the steps
A, cleaning transparent conducting glass substrate, described transparent conducting glass substrate has nesa coating;
B, employing are plated titanium deoxid film as the method that air pressure air-flow reactive sputtering in any described application in the claim 1 to 8 prepares titanium dioxide nano-film on described nesa coating;
C, infrared laser are carved nesa coating;
D, utilize plasma enhanced chemical vapor deposition method deposition of amorphous silicon films;
E, green laser are carved amorphous silicon membrane;
F, deposition of aluminum electrode;
H, green laser are carved described aluminium electrode;
I, after tested, the encapsulation, obtain the solar cell finished product.
10. the method for preparing solar cell according to claim 9 is characterized in that: the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, p-i-n a-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, p-i-na-Si, p-i-n a-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, p-i-na-Si, p-i-n μ c-Si, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, p-i-n a-Si, p-i-nSiGe, rear electrode; Perhaps, the structure of described solar cell is followed successively by glass substrate, nesa coating, TiO
2, CdTe, rear electrode.
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Cited By (5)
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|---|---|---|---|---|
| CN102776481A (en) * | 2012-06-15 | 2012-11-14 | 上海大学 | Method for preparing gradient transition layer between hard film and substrate |
| CN103029371A (en) * | 2012-12-31 | 2013-04-10 | 郭射宇 | Solar selective absorption membrane and preparation method thereof |
| CN103515201A (en) * | 2012-06-29 | 2014-01-15 | 林慧珍 | Method and epitaxial product for forming compound epitaxial layer through chemical bonding |
| CN103668089A (en) * | 2013-12-04 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for sputtering titanium dioxide nanorod arrays on flexible substrate |
| TWI513496B (en) * | 2013-10-23 | 2015-12-21 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776481A (en) * | 2012-06-15 | 2012-11-14 | 上海大学 | Method for preparing gradient transition layer between hard film and substrate |
| CN103515201A (en) * | 2012-06-29 | 2014-01-15 | 林慧珍 | Method and epitaxial product for forming compound epitaxial layer through chemical bonding |
| CN103515201B (en) * | 2012-06-29 | 2016-01-06 | 林慧珍 | Chemical bonded refractory is utilized to form the method for compound epitaxial layer and brilliant product of heap of stone |
| CN103029371A (en) * | 2012-12-31 | 2013-04-10 | 郭射宇 | Solar selective absorption membrane and preparation method thereof |
| TWI513496B (en) * | 2013-10-23 | 2015-12-21 | ||
| CN103668089A (en) * | 2013-12-04 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for sputtering titanium dioxide nanorod arrays on flexible substrate |
| CN103668089B (en) * | 2013-12-04 | 2016-08-17 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method of titanic oxide nanorod array is sputtered in flexible substrates |
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