CN101673786B - Preparation method of CdTe solar cell in magnetic field - Google Patents
Preparation method of CdTe solar cell in magnetic field Download PDFInfo
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- CN101673786B CN101673786B CN2009102016126A CN200910201612A CN101673786B CN 101673786 B CN101673786 B CN 101673786B CN 2009102016126 A CN2009102016126 A CN 2009102016126A CN 200910201612 A CN200910201612 A CN 200910201612A CN 101673786 B CN101673786 B CN 101673786B
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Abstract
The invention discloses a preparation method of a CdTe solar cell in a magnetic field, which comprises the following process steps: pretreating a transparent glass substrate; preparation of In on a transparent glass substrate2O3F a transparent conductive film; putting the glass substrate into a close space sublimation furnace, and growing a CdS buffer layer on the glass substrate; growing a CdTe absorption film on the prepared CdS film by using a near space sublimation method, and applying a magnetic field of 1-15T to the substrate through a superconducting magnet coil to grow a CdTe absorption layer; sputtering a metal back electrode on the surface of CdTe to form ohmic contact; and obtaining the CdTe thin film solar cell. The CdTe solar cell is prepared by using a near space sublimation method in a strong magnetic field, the surface flatness and the compactness of the CdTe absorption film are obviously improved, and the conversion efficiency of the CdTe film solar cell is improved.
Description
Technical field
The present invention relates to a kind of manufacturing approach, belong to nm inorganic compound energy and material manufacturing process field based on cadmium telluride (CdTe) thin film solar cell.
Background technology
Solar energy is a kind of cleaning, pollution-free, inexhaustible natural energy resources, and the natural resources that the mankind depend on for existence almost all is transformed in solar energy, and directly converting solar energy into electric energy is an important technology basis that utilizes solar energy on a large scale.From AT&T Labs in 1954 since to develop efficient be first polycrystalline silicon solar cell of 6%, solar cell market is with annual 35% speed increase now.
CdTe is a kind of compound semiconductor, in solar cell, generally makes absorbed layer.Because its direct band gap is 1.45eV; Be suitable for most photovoltaic energy conversion; Therefore making the CdTe absorbed layer of about 2 micron thick reach 90% at its optical absorptivity more than band gap becomes possibility, the highest theoretical transformation efficient of permission under air quality AM1.5 condition up to 27%.CdTe is deposited as large-area film easily, and deposition rate is also high.Therefore, the manufacturing cost of CdTe thin film solar cell is lower, is a kind of preferably novel solar cell of application prospect, has become the main object of state's research and development such as U.S.A, moral, day, meaning.At present, acquired peak efficiency is 16.5 (1cm), and battery module efficient reaches 11% (0.94m).Yet current characteristics and the preparation method's to the CdTe solar cell of people understanding is very scattered, the understanding of neither one system.
In recent years, the application that magnetic field intensity surpasses the superconducting intense magnetic field of 10T gets more and more people's extensive concerning, and high-intensity magnetic field can suspend in high-intensity magnetic field like water plastics, timber etc. so that the nonferromagnetic material also can demonstrate intrinsic magnetic properties because of its superpower magnetization.The object that acts on macroscopic view with the general magnetic field is different, and high-intensity magnetic field can be delivered to high-intensity magnetic energy the atomic scale of material, changes the behaviors such as arrangement, coupling and migration of atom, thereby the tissue and the performance of material produced far-reaching influence.High-intensity magnetic field is ability control material form, size, distribution and orientation in crystal growing process or the like in material preparation.Thereby influence the institutional framework of material, the final new material that obtains to have premium properties.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of CdTe solar cells under magnetic field; Under magnetic field, use the near space sublimed method to prepare the CdTe solar cell; The surface smoothness of CdTe absorbing membrane and compactness have all had very obviously to be improved, and has improved the transformation efficiency of CdTe thin film solar cell.
For realizing above-mentioned purpose, the present invention takes following technology step scheme:
A kind of preparation method of CdTe solar cells under magnetic field, the near space sublimed method prepares the CdTe thin film solar cell under the employing magnetic field on transparent conducting glass, and this method has following processing step:
A, transparent glass substrate preliminary treatment;
B, on transparent glass substrate, prepare In
2O
3: the F transparent conductive film;
C, put into the near space subliming furnace that has the superconducting magnet coil to the glass substrate for preparing transparent conductive film, growth one deck CdS resilient coating on glass substrate;
D, on the CdS film for preparing, use near space sublimed method growth CdTe absorbing membrane: said substrate is applied the magnetic field of 1～15T, growth one deck CdTe absorbing membrane on the glass substrate for preparing the CdS film through said superconducting magnet coil;
E, use magnetic control sputtering device are at CdTe surface sputtering metal back electrode, 400 ℃ of formation ohmic contact of annealing down;
F, acquisition CdTe thin film solar cell.
Further, said metal back electrode can be nickel electrode or aluminium electrode or copper electrode or gold electrode.
Further; The transparent glass substrate preliminary treatment is meant and adopts clear glass as deposition substrate among the said step a; Adopt acetone ultrasonic cleaning 5～15min, to remove the grease of glass surface, deionized water ultrasonic cleaning 10～20min removes glass surface impurity then; With putting into pretreatment chamber after the glass oven dry, use plasma that glass substrate is cleaned at last.
Further, prepare In among the said step b
2O
3: the F transparent conductive film is meant that sputtering target material is high-purity In through magnetic control sputtering device sputter one floor height conductive layer on transparent glass substrate
2O
3, with vacuum pump sputtering chamber is evacuated to below the 5Pa earlier, with molecular pump reative cell is evacuated to 10 then
-2PaBelow, feed Ar gas and 5%CHF
3, the adjusting flow is 30～60ml/min; Conditioned reaction air pressure is 0.2～0.5Pa; Sputtering power 100～500W; Sputtering time 0.5～2h.
Further, growth CdS resilient coating is meant and with vacuum pump subliming furnace is evacuated to below the 5Pa earlier among the said step c, with molecular pump subliming furnace is evacuated to 10 then
-2PaBelow, feed 50%Ar gas and 50%O
2, the adjusting flow is 5～20ml/min; Adjusting air pressure is 500～2000Pa; Regulating infrared Halogen lamp LED, to make the sublimation source temperature be 550～620 ℃, and underlayer temperature is 500～550 ℃, and source and substrate distance are 2～8mm; The distillation time is 3～10s, closes sublimation source after preparing the CdS film, feeds 80%Ar gas and 20%O
2, keep underlayer temperature at 400 ℃ of following annealing in process 20min.。
Further, growth CdTe absorbing membrane is meant and with vacuum pump subliming furnace is evacuated to below the 5Pa earlier in the said steps d, with molecular pump subliming furnace is evacuated to 10 then
-2PaBelow, feeding Ar gas, the adjusting flow is 5～20ml/min; Adjusting air pressure is 500～2000Pa; Through the superconducting magnet coil substrate is applied the magnetic field of 1～15T, regulating infrared Halogen lamp LED subsequently, to make the sublimation source temperature be 560～600 ℃; Underlayer temperature is 480～520 ℃, and source and substrate distance are 1～5mm; The distillation time is 0.5～2min; Grown and closed sublimation source behind the CdTe absorbing membrane, keeping underlayer temperature is 480～520 ℃, and the maintenance magnetic field intensity is 1～15T, and the CdTe absorbing membrane is carried out annealing in process, and the processing time is 30～50min.
Further, use magnetic control sputtering device to be meant among the said step e and with vacuum pump sputtering chamber is evacuated to below the 5Pa earlier, with molecular pump reative cell is evacuated to 10 then at CdTe surface sputtering metal back electrode
-2PaBelow, feeding Ar gas, adjusting air pressure is 0.3～0.5Pa; Sputtering power is 200～500W; Sputtering time is 20～40min, at last with hull cell 400 ℃ of annealing in process 1～2h in Ar gas.Make electrode form good Ohmic contact.
The present invention adopts near space sublimed method growing high-quality CdTe thin film solar cell in the magnetic field of 1～15T, be raw material with high-purity CdS and CdTe powder, adopts infrared Halogen lamp LED as heating source in the test, and source and substrate distance are 1～5mm; Reative cell background air pressure less than 5Pa after, feed Ar gas, the temperature in source is at 560～600 ℃; Underlayer temperature is between 480～520 ℃, and magnetic field intensity is the adjustable 1～15T that remains on continuously.
High-intensity magnetic field can be delivered to high-intensity magnetic energy the atomic scale of material, behaviors such as the arrangement of change atom and migration.High-intensity magnetic field is the form in the may command material growth course, size and distribution or the like in material preparation, thereby influences the institutional framework of material.Place magnetic field to carry out the distil process of CdTe solar cell of near space; Utilize magnetic field to the extremely strong magnetizing force of material, magnetic energy effect and to the Lip river logical sequence magnetic force of moving charge; The activation and the disassociation of ability intensified response thing promote the interaction between electronics, CdS, the CdTe isoreactivity group, make the more growth of densification of CdTe absorbing membrane; Be magnetic field direction of growth with regard to an optimization of compulsory formation between film growth, influence and control growth for Thin Film process.Under high-intensity magnetic field, use the near space sublimed method to prepare the CdTe solar cell, the surface smoothness of CdTe absorbing membrane and compactness have all had very obviously to be improved.
Characteristics of the present invention are under magnetic field, to adopt the near space sublimed method to prepare high-quality CdTe thin film solar cell.Under the effect in magnetic field; On substrate, deposit the thick high-quality CdTe absorbing membrane of 200～600nm; The present invention is through regulating magnetic field intensity with control growth for Thin Film density; Can overcome prepared CdTe film quality difference of additive method and shaggy shortcoming, be a kind of very effective method for preparing efficient high-quality CdTe thin film solar cell.
Figure of description
Fig. 1 is the structural representation of equipment used herein;
The drawing reference numeral explanation:
1. infrared Halogen lamp LED, 2. sublimation source, 3. magnet, 4. substrate table, 5. sublimation source baffle plate
Embodiment
Further specify technical scheme of the present invention below in conjunction with embodiment.
Infrared Halogen lamp LED 1 is as heating source among the present invention, and temperature is adjustable continuously; Substrate is placed on liftable, on the rotatable substrate table 4; Sublimation source baffle plate 5 is arranged between sublimation source 2 and the substrate, can cut off sublimation source 2; Magnetic field is produced by superconducting magnet 3.
Embodiment:
(1) at first to the transparent glass substrate preliminary treatment: adopt 1713 clear glasses as deposition substrate, adopt the acetone ultrasonic cleaning, to remove the grease of glass surface, glass surface impurity is removed in the deionized water ultrasonic cleaning then; With putting into pretreatment chamber after the glass oven dry, use plasma that glass substrate is cleaned at last.
(2) preparation In
2O
3: the F transparent conductive film: transparent glass substrate is being delivered under the vacuum environment on the sample stage of magnetic control sputtering device by mechanical arm automatically, and sputtering target material is high-purity In
2O
3, with vacuum pump sputtering chamber is vacuumized earlier, with molecular pump reative cell is vacuumized then, feed Ar gas and 5%CHF3, regulate flow; Conditioned reaction air pressure and sputtering power, the sputter certain hour.
(3) growth CdS film: the substrate that will prepare transparent conductive film is being passed under the vacuum environment on the near space subliming furnace substrate table 4 by mechanical arm automatically, and sublimation source 2 is high-purity CdS powder; With vacuum pump subliming furnace is vacuumized earlier, with molecular pump subliming furnace is vacuumized then, feed 50%Ar gas and 50%O
2, regulate flow, regulate air pressure; Regulating infrared Halogen lamp LED 1 makes sublimation source 2 and substrate keep uniform temperature, adjusting source and substrate distance; The distillation certain hour.
(4) CdS film annealing in process: close sublimation source 2 after preparing the CdS film, feed 80%Ar gas and 20%O
2, keep underlayer temperature at 400 ℃ of following annealing in process 20min.
(5) growth CdTe absorbing membrane: the substrate that will prepare the CdS film is put into the vacuum plant of the near space subliming furnace that has superconducting magnet 3, with vacuum pump subliming furnace is vacuumized earlier, with molecular pump subliming furnace is vacuumized then, feeds Ar gas, regulates flow; Regulate air pressure; Apply the magnetic field of certain intensity through 3 pairs of substrate bases of superconducting magnet, regulate infrared Halogen lamp LED subsequently and make sublimation source 2 and substrate keep uniform temperature, adjusting source and substrate distance; The distillation certain hour.
(6) CdTe absorbing membrane annealing in process: close sublimation source behind the CdTe absorbing membrane of having grown, keep substrate to reach uniform temperature, keep magnetic field intensity, the CdTe absorbing membrane is carried out annealing in process, handle certain hour.
(7) back electrode preparation: in the sputtering chamber of magnetic control magnetic control sputtering device, prepare back electrode; Sputtering target material is high-purity N i, with vacuum pump sputtering chamber is vacuumized earlier, with molecular pump reative cell is vacuumized then; Feed Ar gas, regulate air pressure and sputtering power and sputtering time.With hull cell 400 ℃ of annealing in process certain hours in Ar gas, make electrode form better ohmic contact at last.
The specified data of according to the form below prepare the CdTe thin film solar cell by above-mentioned steps under the magnetic field on transparent conducting glass:
| Step (2) molecular pump vacuumizes air pressure (Pa) | 10 -3 | 2×10 -3 | 2×10 -3 | 3×10 -3 | 3×10 -3 |
| Step (2) feeds mixed gas flow (ml/min) | 30 | 40 | 45 | 50 | 60 |
| Step (2) reaction pressure (Pa) | 0.2 | 0.3 | 0.35 | 0.4 | 0.5 |
| Step (2) sputtering power (w) | 100 | 200 | 300 | 400 | 500 |
| Step (2) sputtering time (h) | 0.5 | 0.8 | 1.2 | 1.6 | 2 |
| Step (3) vacuum pump vacuumizes (Pa) | 5 | 3 | 2 | 2 | 1 |
| Step (3) molecular pump vacuumizes (Pa) | 10 -3 | 2×10 -3 | 2×10 -3 | 3×10 -3 | 3×10 -3 |
| Step (3) feeds mixed gas flow (ml/min) | 5 | 8 | 12 | 16 | 20 |
| Step (3) reaction pressure (Pa) | 500 | 80 | 1200 | 1600 | 2000 |
| Step (3) sublimation source temperature (℃) | 550 | 570 | 590 | 600 | 620 |
| Step (3) underlayer temperature (℃) | 500 | 510 | 520 | 540 | 550 |
| Step (3) source and substrate distance (mm) | 2 | 4 | 5 | 7 | 8 |
| Step (3) distillation time (s) | 3 | 5 | 7 | 9 | 10 |
| Step (5) vacuum pump vacuumizes air pressure (Pa) | 5 | 3 | 2 | 2 | 1 |
| Step (5) molecular pump vacuumizes air pressure (Pa) | 10 -3 | 2×10 -3 | 2×10 -3 | 3×10 -3 | 3×10 -3 |
| Step (5) feeds Ar throughput (ml/min) | 5 | 8 | 12 | 16 | 20 |
| Step (5) reaction pressure (Pa) | 500 | 80 | 1200 | 1600 | 2000 |
[0040]
| Step (5) magnetic field intensity (T) | 1 | 4 | 8 | 12 | 15 |
| Step (5) sublimation source temperature (℃) | 560 | 570 | 580 | 590 | 600 |
| Step (5) underlayer temperature (℃) | 480 | 490 | 500 | 510 | 520 |
| Step (5) source and substrate distance (mm) | 1 | 2 | 3 | 4 | 5 |
| Step (5) distillation time (min) | 0.5 | 0.8 | 1.2 | 1.6 | 2 |
| Step (6) underlayer temperature (℃) | 480 | 490 | 500 | 510 | 520 |
| Step (6) magnetic field intensity (T) | 1 | 4 | 8 | 12 | 15 |
| Step (6) processing time (min) | 30 | 35 | 40 | 45 | 50 |
| Step (7) vacuum pump vacuumizes air pressure (Pa) | 5 | 3 | 2 | 2 | 1 |
| Step (7) molecular pump vacuumizes air pressure (Pa) | 10 -3 | 2×10 -3 | 2×10 -3 | 3×10 -3 | 3×10 -3 |
| Step (7) is regulated air pressure (Pa) | 0.3 | 0.35 | 0.4 | 0.45 | 0.5 |
| Step (7) sputtering power (w) | 200 | 250 | 300 | 400 | 500 |
| Step (7) sputtering time (mi n) | 20 | 25 | 30 | 35 | 40 |
| Step (7) annealing in process time (h) | 1 | 1.2 | 1.6 | 1.8 | 2 |
Through to above prepared CdTe solar cell, use the solar simulator test after, the result shows that the photoelectric conversion efficiency of CdTe thin film solar cell is excellent, battery efficiency is greater than 13%.Through the epitaxial growth CdTe hull cell on glass substrate of near space sublimating technologe under high-intensity magnetic field, the accurate thickness of the growth of control material and layers of material, thus further improve the efficient of solar cell.
Those skilled in the art will recognize that; Above-mentioned embodiment is exemplary; Be in order better to make those skilled in the art can understand this patent; Can not be interpreted as it is the restriction that this patent is comprised scope, so long as according to spirit that this patent discloses done anyly be equal to change or modify, all fall into the scope that this patent comprises.
Claims (7)
1. the preparation method of a CdTe solar cells under magnetic field is characterized in that: adopt that the near space sublimed method prepares the CdTe thin film solar cell under the magnetic field on transparent conducting glass, this method has following processing step:
A, transparent glass substrate preliminary treatment;
B, on transparent glass substrate, prepare In
2O
3: the F transparent conductive film;
C, put into the near space subliming furnace that has the superconducting magnet coil to the glass substrate for preparing transparent conductive film, growth one deck CdS resilient coating on glass substrate;
D, on the CdS film for preparing, use near space sublimed method growth CdTe absorbing membrane: said substrate is applied the magnetic field of 1～15T, growth one deck CdTe absorbing membrane on the glass substrate for preparing the CdS film through said superconducting magnet coil;
E, use magnetic control sputtering device are at CdTe surface sputtering metal back electrode, 400 ℃ of formation ohmic contact of annealing down;
F, acquisition CdTe thin film solar cell.
2. according to the preparation method of claims 1 described CdTe solar cells under magnetic field, it is characterized in that: said metal back electrode can be nickel electrode or aluminium electrode or copper electrode or gold electrode.
3. according to the preparation method of claims 1 described CdTe solar cells under magnetic field; It is characterized in that: the transparent glass substrate preliminary treatment is meant and adopts clear glass as deposition substrate among the said step a; Adopt acetone ultrasonic cleaning 5～15min; To remove the grease of glass surface, deionized water ultrasonic cleaning 10～20min removes glass surface impurity then; With putting into pretreatment chamber after the glass oven dry, use plasma that glass substrate is cleaned at last.
4. according to the preparation method of claims 1 described CdTe solar cells under magnetic field, it is characterized in that: prepare In among the said step b
2O
3: the F transparent conductive film is meant that sputtering target material is high-purity In through magnetic control sputtering device sputter one floor height conductive layer on transparent glass substrate
2O
3, with vacuum pump sputtering chamber is evacuated to below the 5Pa earlier, with molecular pump reative cell is evacuated to 10 then
-2Below the Pa, feed Ar gas and 5%CHF
3, the adjusting flow is 30～60ml/min; Conditioned reaction air pressure is 0.2～0.5Pa; Sputtering power 100～500W; Sputtering time 0.5～2h.
5. according to the preparation method of claims 1 described CdTe solar cells under magnetic field, it is characterized in that: growth CdS resilient coating is meant and with vacuum pump subliming furnace is evacuated to below the 5Pa earlier among the said step c, with molecular pump subliming furnace is evacuated to 10 then
-2Below the Pa, feed 50%Ar gas and 50%O
2, the adjusting flow is 5～20ml/min; Adjusting air pressure is 500～2000Pa; Regulating infrared Halogen lamp LED, to make the sublimation source temperature be 550～620 ℃, and underlayer temperature is 500～550 ℃, and source and substrate distance are 2～8mm; The distillation time is 3～10s; Close sublimation source after preparing the CdS film, feed 80%Ar gas and 20%O
2, keep underlayer temperature at 400 ℃ of following annealing in process 20min.
6. according to the preparation method of claims 1 described CdTe solar cells under magnetic field, it is characterized in that: growth CdTe absorbing membrane is meant and with vacuum pump subliming furnace is evacuated to below the 5Pa earlier in the said steps d, with molecular pump subliming furnace is evacuated to 10 then
-2Below the Pa, feed Ar gas, the adjusting flow is 5～20ml/min; Adjusting air pressure is 500～2000Pa; Through the superconducting magnet coil substrate is applied the magnetic field of 1～15T, regulating infrared Halogen lamp LED subsequently, to make the sublimation source temperature be 560～600 ℃; Underlayer temperature is 480～520 ℃, and source and substrate distance are 1～5mm; The distillation time is 0.5～2min; Grown and closed sublimation source behind the CdTe absorbing membrane, keeping underlayer temperature is 480～520 ℃, and the maintenance magnetic field intensity is 1～15T, and the CdTe absorbing membrane is carried out annealing in process, and the processing time is 30～50min.
7. according to the preparation method of claims 1 described CdTe solar cells under magnetic field; It is characterized in that: use magnetic control sputtering device to be meant among the said step e and with vacuum pump sputtering chamber is evacuated to below the 5Pa earlier, with molecular pump reative cell is evacuated to 10 then at CdTe surface sputtering metal back electrode
-2Below the Pa, feed Ar gas, adjusting air pressure is 0.3～0.5Pa; Sputtering power is 200～500W; Sputtering time is 20～40min, at last with hull cell 400 ℃ of annealing in process 1～2h in Ar gas, makes electrode form good Ohmic contact.
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