CN103165743B - The preparation method and halogen doping cadmium telluride diaphragm solar battery and preparation method thereof of halogen doping cadmium telluride - Google Patents
The preparation method and halogen doping cadmium telluride diaphragm solar battery and preparation method thereof of halogen doping cadmium telluride Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of halogen doping cadmium telluride, halogen doping cadmium telluride diaphragm solar battery and preparation method thereof.The preparation method of described halogen doping cadmium telluride comprises: load in reactor according to the first definite quality than weighing by 5N cadmium and 5N tellurium, and to obtain cadmium tellurium mixture, described first definite quality is than being mass ratio between described 5N cadmium and described 5N tellurium; In described reactor according to the second definite quality than the halogenation cadmium adding 4N or more, described second definite quality is than being mass ratio between described halogenation cadmium and described cadmium tellurium mixture; Described reactor is carried out being evacuated to specified vacuum degree and sealing; The described reactor of sealing is put into a heater, carries out hyperthermic treatment; And cooling processing is carried out to the described reactor of the sealing after hyperthermic treatment.The halogen doping cadmium telluride that described halogen doping cadmium telluride diaphragm solar battery and preparation method thereof adopts the preparation method of described halogen doping cadmium telluride to obtain.
Description
Technical field
The present invention relates to the preparation of a kind of cadmium telluride (CdTe) and thin-film solar cells thereof, particularly a kind of preparation method, a kind of halogen doping cadmium telluride diaphragm solar battery and preparation method thereof of halogen doping cadmium telluride.
Background technology
II-VI group semi-conducting material CdTe, its energy gap is 1.46eV, is direct transition type, mates better with solar spectrum, and being the absorbent material that structure photovoltaic cell is good, is also the various light-sensitive device of function admirable and the material of visual display system.CdTe is applied to LEDs, photonics material, biomarker, spectrum analysis, CO
2the Q modulation of laser, infrared modulator, Hg
xcd
1-xte substrate, infrared window electroluminescent device, infrared acquisition, X-ray detection, nuclear activity detector, luminescent device etc. close to visible region.
Show weak P type conductance because CdTe has the Cd room of low concentration, its intrinsic conductivity is very little, improves the electric conductivity of CdTe mainly by adulterating to it.At present, the research report about halogen doping CdTe material is little, and appropriate doping halogen can improve the crystal property of cadmium telluride, reduces defect density, increases carrier concentration, improves its electricity and optical property.The existence of halogen simultaneously can promote CdTe grain growth, improves its structure, pattern and performance further.
Chinese invention patent publication number CN1623014A discloses a kind of CdTe monocrystalline and CdTe polycrystalline and preparation method thereof disclosed in the 1 day June in 2005, wherein loaded in PBN (pyrolytic boron nitride: Pyrolytic Boron Nitride) container by the caddy of 6N cadmium and 6N tellurium and 4N or more, an additional container carries out vacuumizing sealing.This double-layer seal container is put into high-pressure bottle, when the temperature of high-pressure bottle exceedes the fusing point of tellurium or vessel temp sharply rises, reduce amount of power supply, when temperature starts slowly to fall, be heated to 1100 ~ 1130 DEG C keep 1 hour, then cool to room temperature with the furnace.The N of different pressures is passed into (double-layer seal container is outer) in high-pressure bottle in heating process
2, pressure and the outside applied pressure of the generation of maintenance double-layer seal internal tank are constant.Obtain and mix chlorine polycrystalline cadmium telluride, with the polycrystalline cadmium telluride obtained for single crystal tellurium cadmium prepared by raw material.The method to raw material and equipment requirement high, need repeatedly to change pressure, complex process, cost is high, waywardly mixes cl concn.
A kind of P type doping method of cadmium telluride is disclosed in the Chinese invention patent publication No. CN102142481A announced on August 3rd, 2011, the cadmium telluride of wherein employing liquid state or gaseous state and halogen, after functionalization, carry out annealing in process 1-60min at 300 ~ 500 DEG C.The sample homogeneity obtained is poor, complex process, and equipment requirement is higher, easily pollutes.
In addition, prepare halogen doping cadmium telluride film solar cells normally depositing n-type CdS layer on glass film plates, the upper edge depositing p-type CdTe layer again of CdS layer, adopt the modes such as solution infiltration, the evaporation of halogenation cadmium source, ultrasonic atomizatio halogenation cadmium solution to be covered in CdTe surface, then carry out high-temperature process and obtain halogen doping cadmium-telluride layer.On CdTe, edge engages back electrode layer again, forms solar battery structure.There is lack of homogeneity in the method deposition halogenation cadmium, equipment requirement is high, complex process, and the production cycle is long, and production cost is high, and fail safe is low, can produce harm to operating personnel and environment.
Summary of the invention
In view of prior art Problems existing, object of the present invention object is the preparation method providing a kind of halogen doping cadmium telluride, solve exist in existing preparation method to raw material and/or the technical problem such as equipment requirement is high, high, the wayward halogen doping concentration of complex process, cost.
Another object of the present invention is the preparation method providing a kind of thin film solar cell, solve exist in existing preparation method halogenation cadmium lack of homogeneity, complex process, production cost is high, fail safe is low, can produce the technical problems such as harm to operating personnel and environment.
In order to reach above-mentioned purpose of the present invention, in first of the present invention, the invention provides a kind of preparation method of halogen doping cadmium telluride, the preparation method of described halogen doping cadmium telluride comprises step: load in reactor according to the first definite quality than weighing by 5N cadmium and 5N tellurium, to obtain cadmium tellurium mixture, described first definite quality is than being mass ratio between described 5N cadmium and described 5N tellurium; In described reactor according to the second definite quality than the halogenation cadmium adding 4N or more, described second definite quality is than being mass ratio between described halogenation cadmium and described cadmium tellurium mixture; Described reactor is carried out being evacuated to specified vacuum degree and sealing; The described reactor of sealing is put into a heater, carries out hyperthermic treatment; And cooling processing is carried out to the described reactor of the sealing after hyperthermic treatment.
In order to reach above-mentioned purpose of the present invention, in second of the present invention, the invention provides a kind of preparation method of halogen doping cadmium telluride diaphragm solar battery, the preparation method of described halogen doping cadmium telluride diaphragm solar battery comprises step: at SnO
2: F deposition on glass N-type CdS layer; Described N-type CdS layer deposits P type halogen doping cadmium-telluride layer, and the preparation method of the halogen doping cadmium telluride of halogen doping cadmium telluride according to above-mentioned first aspect of the present invention in wherein said P type halogen doping cadmium-telluride layer obtains; Utilize evaporation source ZnTe and evaporation source Cu to deposit on described P type halogen doping cadmium-telluride layer and form back contact; And back electrode layer is deposited on described back contact.
In order to reach above-mentioned purpose of the present invention, in the 3rd face of the present invention, the invention provides a kind of halogen doping cadmium telluride diaphragm solar battery, comprising: SnO
2: F glassy layer; N-type CdS layer, is arranged at described SnO
2: on F glassy layer; P type halogen doping cadmium-telluride layer, is arranged on described CdS layer, and the P type halogen doping cadmium telluride in described P type halogen doping cadmium-telluride layer obtains according to the preparation method of the halogen doping cadmium telluride described in first aspect present invention; Back contact, is arranged on described P type halogen doping cadmium-telluride layer; And back electrode layer; Be arranged on described back contact.
Beneficial effect of the present invention is as follows.
Compared with prior art CN1623014A, the preparation method of halogen doping cadmium telluride of the present invention does not use PBN crucible and high-tension apparatus, greatly reduces equipment requirement; Do not use nitrogen, do not need to regulate reaction vessel external pressure, simple to operate, fail safe is high, cost-saving; Heating process easily controls, sufficient reacting, and aggregate velocity is fast; Can adulterate as required, the content of halogen, close to stoicheiometry, does not have tellurium sedimentary facies.
Compared with prior art CN102142481A, the preparation method of halogen doping cadmium telluride of the present invention adopts solid-state reactants, avoid in the raw material preparation of liquid and gaseous reactant, transport, operating process and be difficult to control, the requirement high problem of, equipment low to ingredient requirement; In the sample obtained, chlorine is evenly distributed, and output is high, and course of reaction easily controls, and reactions steps is comparatively simple, and handling safety, is conducive to the advantages such as suitability for industrialized production.
Compared with prior art, the preparation method of the halogen doping cadmium telluride diaphragm solar battery of the halogen doping cadmium telluride that employing first aspect present invention of the present invention obtains, simplify in existing solar cell technique the halogen that adulterates, the steps such as corrosion and cleaning, decrease operating process and experimental facilities, content of halogen can control as required, for enhancing productivity, reduce the production cycle, reduce production cost, ensure that the purity of material has certain directive significance, can be used for large-scale production, can not to environment and the health endangering operating personnel.
Compared with prior art, the halogen doping cadmium telluride diaphragm solar battery that third aspect present invention obtains also has the beneficial effect identical with second aspect present invention.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of halogen doping cadmium telluride of the present invention;
Fig. 2 is the flow chart of the preparation method of halogen doping cadmium telluride diaphragm solar battery of the present invention;
Fig. 3 is the structural representation of halogen doping cadmium telluride diaphragm solar battery of the present invention.
Wherein, description of reference numerals is as follows:
11 glassy layer 12SnO
2: F layer 13N type CdS layer
14P type halogen doping cadmium-telluride layer 15 back contact 151ZnTe layer
152ZnTe:Cu layer 16 back electrode layer
S1, S2, S3, S4, S5 step S10, S20, S30, S40 step
Embodiment
Below in conjunction with accompanying drawing, the preparation method, halogen doping cadmium telluride diaphragm solar battery and preparation method thereof according to halogen doping cadmium telluride of the present invention is described.Three aspects below will be divided to be described.
The preparation method of first aspect-halogen doping cadmium telluride
The first, the preparation method according to halogen doping cadmium telluride of the present invention is described.
As shown in Figure 1, preparation method according to halogen doping cadmium telluride of the present invention comprises step: load in reactor according to the first definite quality than weighing by 5N cadmium and 5N tellurium, to obtain cadmium tellurium mixture (step S1), wherein, described first definite quality is than being mass ratio between described 5N cadmium and described 5N tellurium; In described reactor according to the second definite quality than the halogenation cadmium (step S2) adding 4N or more, described second definite quality is than being mass ratio between described halogenation cadmium and described cadmium tellurium mixture; Described reactor is carried out being evacuated to specified vacuum degree and seals (step S3); The described reactor of sealing is put into a heater, carries out hyperthermic treatment (step S4); And cooling processing (step S5) is carried out to the described reactor of the sealing after hyperthermic treatment.
In step sl, preferably, described first definite quality ratio is 1: 1 ~ 1.15.
In step sl, described reactor can be quartz ampoule.
In step s 2, preferably, described second definite quality ratio is 0.01 ~ 200mg/kg.
In step s 2, described halogenation cadmium can be selected from any one in cadmium fluoride, caddy, cadmium bromide and cadmium iodide.
In step s3, preferably, described specified vacuum degree is 10
-2~ 10
-5pa.
In step s 4 which, preferably, before the described reactor of sealing is put into heater, described heater is warming up to the first set point of temperature, and described first set point of temperature is below the fusing point of described cadmium; And described hyperthermic treatment comprises step: after the described reactor of sealing is put into described heater, be incubated for the first stipulated time under described first set point of temperature; Afterwards, be warming up to the second set point of temperature with the first heating rate, be incubated for the second stipulated time, described second set point of temperature is more than the fusing point of described tellurium; And afterwards, being warming up to the 3rd set point of temperature with the second heating rate, the 3rd stipulated time of insulation, wherein said second heating rate is lower than described first heating rate, and described 3rd set point of temperature is more than the fusing point of described halogenation cadmium.More preferably, described first set point of temperature is 100 ~ 300 DEG C, and described first stipulated time is 10 ~ 30min; Described first heating rate is 12 ~ 15 DEG C/min, and described second set point of temperature is 700 ~ 900 DEG C, and described second stipulated time is 8 ~ 30min; Described second heating rate is 1 ~ 5 DEG C/min, and described 3rd set point of temperature is 1092 ~ 1200 DEG C, and described 3rd stipulated time is 10 ~ 18min.Certainly in alternative, described heater before the described reactor of sealing is put into heater is in the present invention warming up to the first set point of temperature and under described first set point of temperature, was incubated for the first stipulated time after the described reactor of sealing is put into described heater and can be replaced by: ramp to the first set point of temperature according to the rules after the described reactor of sealing is put into described heater, was incubated for the first stipulated time.
In step s 5, described cooling processing can adopt various ways.First kind of way is: described reactor monolith directly taken out in described heater, makes described reactor carry out room temperature cooling.The second way is: the temperature of described reactor is down to predetermined temperature with predetermined cool down rate, the insulation scheduled time; Afterwards described reactor is directly taken out in described heater, make described reactor carry out room temperature cooling.Under the described second way, preferably, described predetermined cool down rate is 0.1 ~ 20 DEG C/min, and described predetermined temperature is 900 ~ 1080 DEG C, and the described scheduled time is 10 ~ 360min.The third mode is: to specify that described reactor takes out by movement velocity in described heater, make described reactor carry out room temperature cooling.Under a third procedure, preferably, described regulation movement velocity is 1 ~ 20mm/h.
The second, provide the embodiment of the preparation method according to halogen doping cadmium telluride of the present invention.Wherein, in the examples below, Synthesis conversion is the quality of target product after reaction and the ratio of the front raw material gross mass of reaction, is expressed as a percentage.
Embodiment 1
(1) first, by 5N cadmium and 5N tellurium by 1: 1 quality load reactor than weighing 500g and obtain cadmium tellurium mixture;
(2) be that 15mg/kg adds 4N caddy in above-mentioned reactor according to the mass ratio of caddy and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-2pa also seals;
(4) heating process is as follows: when heater is warming up to 200 DEG C, put into by the reactor of good seal, after insulation 10min, 700 DEG C are warming up to heating rate 13 DEG C/min, insulation 15min, is then warming up to 1150 DEG C with heating rate 3 DEG C/min, insulation 10min;
(5) cooling procedure is as follows: taken out from above-mentioned heater by reactor with the speed of 1mm/h, carries out room temperature cooling;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 97.2%
Embodiment 2
(1) first, by 5N cadmium and 5N tellurium by 1: 1.13 quality load reactor than weighing 450g and obtain cadmium tellurium mixture;
(2) be that 50mg/kg adds 5N caddy in above-mentioned reactor according to the mass ratio of caddy and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-2pa also seals;
(4) heating process is as follows: when heater is warming up to 200 DEG C, put into by the reactor of good seal, after insulation 30min, 800 DEG C are warming up to heating rate 13 DEG C/min, insulation 30min, is then warming up to 1200 DEG C with heating rate 5 DEG C/min, insulation 10min;
(5) cooling procedure is as follows: charging reactor monolith directly taken out from heater, carries out room temperature cooling;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 98%.
Embodiment 3
(1) first, by 5N cadmium and 5N tellurium by 1: 1.15 quality load reactor than weighing 600g and obtain cadmium tellurium mixture;
(2) be that 200mg/kg adds 4.5N caddy in above-mentioned reactor according to the mass ratio of caddy and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-3pa also seals;
(4) heating process is as follows: when heater is warming up to 300 DEG C, put into by the reactor of good seal, after insulation 30min, 800 DEG C are warming up to heating rate 12 DEG C/min, insulation 30min, is then warming up to 1200 DEG C with heating rate 5 DEG C/min, insulation 13min;
(5) cooling procedure is as follows: taken out from above-mentioned heater by reactor with the speed of 20mm/h, carries out room temperature cooling;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 96.7%.
Embodiment 4
(1) first, by 5N cadmium and 5N tellurium by 1: 1.15 quality load reactor than weighing 550g and obtain cadmium tellurium mixture;
(2) be that 15mg/kg adds 4.5N caddy in above-mentioned reactor according to the mass ratio of caddy and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-5pa also seals;
(4) heating process is as follows: when heater is warming up to 100 DEG C, put into by the reactor of good seal, after insulation 20min, 700 DEG C are warming up to heating rate 15 DEG C/min, insulation 15min, is then warming up to 1092 DEG C with heating rate 3 DEG C/min, insulation 18min;
(5) cooling procedure is as follows: cooling procedure is, after the temperature of charging reactor is down to 1080 DEG C of insulation 10min with the cooldown rate of 0.1 DEG C/min, is directly taken out by this reactor, carry out room temperature cooling from above-mentioned heater;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 97.4%.
Embodiment 5
(1) first, by 5N cadmium and 5N tellurium by 1: 1.12 quality load reactor than weighing 620g and obtain cadmium tellurium mixture;
(2) be that 0.01mg/kg adds 5N caddy in above-mentioned reactor according to the mass ratio of caddy and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-5pa also seals;
(4) heating process is as follows: when heater is warming up to 100 DEG C, put into by the reactor of good seal, after insulation 20min, 900 DEG C are warming up to heating rate 15 DEG C/min, insulation 8min, is then warming up to 1092 DEG C with heating rate 1 DEG C/min, insulation 18min;
(5) cooling procedure is as follows: cooling procedure is, after the temperature of charging reactor is down to 950 DEG C of insulation 180min with the cooldown rate of 5 DEG C/min, is directly taken out by this reactor, carry out room temperature cooling from above-mentioned heater;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 98.2%.
Embodiment 6
(1) first, by 5N cadmium and 5N tellurium by 1: 1 quality load reactor than weighing 600g and obtain cadmium tellurium mixture;
(2) be that 25mg/kg adds 5N caddy in above-mentioned reactor according to the mass ratio of caddy and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-3pa also seals;
(4) heating process is as follows: when heater is warming up to 250 DEG C, put into by the reactor of good seal, after insulation 10min, 900 DEG C are warming up to heating rate 12 DEG C/min, insulation 8min, is then warming up to 1100 DEG C with heating rate 4 DEG C/min, insulation 12min;
(5) cooling procedure is as follows: cooling procedure is, after the temperature of charging reactor is down to 900 DEG C of insulation 360min with the cooldown rate of 20 DEG C/min, is directly taken out by this reactor, carry out room temperature cooling from above-mentioned heater;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 97.8%.
Embodiment 7
(1) first, by 5N cadmium and 5N tellurium by 1: 1.12 quality load reactor than weighing 650g and obtain cadmium tellurium mixture;
(2) be that 15mg/kg adds 4.5N caddy in above-mentioned reactor according to the mass ratio of caddy and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-4pa also seals;
(4) heating process is as follows: when heater is warming up to 300 DEG C, put into by the reactor of good seal, after insulation 15min, 850 DEG C are warming up to heating rate 12 DEG C/min, insulation 20min, is then warming up to 1200 DEG C with heating rate 2 DEG C/min, insulation 15min;
(5) cooling procedure is as follows: charging reactor monolith directly fallen from heater, carries out room temperature cooling;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 96.1%.
Embodiment 8
(1) first, by 5N cadmium and 5N tellurium by 1: 1 quality load reactor than weighing 600g and obtain cadmium tellurium mixture;
(2) be that 25mg/kg adds 4N cadmium fluoride in above-mentioned reactor according to the mass ratio of cadmium fluoride and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-3pa also seals;
(4) heating process is as follows: when heater is warming up to 250 DEG C, put into by the reactor of good seal, after insulation 10min, 900 DEG C are warming up to heating rate 12 DEG C/min, insulation 8min, is then warming up to 1150 DEG C with heating rate 4 DEG C/min, insulation 12min;
(5) cooling procedure is as follows: charging reactor monolith directly fallen from heater, carries out room temperature cooling;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 97.4%.
Embodiment 9
(1) first, by 5N cadmium and 5N tellurium by 1: 1 quality load reactor than weighing 600g and obtain cadmium tellurium mixture;
(2) be that 25mg/kg adds 4N cadmium bromide in above-mentioned reactor according to the mass ratio of cadmium bromide and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-3pa also seals;
(4) heating process is as follows: when heater is warming up to 250 DEG C, put into by the reactor of good seal, after insulation 10min, 900 DEG C are warming up to heating rate 12 DEG C/min, insulation 8min, is then warming up to 1100 DEG C with heating rate 4 DEG C/min, insulation 12min;
(5) cooling procedure is as follows: taken out from above-mentioned heater by reactor with the speed of 15mm/h, carries out room temperature cooling;
(6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 97.6%.
Embodiment 10
(1) first, by 5N cadmium and 5N tellurium by 1: 1 quality load reactor than weighing 600g and obtain cadmium tellurium mixture;
(2) be that 25mg/kg adds 4N cadmium iodide in above-mentioned reactor according to the mass ratio of cadmium iodide and cadmium tellurium mixture;
(3) reactor after above-mentioned charging is vacuumized, make its vacuum degree to 10
-3pa also seals;
(4) heating process is as follows: when heater is warming up to 250 DEG C, put into by the reactor of good seal, after insulation 10min, 900 DEG C are warming up to heating rate 12 DEG C/min, insulation 8min, is then warming up to 1100 DEG C with heating rate 4 DEG C/min, insulation 12min;
(5) cooling procedure is as follows: charging reactor monolith directly fallen from heater, carries out room temperature cooling; (6) take out sample from reactor, the Synthesis conversion obtaining sample after weighing reaches 97.3%.
In embodiment 1-10, from Synthesis conversion, high according to preparation method's synthetic ratio of halogen doping cadmium telluride of the present invention.
3rd, provide the test result of the embodiment of the preparation method of halogen doping cadmium telluride.
In order to the effect of the preparation method to halogen doping cadmium telluride of the present invention is verified, with the portioned product in above-mentioned 10 embodiments for sample carries out relative substance content analysis.
Table 1 is outer other impurity contents (unit mg/kg) of dechlorination of the halogen doping cadmium telluride that the section Example in above-described embodiment obtains.From data, the compound purity obtained is high, and impurity content is low.
Table 2 is chlorine in the halogen doping cadmium telluride that obtains of embodiment 7 and the tellurium content at diverse location, and wherein, the halogen doping cadmium telluride obtained is column.From analysis result, chlorine and tellurium element are evenly distributed in compound, composition and stoicheiometry close, namely has succeeded well at complete the doping of chlorine element.The impurity content (dechlorination is outer) (unit mg/kg) of the halogen doping cadmium telluride that table 1 section Example obtains
Chlorine in the halogen doping cadmium telluride that table 2 embodiment 7 obtains and tellurium are at the content of diverse location
| Upside | Downside | Side | |
| Chlorinity (mg/kg) | 16.7 | 14.8 | 15.3 |
| Tellurium content (wt%) | 53.18 | 53.12 | 53.16 |
4th, the beneficial effect of the preparation method of halogen doping cadmium telluride of the present invention.
Compared with prior art CN1623014A, the preparation method of halogen doping cadmium telluride of the present invention does not use PBN crucible and high-tension apparatus, greatly reduces equipment requirement; Do not use nitrogen, do not need to regulate reaction vessel external pressure, simple to operate, fail safe is high, cost-saving; Heating process easily controls, sufficient reacting, and aggregate velocity is fast; Can adulterate as required, the content of halogen, close to stoicheiometry, does not have tellurium sedimentary facies.
Compared with prior art CN102142481A, the preparation method of halogen doping cadmium telluride of the present invention adopts solid-state reactants, avoids in the raw material preparation of liquid state and gaseous reactant, transport, operating process and is difficult to control, to the requirement high problem of equipment; In the sample obtained, chlorine is evenly distributed, and output is high, and course of reaction easily controls, and reactions steps is comparatively simple, and handling safety, is conducive to the advantages such as suitability for industrialized production.
The preparation method of second aspect-halogen doping cadmium telluride diaphragm solar battery
The first, with reference to Fig. 2 and Fig. 3, the preparation method according to halogen doping cadmium telluride diaphragm solar battery of the present invention is described.
Preparation method according to halogen doping cadmium telluride diaphragm solar battery of the present invention comprises step: at SnO
2: F glass is (by glassy layer 11 and SnO
2: F layer 12 is formed) upper deposited n-type CdS layer 13 (step S10); N-type CdS layer 13 deposits P type halogen doping cadmium-telluride layer 14 (step S20), and the halogen doping cadmium telluride wherein in P type halogen doping cadmium-telluride layer 14 obtains according to the preparation method of the halogen doping cadmium telluride of the above-mentioned first aspect of the present invention; Utilize evaporation source ZnTe and evaporation source Cu to deposit on P type halogen doping cadmium-telluride layer 14 and form back contact 15 (step S30); And on back contact 15, deposit back electrode layer 16 (step S40).
In step slo, at SnO
2: F deposition on glass N-type CdS layer 24 can adopt chemical bath deposition method.
In step slo, preferably, the thickness of N-type CdS layer 13 is 0.1 ~ 0.5 μm.
In step S20, N-type CdS layer 13 deposits P type halogen doping cadmium-telluride layer 14 can adopt argon oxygen atmosphere under close spaced sublimation method.
In step S20, preferably, the thickness of P type halogen doping cadmium-telluride layer 14 is 2 ~ 5 μm.
In step s 30, described utilize evaporation source ZnTe and evaporation source Cu deposit on P type halogen doping cadmium-telluride layer 14 formed back contact 15 can comprise step: under certain vacuum degree, first, independent heating evaporation source ZnTe, obtains unadulterated ZnTe layer 151 to utilize the independent hydatogenesis of evaporation source ZnTe; Then heat the described evaporation source ZnTe that separated by dividing plate and described evaporation source Cu and carry out Co-evaporated Deposition and obtain ZnTe:Cu layer 152 secondly; Then, anneal under regulation annealing temperature in the atmosphere of protective gas.Preferably, described protective gas is selected from nitrogen, one of helium and argon gas, and described regulation annealing temperature is 100 ~ 300 DEG C, and described certain vacuum degree is 1 × 10
-5pa.
In step s 30, preferably, back contact 151 comprises ZnTe layer 151 and ZnTe:Cu layer 152.The thickness of ZnTe layer 151 is 10 ~ 20nm; The thickness of ZnTe:Cu layer 152 is that in 30 ~ 50nm, ZnTe:Cu layer 152, Cu atomic concentration is 3 ~ 15%.
In step s 40, back electrode layer 16 can adopt electron beam evaporation nickel to obtain.
In step s 40, preferably, the thickness of back electrode layer 16 is 100 ~ 300nm.
The second, the embodiment of the preparation method according to halogen doping cadmium telluride diaphragm solar battery of the present invention is described.Wherein for the sake of clarity, the numbering of embodiment continues the embodiment numbering of above-mentioned first aspect.
Embodiment 11
First, adopt chemical bath deposition method at SnO
2: F glass is (by glassy layer 11 and SnO
2: F layer 12 is formed) go up the thick N-type CdS layer 13 of deposition about 0.1 μm;
Secondly, under argon oxygen atmosphere, on N-type CdS layer 13, about 3 μm of thick P type halogen doping cadmium-telluride layers 14 (deposition process P used type halogen doping cadmium telluride uses the preparation method of above-mentioned first aspect to obtain) are deposited by close spaced sublimation method;
Then on P type halogen doping cadmium-telluride layer 14, back contact 15 is deposited by method of evaporating, the ZnTe:Cu layer 152 that the Co-evaporated Deposition that back contact comprises the unadulterated ZnTe layer 151 of one deck and ZnTe evaporation source and the Cu evaporation source obtained by the independent hydatogenesis of ZnTe evaporation source obtains, when depositing this two films, vacuum degree is 1 × 10
-5pa, heats two evaporation source ZnTe and Cu separated by dividing plate respectively in deposition process.The thickness of ZnTe layer 151 and ZnTe:Cu layer 152 is about 20nm, 35nm respectively, and wherein in ZnTe:Cu layer 152, Cu atomic concentration is 8%.
Co-evaporated Deposition obtains ZnTe:Cu layer 152 afterwards at N
2naturally cool after protecting lower 150 DEG C of annealing;
Finally, on back contact 15, obtained the back electrode layer 16 of battery by deposited by electron beam evaporation nickel, this layer thickness is about 100nm.
The main purpose of formation back contact 15 and back electrode layer 16 is the contact berrier in order to reduce CdTe and metal electrode (referring to Ni), and extracted current, makes metal electrode and CdTe form ohmic contact.
Obtain the solar cell with P type halogen doping cadmium-telluride layer like this.
Embodiment 12
First, adopt chemical bath deposition method at SnO
2: F glass is (by glassy layer 11 and SnO
2: F layer 12 is formed) go up the thick N-type CdS layer 13 of deposition about 0.2 μm;
Secondly, under argon oxygen atmosphere, on N-type CdS layer 13, about 2 μm of thick P type halogen doping cadmium-telluride layers 14 (deposition process P used type halogen doping cadmium telluride uses the preparation method of above-mentioned first aspect to obtain) are deposited by close spaced sublimation method;
Then on P type halogen doping cadmium-telluride layer 14, back contact 15 is deposited by method of evaporating, the ZnTe:Cu layer 152 that the Co-evaporated Deposition that back contact 15 comprises the unadulterated ZnTe layer 151 of one deck and ZnTe evaporation source and the Cu evaporation source obtained by the independent hydatogenesis of ZnTe evaporation source obtains, when depositing this two films, vacuum degree is 1 × 10
-5pa, heats two evaporation source ZnTe and Cu separated by dividing plate respectively in deposition process.The thickness of ZnTe layer 151 and ZnTe:Cu layer 152 is about 25nm, 45nm respectively, and wherein in ZnTe:Cu layer 152, Cu atomic concentration is 10%.
Co-evaporated Deposition obtains ZnTe:Cu layer 152 afterwards at N
2naturally cool after protecting lower 300 DEG C of annealing;
Finally, on back contact 15, obtained the back electrode layer 16 of battery by deposited by electron beam evaporation nickel, this layer thickness is about 250nm.
Obtain the solar cell with P type halogen doping cadmium-telluride layer like this.
Embodiment 13
First, adopt chemical bath deposition method at SnO
2: F glass is (by glassy layer 11 and SnO
2: F layer 12 is formed) go up the thick N-type CdS layer 13 of deposition about 0.5 μm;
Secondly, under argon oxygen atmosphere, on N-type CdS layer 13, about 4 μm of thick P type halogen doping cadmium-telluride layers 14 (deposition process P used type halogen doping cadmium telluride uses the preparation method of above-mentioned first aspect to obtain) are deposited by close spaced sublimation method;
Then on P type halogen doping cadmium-telluride layer 14, back contact 15 is deposited by method of evaporating, the ZnTe:Cu layer 152 that the Co-evaporated Deposition that back contact 15 comprises the unadulterated ZnTe layer 151 of one deck and ZnTe evaporation source and the Cu evaporation source obtained by the independent hydatogenesis of ZnTe evaporation source obtains, when depositing this two films, vacuum degree is 1 × 10
-5pa, heats two evaporation source ZnTe and Cu separated by dividing plate respectively in deposition process.The thickness of ZnTe layer 151 and ZnTe:Cu layer 152 is about 35nm, 50nm respectively, and wherein in ZnTe:Cu layer 152, Cu atomic concentration is 3%.
Co-evaporated Deposition obtains ZnTe:Cu layer 152 afterwards at N
2naturally cool after protecting lower 100 DEG C of annealing;
Finally, on back contact 15, obtained the back electrode layer 16 of battery by deposited by electron beam evaporation nickel, this layer thickness is about 200nm.
Obtain the solar cell with P type halogen doping cadmium-telluride layer like this.
Embodiment 14
First, adopt chemical bath deposition method at SnO
2: F glass is (by glassy layer 11 and SnO
2: F layer 12 is formed) go up the thick N-type CdS layer 13 of deposition about 0.15 μm;
Secondly, under argon oxygen atmosphere, on N-type CdS layer 13, about 5 μm of thick P type halogen doping cadmium-telluride layers 14 (deposition process P used type halogen doping cadmium telluride uses the preparation method of above-mentioned first aspect to obtain) are deposited by close spaced sublimation method);
Then on P type halogen doping cadmium-telluride layer 14, back contact 15 is deposited by method of evaporating, the ZnTe:Cu layer 152 that the Co-evaporated Deposition that back contact 15 comprises the unadulterated ZnTe layer 151 of one deck and ZnTe evaporation source and the Cu evaporation source obtained by the independent hydatogenesis of ZnTe evaporation source obtains, when depositing this two films, vacuum degree is 1 × 10
-5pa, heats two evaporation source ZnTe and Cu separated by dividing plate respectively in deposition process.The thickness of ZnTe layer 151 and ZnTe:Cu layer 152 is about 50nm, 30nm respectively, and wherein in ZnTe:Cu layer 152, Cu atomic concentration is 15%.
Co-evaporated Deposition obtains ZnTe:Cu layer 152 afterwards at N
2naturally cool after protecting lower 200 DEG C of annealing;
Finally, on back contact 15, obtained the back electrode layer 16 of battery by deposited by electron beam evaporation nickel, this layer thickness is about 300nm.
Obtain the solar cell with P type halogen doping cadmium-telluride layer like this.
In above-described embodiment 11-14, although be all adopt N2 to anneal as protective gas, even if adopt helium, argon gas etc., also can reach same effect.
3rd, the beneficial effect of the preparation method of halogen doping cadmium telluride diaphragm solar battery of the present invention is described.
Compared with prior art, the preparation method of the halogen doping cadmium telluride diaphragm solar battery of the halogen doping cadmium telluride that employing first aspect present invention of the present invention obtains, simplify in existing solar cell technique the halogen that adulterates, the steps such as corrosion and cleaning, decrease operating process and experimental facilities, content of halogen can control as required, for enhancing productivity, reduce the production cycle, reduce production cost, ensure that the purity of material has certain directive significance, can be used for large-scale production, can not to environment and the health endangering operating personnel.
The third aspect-halogen doping cadmium telluride diaphragm solar battery
Illustrate referring to Fig. 3 and the invention still further relates to halogen doping cadmium telluride diaphragm solar battery.
As shown in Figure 3, comprise according to halogen doping cadmium telluride diaphragm solar battery of the present invention: SnO
2: F glassy layer is (by glassy layer 11 and SnO
2: F layer 12 is formed); N-type CdS layer 13, is arranged at described SnO
2: on F glassy layer; P type halogen doping cadmium-telluride layer 14, is arranged on CdS layer 13, and the P type halogen doping cadmium telluride in P type halogen doping cadmium-telluride layer 14 obtains according to the preparation method of the halogen doping cadmium telluride described in first aspect present invention; Back contact 15, is arranged on P type halogen doping cadmium-telluride layer 14; And back electrode layer 16; To be arranged on back contact 15.
According in halogen doping cadmium telluride diaphragm solar battery of the present invention, preferably, the thickness of N-type CdS layer 13 is 0.1 ~ 0.5 μm.
According in halogen doping cadmium telluride diaphragm solar battery of the present invention, preferably, the thickness of P type halogen doping cadmium-telluride layer 14 is 2 ~ 5 μm.
According in halogen doping cadmium telluride diaphragm solar battery of the present invention, preferably, the thickness that back contact 15 comprises ZnTe layer 151 and ZnTe:Cu layer 152, ZnTe layer 151 can be 10 ~ 20nm; The thickness of ZnTe:Cu layer 152 is that in 30 ~ 50nm, ZnTe:Cu layer 152, Cu atomic concentration is 3 ~ 15%.
According in halogen doping cadmium telluride diaphragm solar battery of the present invention, preferably, the thickness of back electrode layer 16 is 100 ~ 300nm.
Although describe preparation method of the present invention and embodiment herein, the present invention is not limited to given embodiment.When not departing from the spirit and scope of claim of enclosing, those skilled in the art can visualize various amendment, modification and substitute, these change, modification and substitute all fall in the scope of claim of the present invention.
Claims (26)
1. a preparation method for halogen doping cadmium telluride, is characterized in that, the preparation method of described halogen doping cadmium telluride comprises step:
Load in reactor according to the first definite quality than weighing by 5N cadmium and 5N tellurium, to obtain cadmium tellurium mixture, described first definite quality is than being mass ratio between described 5N cadmium and described 5N tellurium;
In described reactor according to the second definite quality than the halogenation cadmium adding 4N or more, described second definite quality is than being mass ratio between described halogenation cadmium and described cadmium tellurium mixture;
Described reactor is carried out being evacuated to specified vacuum degree and sealing;
The described reactor of sealing is put into a heater, carries out hyperthermic treatment; And
Cooling processing is carried out to the described reactor of the sealing after hyperthermic treatment;
Before the described reactor of sealing is put into heater, described heater is warming up to the first set point of temperature, and described first set point of temperature is below the fusing point of described cadmium;
Described hyperthermic treatment comprises step:
After the described reactor of sealing is put into described heater, under described first set point of temperature, be incubated for the first stipulated time;
Afterwards, be warming up to the second set point of temperature with the first heating rate, be incubated for the second stipulated time, described second set point of temperature is more than the fusing point of described tellurium; And
Afterwards, be warming up to the 3rd set point of temperature with the second heating rate, the 3rd stipulated time of insulation, wherein said second heating rate is lower than described first heating rate, and described 3rd set point of temperature is more than the fusing point of described halogenation cadmium;
Described first set point of temperature is 100 ~ 300 DEG C, and described first stipulated time is 10 ~ 30min;
Described first heating rate is 12 ~ 15 DEG C/min, and described second set point of temperature is 700 ~ 900 DEG C, and described second stipulated time is 8 ~ 30min;
Described second heating rate is 1 ~ 5 DEG C/min, and described 3rd set point of temperature is 1092 ~ 1200 DEG C, and described 3rd stipulated time is 10 ~ 18min.
2. the preparation method of halogen doping cadmium telluride as claimed in claim 1, it is characterized in that, described first definite quality ratio is 1:1 ~ 1.15.
3. the preparation method of halogen doping cadmium telluride as claimed in claim 1, it is characterized in that, described reactor is quartz ampoule.
4. the preparation method of halogen doping cadmium telluride as claimed in claim 1, it is characterized in that, described second definite quality ratio is 0.01 ~ 200mg/kg.
5. the preparation method of halogen doping cadmium telluride as claimed in claim 1, it is characterized in that, described halogenation cadmium is selected from any one in cadmium fluoride, caddy, cadmium bromide and cadmium iodide.
6. the preparation method of halogen doping cadmium telluride as claimed in claim 1, it is characterized in that, described specified vacuum degree is 10
-2~ 10
-5pa.
7. the preparation method of halogen doping cadmium telluride as claimed in claim 1, it is characterized in that, described cooling processing is: described reactor monolith directly taken out in described heater, makes described reactor carry out room temperature cooling.
8. the preparation method of halogen doping cadmium telluride as claimed in claim 1, it is characterized in that, described cooling processing is: the temperature of described reactor is down to predetermined temperature with predetermined cool down rate, the insulation scheduled time; Afterwards described reactor is directly taken out in described heater, make described reactor carry out room temperature cooling.
9. the preparation method of halogen doping cadmium telluride as claimed in claim 8, it is characterized in that, described predetermined cool down rate is 0.1 ~ 20 DEG C/min, and described predetermined temperature is 900 ~ 1080 DEG C, and the described scheduled time is 10 ~ 360min.
10. the preparation method of halogen doping cadmium telluride as claimed in claim 1, it is characterized in that, described cooling processing is: to specify that described reactor takes out by movement velocity in described heater, make described reactor carry out room temperature cooling.
The preparation method of 11. halogen doping cadmium tellurides as claimed in claim 10, it is characterized in that, described regulation movement velocity is 1 ~ 20mm/h.
The preparation method of 12. 1 kinds of halogen doping cadmium telluride diaphragm solar batteries, is characterized in that, comprises step:
At SnO
2: F deposition on glass N-type CdS layer;
Described N-type CdS layer deposits P type halogen doping cadmium-telluride layer, and the halogen doping cadmium telluride in wherein said P type halogen doping cadmium-telluride layer obtains according to the preparation method of the halogen doping cadmium telluride according to any one of claim 1 ~ 11;
Utilize evaporation source ZnTe and evaporation source Cu to deposit on described P type halogen doping cadmium-telluride layer and form back contact; And
Described back contact deposits back electrode layer.
The preparation method of 13. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 12, is characterized in that, at SnO
2: F deposition on glass N-type CdS layer adopts chemical bath deposition method.
The preparation method of 14. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 12, is characterized in that, the thickness of described N-type CdS layer is 0.1 ~ 0.5 μm.
The preparation method of 15. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 12, is characterized in that, described N-type CdS layer deposits the close spaced sublimation method under P type halogen doping cadmium-telluride layer employing argon oxygen atmosphere.
The preparation method of 16. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 12, is characterized in that, the thickness of described P type halogen doping cadmium-telluride layer is 2 ~ 5 μm.
The preparation method of 17. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 12, is characterized in that, described utilize evaporation source ZnTe and evaporation source Cu deposit on P type halogen doping cadmium-telluride layer formed back contact comprise step:
Under certain vacuum degree, first, independent heating evaporation source ZnTe, obtains unadulterated ZnTe layer to utilize the independent hydatogenesis of evaporation source ZnTe;
Then heat the described evaporation source ZnTe that separated by dividing plate and described evaporation source Cu and carry out Co-evaporated Deposition and obtain ZnTe:Cu layer secondly;
Then, anneal under regulation annealing temperature in the atmosphere of protective gas.
The preparation method of 18. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 17, it is characterized in that, described protective gas is selected from nitrogen, one of helium and argon gas, and described regulation annealing temperature is 100 ~ 300 DEG C, and described certain vacuum degree is 1 × 10
-5pa.
The preparation method of 19. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 12, it is characterized in that, described back contact comprises ZnTe layer and ZnTe:Cu layer, and the thickness of described ZnTe layer is 10 ~ 20nm; The thickness of described ZnTe:Cu layer is 30 ~ 50nm, and in described ZnTe:Cu layer, Cu atomic concentration is 3 ~ 15%.
The preparation method of 20. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 12, is characterized in that, described back electrode layer adopts electron beam evaporation nickel to obtain.
The preparation method of 21. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 12, is characterized in that, the thickness of described back electrode layer is 100 ~ 300nm.
22. 1 kinds of halogen doping cadmium telluride diaphragm solar batteries, comprising:
SnO
2: F glassy layer;
N-type CdS layer, is arranged at described SnO
2: on F glassy layer;
Back contact;
Back electrode layer; Be arranged on described back contact;
It is characterized in that, described halogen doping cadmium telluride diaphragm solar battery also comprises:
P type halogen doping cadmium-telluride layer, be arranged on described CdS layer, back contact is arranged on described P type halogen doping cadmium-telluride layer, and the P type halogen doping cadmium telluride in described P type halogen doping cadmium-telluride layer obtains according to the preparation method of the halogen doping cadmium telluride according to any one of claim 1 ~ 11.
23. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 22, is characterized in that, the thickness of described N-type CdS layer is 0.1 ~ 0.5 μm.
24. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 22, is characterized in that, the thickness of described P type halogen doping cadmium-telluride layer is 2 ~ 5 μm.
25. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 22, it is characterized in that, described back contact comprises ZnTe layer and ZnTe:Cu layer, and the thickness of described ZnTe layer is 10 ~ 20nm; The thickness of described ZnTe:Cu layer is 30 ~ 50nm, and in described ZnTe:Cu layer, Cu atomic concentration is 3 ~ 15%.
26. halogen doping cadmium telluride diaphragm solar batteries as claimed in claim 22, is characterized in that, the thickness of described back electrode layer is 100 ~ 300nm.
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| CN101978101A (en) * | 2008-03-18 | 2011-02-16 | 索莱克山特公司 | Improved back contact in thin solar cells |
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