CN110165020A - One kind being based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Hull cell and preparation method thereof - Google Patents

One kind being based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Hull cell and preparation method thereof Download PDF

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CN110165020A
CN110165020A CN201910457215.9A CN201910457215A CN110165020A CN 110165020 A CN110165020 A CN 110165020A CN 201910457215 A CN201910457215 A CN 201910457215A CN 110165020 A CN110165020 A CN 110165020A
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丁建宁
陈志文
袁宁一
郭华飞
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Changzhou University
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Abstract

The invention belongs to solar cell preparation fields, and in particular to one kind is based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Hull cell and preparation method thereof, it is of the invention based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Hull cell is by using CdS/SnO2N-type layer is mixed to replace single SnO2Buffer layer passes through the Sb of both comparisons2Se3XRD spectrum can significantly find, use SnO2When as N-type layer, (120) are Sb2Se3Preferred orientation, and using mixing N-type layer can make Sb2Se3The orientation of (120) crystal face be preferably minimized, and (221) is made to become preferred orientation, is more conducive to the transmission of electronics, and since the presence of CdS film can not only induce Sb2Se3The columnar growth of film can also improve its crystallinity to improve its battery efficiency.

Description

One kind being based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Hull cell and its preparation Method
Technical field
The invention belongs to solar cell preparation fields, and in particular to one kind is based on CdS/SnO2Mix the efficient of N-type layer Sb2Se3Hull cell and preparation method thereof.
Background technique
In recent years, gradually exhausting with non-renewable resources such as oil and coal limited on the earth, renewable energy Utilization with exploitation seem more and more urgent, wherein solar energy power generating is by the inexhaustible sun being radiated on ground Electric energy can be continuously transformed by the photoelectric conversion of the photovoltaic devices such as solar cell, have become renewable energy In most safe, most environmentally friendly and most potential competitor.
So far, common solar cell mainly includes silion cell, hull cell etc., is mainly divided in hull cell For perovskite, CIGS and CZTS etc., however perovskite battery has an environment unstability, CIGS higher cost, Sn in CZTS Fusing point is lower, during the preparation process and its is easy to scatter and disappear, it is difficult to prepare.And Sb2Se3As a kind of binary semiconductor material, due to Its excellent photoelectric properties, such as: band gap (1.1eV) appropriate, absorption coefficient big (> 105cm-1), high carrier mobility (10cm2V-1s-1Refer to minority carrier) and long carrier lifetime (60ns based on transient absorption spectra), there is great steam Pressure (1,200 550 DEG C of Pa@) etc. make many research institutions both domestic and external to antimony selenide hull cell expand deeper into grind Study carefully.
But up to the present, most of antimony selenide hull cell is based on toxic CdS film as buffer layer, one Aspect CdS is because its smaller band gap (about 2.4eV) can absorb most incident light, on the other hand due to the expansion of Cd element The unstability that may result in device is dissipated, therefore we select a kind of environmentally friendly buffer layer SnO2It is toxic to replace CdS film, because it has broad-band gap (3.6eV) and high n-type doping concentration (1019To 1020cm-3).Another aspect SnO2It is wide General use also indicates that its stable chemical property, and non-toxic, big band gap and high stability make SnO2CdS can be replaced as buffering Layer.In addition, SnO2Similitude between the transparency conducting layer of FTO will generate less lattice mismatch, so as to cause better Electron-transport.But simple use SnO2It goes that CdS is replaced to still have several drawbacks place, because of SnO2The lower crystallinity of film With biggish surface roughness with Sb2Se3Film can introduce the compound of more boundary defects and electronics when forming P-N junction, and And Sb2Se3The orientation of growth of film is bad, relatively low so as to cause efficiency.
Summary of the invention
In order to further increase Sb2Se3The efficiency of hull cell, the present invention provides one kind to be based on CdS/SnO2Mix N-type The efficient Sb of layer2Se3Hull cell and preparation method thereof.
The present inventor, which suspects, influences SnO2/Sb2Se3The principal element of the final efficiency of solar cell is film surface Roughness and crystallinity, still, pass through low temperature solution polycondensation prepare SnO2Film has good superficiality and crystallinity, institute Guess that the main reason for efficiency is lower than other buffer layers is due to Sb with us2Se3Caused by the orientation of growth of film.For this purpose, this Inventive method is in SnO2One layer of ultra-thin CdS is added under film to wish to change Sb2Se3The growth pattern of film.To improve Its battery efficiency.
It is according to the present invention a kind of based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3The preparation method of hull cell Implement according to the following steps:
(1) FTO glass is used foam water, acetone, ethyl alcohol, deionized water difference ultrasound by the cleaning of FTO substrate glasses respectively Cleaning 30 minutes, and with being dried with nitrogen.
(2) preparation of CdS film, by 15~20mL CdSO4Solution (15mmol/L), (concentration is 19~35mL ammonium hydroxide 25%~28% industrial ammonia), 15~20mL thiourea solution (75mmol/L) is successively poured into equipped with 250mL deionized water Mixed solution is obtained in beaker, and cleaned FTO glass is clamped with clip and is put into wherein, and agitating solution, the reaction time For 8~20min, reaction temperature is 65~80 DEG C, obtains the CdS film with a thickness of 10-40nm.
(3)SnO2The CdS film with a thickness of 10-40nm that above-mentioned steps (2) obtain is put into spin coating instrument by the preparation of film In, configured SnO is added dropwise2Aqueous solution is (according to mass ratio SnO2:H2O/1:4) in CdS film, spin coating 1-4 times is revolved every time 30s, revolving speed 5000rpm are applied, 150 DEG C of annealing 30min, obtain the SnO with a thickness of 10-40nm later2Film.
N-type layer generally has optimal thickness, if thickness is excessively thin or the blocked up quality that can all influence p-n junction, with And influence the extraction and transmission of electronics, open the reduction of pressure so as to cause battery, efficiency reduces, therefore, in the present invention CdS film and SnO2The thickness of film is preferably 10-40nm.
SnO2The proportion of aqueous solution will affect SnO2The thickness of film will obtain identical thickness if proportion is too dilute, Will more spin coatings several times, will lead to the increase of interface problem between layers in this way, also result in the difficulty of electron-transport, from And influence battery efficiency.
Spin-coating time and revolving speed also will affect SnO2The thickness of film, to influence the efficiency of battery.
Annealing can be improved SnO2The crystallinity of film, annealing temperature and the time it is inadequate if, crystal grain will not be merged one It rises and becomes larger, many cavities and grain boundary defects will be generated, to influence the transmission of electronics, will lead to film production if excessively high Raw slight crack, also results in the generation of cavity and grain boundary defects, to reduce battery efficiency.
(4)Sb2Se3The preparation of film, the CdS/SnO that above-mentioned steps (3) are obtained2Film is put into quick anneal oven, and The Sb that 0.4-0.6g is produced by Jiangxi Ke Tai company2Se3Powder is put into chamber, in the case where pressure is 0.34Pa, temperature 580 DEG C deposition 110s obtain Sb2Se3Film.
In annealing furnace, pressure when annealing is exactly the vacuum degree of chamber, the Sb if vacuum degree is inadequate2Se3Meeting under high temperature It is oxidized and generates Sb203, temperature is excessively high or too low can all influence Sb2Se3The evaporation rate of film, it is excessively high too low all to cause Sb2Se3Film generates many cavity and defect, and the time is too low excessively high to will affect Sb2Se3The thickness of film, thus cannot get one A good p-n junction, so as to cause the reduction of efficiency.
(5) preparation of gold electrode, the Sb that step (4) is obtained2Se3Film is put into evaporimeter, evaporates one layer of 80nm thickness Gold electrode.
Compared with prior art, the invention has the following advantages: the method for the present invention have it is easy to operate, it is at low cost, The advantages that industrialization level is high.Using this method be prepared based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Thin-film electro Pond is by using CdS/SnO2N-type layer is mixed to replace single SnO2The presence of buffer layer, CdS film can induce Sb2Se3Columnar growth, Sb can be made2Se3The orientation of (120) crystal face be preferably minimized, and make (221) preferred orientation, more Be conducive to the transmission of electronics, and induce selenizing Sb film along columnar growth, further, it is also possible to its crystallinity be improved, to mention High Sb2Se3The battery efficiency of film, for promoting the development of antimony selenide hull cell that there is highly important scientific meaning.
Detailed description of the invention
Fig. 1 is CdS/SnO prepared by the present invention2/Sb2Se3The structural schematic diagram of hull cell.
Fig. 2 is prepared by the present invention based on SnO2, CdS/SnO2, Sb of the CdS as buffer layer2Se3The XRD diagram of film.
Fig. 3 is prepared by the present invention based on SnO2, CdS/SnO2, Sb of the CdS as buffer layer2Se3The SEM of film schemes.
Fig. 4 is prepared by the present invention based on SnO2, CdS/SnO2, Sb of the CdS as buffer layer2Se3The section of hull cell SEM figure.
Fig. 5 is prepared by the present invention based on SnO2, CdS/SnO2, Sb of the CdS as buffer layer2Se3The efficiency of hull cell Figure.
Specific embodiment
The present invention is described in further details below by embodiment, these embodiments are only used to illustrate the present invention, and It does not limit the scope of the invention, the object of the present invention is to provide one kind to be based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Film The preparation method of battery, detailed process is as follows:
CdS film is prepared using immersion method, obtained CdS film is deposited into one layer of SnO using the method for spin coating2Film, Then Sb is prepared using RTE method2Se3Film finally deposits one layer of gold electrode using evaporation technique.
These embodiments are only used to illustrate the present invention, not limit the scope of the invention.
Embodiment 1
The cleaning of FTO substrate glasses
Substrate selects FTO glass, successively uses foam water, acetone, ethyl alcohol, deionized water is cleaned by ultrasonic 30 minutes respectively, dry It is spare after dry.
The preparation of CdS film:
By 15mL CdSO4Solution (15mmol/L), 19mL ammonium hydroxide (industrial ammonia that concentration is 25%~28%), 15mL Thiourea solution (75mmol/L), successively pours into the beaker equipped with 250mL deionized water and obtains mixed solution, will be cleaned FTO glass is clamped with clip to be put into wherein, and agitating solution, reaction time 8min, and reaction temperature is 70 DEG C, obtains thickness For the CdS film of 10nm.
SnO2The preparation of film:
It will be put into spin coating instrument with a thickness of the CdS film of 10nm, configured SnO be added dropwise2Aqueous solution (SnO2:H2O/1:4) In in CdS film, spin coating 4 times, each spin coating 30s, revolving speed 5000rpm, 150 DEG C of annealing 30min, are obtained with a thickness of 40nm later SnO2Film.
Sb2Se3The preparation of film:
1. by the above-mentioned N-type CdS/SnO handled well2Film is put into quick anneal oven, using vacuum pump by chamber pressure It is evacuated to 0.34Pa.
2. furnace temperature is warming up to 300 DEG C with the speed of 10 DEG C/s, 20min is kept, so that substrate and Sb2Se3Source obtains adequately Heating.
3. temperature is then warming up to 580 DEG C with the speed of 10 DEG C/s, keep 110s, then Temperature fall, to 50 DEG C with Lower taking-up, that is, be prepared Sb2Se3Film.
Find that its (120) peak minimizes using XRD powder diffraction analysis, (221) peak becomes preferred orientation.It is sent out using field The surface topography for penetrating scanning electron microscopic observation film finds preparation-obtained Sb2Se3Film is fully crystallized.And pass through section SEM figure is it can be seen that it induces Sb2Se3Film is along columnar growth.
The preparation of Au electrode
In Sb obtained above2Se3Film surface plates the gold electrode that a layer thickness is about 80nm using evaporimeter to get arriving One kind being based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Hull cell, discovery is in CdS film with a thickness of 10nm, SnO2Thickness It is efficiency highest battery performance parameter for 40nm are as follows: open-circuit voltage Voc=0.36V, short-circuit current density Jsc=27.8mA/cm2, Fill factor FF=52.7, battery efficiency PCE=5.27%.
Comparative example 1
The cleaning of FTO substrate glasses:
Substrate selects FTO glass, successively uses foam water, acetone, ethyl alcohol, deionized water is cleaned by ultrasonic 30 minutes respectively, dry It is spare after dry.
SnO2The preparation of film:
The FTO cleaned up is put into spin coating instrument, configured SnO is added dropwise2Aqueous solution (SnO2:H2O/1:4) in FTO On, spin coating 4 times, each spin coating 30s, revolving speed 5000rpm, 150 DEG C of annealing 30min, obtain the SnO with a thickness of 40nm later2It is thin Film.
Sb2Se3The preparation of film:
1. by the above-mentioned N-type SnO handled well2Film is put into quick anneal oven, is evacuated to chamber pressure using vacuum pump 0.34Pa。
2. furnace temperature is warming up to 300 DEG C with the speed of 10 DEG C/s, 20min is kept, so that substrate and Sb2Se3Source obtains adequately Heating.
3. temperature is then warming up to 580 DEG C with the speed of 10 DEG C/s, keep 110s, then Temperature fall, to 50 DEG C with Lower taking-up, that is, be prepared Sb2Se3Film.
Find that its (120) peak is preferred orientation using XRD powder diffraction analysis, (221) peak is relatively low.It is scanned using Flied emission Electronic Speculum observes the surface topography of film, finds preparation-obtained Sb2Se3Film is fully crystallized.And it can by section SEM figure To find out Sb2Se3Film is disorderly arranged.
The preparation of Au electrode
In Sb obtained above2Se3Film surface plates the gold electrode that a layer thickness is about 80nm using evaporimeter to get arriving SnO2Sb as N-type layer2Se3Hull cell, battery performance parameter are as follows: open-circuit voltage Voc=0.32V, short-circuit current density Jsc =18.4mA/cm2, fill factor FF=39.4, battery efficiency PCE=2.33%.
Comparative example 2
The cleaning of FTO substrate glasses:
Substrate selects FTO glass, successively uses foam water, acetone, ethyl alcohol, deionized water is cleaned by ultrasonic 30 minutes respectively, dry It is spare after dry.
The preparation of CdS film:
By CdSO4Solution 15mL, ammonium hydroxide 19mL, thiourea solution 15mL successively pour into the beaker equipped with 250mL deionized water In, cleaned FTO glass is clamped with clip and is put into wherein, and agitating solution, reaction time 20min, reaction temperature It is 70 DEG C, obtains the CdS film with a thickness of 40nm or so.
Sb2Se3The preparation of film:
1. the above-mentioned N-type CdS film handled well is put into quick anneal oven, chamber pressure is evacuated to using vacuum pump 0.34Pa。
2. furnace temperature is warming up to 300 DEG C with the speed of 10 DEG C/s, 20min is kept, so that substrate and Sb2Se3Source obtains adequately Heating.
3. temperature is then warming up to 580 DEG C with the speed of 10 DEG C/s, keep 110s, then Temperature fall, to 50 DEG C with Lower taking-up, that is, be prepared Sb2Se3Film.
It is its preferred orientation using XRD powder diffraction analysis discovery (221) peak.It is thin using field emission microscopy observation The surface topography of film finds preparation-obtained Sb2Se3The crystallinity of film is less than CdS/SnO2Sb as buffer layer2Se3 The crystallinity of film, and there are more cavities.And by section SEM figure it can be seen that it induces Sb2Se3Film is along column Growth.
The preparation of Au electrode
In Sb obtained above2Se3Film surface plates the gold electrode that a layer thickness is about 80nm using evaporimeter to get arriving Sb of the CdS as N-type layer2Se3Hull cell, battery performance parameter are as follows: open-circuit voltage Voc=0.36V, short-circuit current density Jsc =26.2mA/cm2, fill factor FF=52.2, battery efficiency PCE=4.94%.

Claims (6)

1. one kind is based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3The preparation method of hull cell, which is characterized in that described Steps are as follows for preparation method:
(1) method for using chemical bath deposition, prepares one layer of CdS film on FTO substrate；
(2) method for using spin coating, one layer of SnO of spin-on deposition in the CdS film that step (1) obtains2Film；
(3) using the method for quick thermal evaporation, in the CdS/SnO that step (2) obtains2One layer of Sb is deposited on film2Se3Film；
(4) using the method for evaporation, in the Sb that step (3) obtains2Se3One layer of gold electrode is prepared on film.
2. being based on CdS/SnO as described in claim 12Mix the efficient Sb of N-type layer2Se3The preparation method of hull cell, It is characterized in that, the step (1), which sequentially includes the following steps:, successively uses foam water, acetone, ethyl alcohol and deionized water to FTO glass Ultrasonic cleaning prepares the CdS film with a thickness of 10-40nm with immersion method after dry.
3. being based on CdS/SnO as described in claim 12Mix the efficient Sb of N-type layer2Se3The preparation method of hull cell, It is characterized in that, the step (2) sequentially includes the following steps: and is put into a thickness of the CdS film of 10-40nm by step (1) is resulting In spin coating instrument, configured SnO is added dropwise2Aqueous solution is in CdS film, and spin coating 4 times, each spin coating 30s, revolving speed 5000rpm, it 150 DEG C of annealing 30min afterwards, obtain the SnO with a thickness of 10-40nm2, wherein SnO2Aqueous solution is according to mass ratio SnO2:H2O=1: 4 prepare.
4. being based on CdS/SnO as described in claim 12Mix the efficient Sb of N-type layer2Se3The preparation method of hull cell, It is characterized in that, the step (3) sequentially includes the following steps: the CdS/SnO for obtaining step (2)2Film is put into quick anneal oven In, it is 0.34Pa in pressure, temperature is that deposition 110s obtains Sb at 580 DEG C2Se3Film.
5. being based on CdS/SnO as described in claim 12Mix the efficient Sb of N-type layer2Se3The preparation method of hull cell, It is characterized in that, the Sb that step (3) is obtained2Se3Film is put into evaporimeter, evaporates the gold electrode of one layer of 80nm thickness.
6. a kind of method as described in claim 1 is obtained to be based on CdS/SnO2Mix the efficient Sb of N-type layer2Se3Hull cell, It is characterized in that, the structure of the hull cell is from bottom to top successively are as follows: FTO substrate, CdS layer, SnO2Layer, Sb2Se3Layer, Au.
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CN111560583A (en) * 2020-05-05 2020-08-21 东北电力大学 Induction (Sb)4Se6)nMethod for preparing antimony selenide photoelectric film with longitudinally-grown molecular chain
CN113013286A (en) * 2021-01-27 2021-06-22 西北工业大学深圳研究院 Antimony selenide film with high (hk1) crystal face abundance, antimony selenide film solar cell and preparation method thereof

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