CN103288143A - Synthetic method of forbidden bandwidth-adjustable nanometer chalcopyrite - Google Patents
Synthetic method of forbidden bandwidth-adjustable nanometer chalcopyrite Download PDFInfo
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- CN103288143A CN103288143A CN2013101899509A CN201310189950A CN103288143A CN 103288143 A CN103288143 A CN 103288143A CN 2013101899509 A CN2013101899509 A CN 2013101899509A CN 201310189950 A CN201310189950 A CN 201310189950A CN 103288143 A CN103288143 A CN 103288143A
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Abstract
The invention discloses a synthetic method of forbidden bandwidth-adjustable nanometer chalcopyrite. The synthetic method is characterized by comprising the following steps of: adopting a solvothermal method to continuously react for 24 hours under the constant-temperature condition of 200 DEG C by using copper chloride dehydrate, iron chloride hexahydrate and thiourea as reaction materials, using aluminum chloride anhydrous and selenium powder as doping agent and using distilled water and alcohol as reaction solvent; cooling to the room temperature; respectively washing the centrifugally-separated product for three times by virtue of the distilled water and absolute ethyl alcohol; drying for 12 hours under the condition of 80 DEG C to obtain pure nanometer chalcopyrite and doped chalcopyrite products. The synthetic method of the forbidden bandwidth-adjustable nanometer chalcopyrite is reasonable in design and simple in process. Moreover, the forbidden bandwidth of the obtained product is adjustable within a range of 1.2 eV to 2.2eV.
Description
Technical field
The invention belongs to the synthetic technical field of natural mineral, relate in particular to the preparation method of the adjustable nanometer chalcopyrite of energy gap.
Background technology
I-III-VI
2Ternary compound chalcopyrite (CuFeS
2) be a kind of important semiconductor functional material, it has narrow energy gap (0.6 eV) and high Ne﹠1﹠el temperature (550 ℃), performance such as its unique light, electricity, magnetic and have at the numerous areas of modern society is used widely in addition, for example aspects such as sensor, phototube, solar cell, catalyzer, thereby CuFeS
2Become the indispensable functional materials that a class is generally acknowledged.The foreign matter content of naturally occurring chalcopyrite is higher, and the extraction of pure substance is difficulty comparatively, so the synthetic technology becomes one of approach that obtains pure chalcopyrite, and synthetic has also been obtained certain success (CN102603008A) simultaneously.We know that along with the growing interest to lack of energy and environmental protection problem, seeking renewable energy source cheap, cleaning becomes problem demanding prompt solution.In various renewable energy sources, the selection that sun power is best beyond doubt.The II-VI family more with present research compares I-III-VI with IV-VI family is nanocrystalline
2Family's semiconductor nano does not contain heavy metal elements such as cadmium and lead, has characteristics such as toxicity is little, photoabsorption coefficient is big, band gap is narrow, therefore is expected to become low-cost solar battery material of new generation.The energy gap of desirable solar cell material is 1.4~1.5 eV, and the energy gap of chalcopyrite is less relatively, has therefore limited it in the performance of aspect performances such as photoelectricity.In recent years, have a lot of researchists to be engaged in being with the work of cutting out and having obtained good progress of semiconductor material, along with being with the increasingly mature of the work of cutting out, we wish to find and CuFeS
2Crystalline structure is identical, and lattice parameter is close, and the material that energy gap is different is in order to widen CuFeS
2Range of application.Be both the CuAlS of yellow copper structure
2And CuFeSe
2Energy gap be respectively 3.5 eV and 0.16 eV, therefore utilize Al and Se element that chalcopyrite is mixed respectively, part replaces CuFeS respectively
2In Al atom and S atom, thereby change the band gap of chalcopyrite, make its energy gap between 0.16~3.5 eV, change adjustable and crystalline structure chalcopyrite self remains unchanged, thereby improved CuFeS
2The optical property of semiconductor material and electrical property are widened the Application Areas of chalcopyrite material.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of employing solvent-thermal method, by doped with Al and Se element, prepare the artificial synthesis of the adjustable nanometer chalcopyrite of energy gap, to overcome the synthetic too small and nonadjustable defective of chalcopyrite material energy gap of prior art.
The synthetic method of a kind of energy gap of the present invention is adjustable nanometer chalcopyrite, it is characterized in that, take by weighing 0.5114~0.6819 g copper chloride dihydrate, 0.1351~1.0812 g Iron trichloride hexahydrates, 0.6394~0.9134 g thiocarbamide, 0.0666~0.3333 g Aluminum chloride anhydrous and 0.2842~0.0474 g selenium powder join respectively in the beaker that contains 15 mL dehydrated alcohols, ultrasound procedure mixed it in 3 minutes, continued ultrasonic 6 minutes to wherein adding 15 mL distilled water again, then the solution that mixes is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to room temperature afterwards, centrifugation goes out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtains nano-scale yellow copper and doping chalcopyrite product.
The product thing uses X-ray powder diffraction (XRD) to test mutually, and the instrument model is Bruker D8 Focus type x-ray diffractometer, and X-ray source is Cu-K α radiation (λ=1.5418), and scanning angle scope 2 θ are between 20o~70o.The energy gap size of product adopts ultraviolet-visible diffuse-reflectance instrument to measure, and carries out on the UV-3101 ultraviolet spectrophotometer of instrument model for day island proper Tianjin company, and the test wavelength region is 200~1200 nm.
Fig. 1 a
0~a
5Be respectively the X-ray powder diffraction spectrogram of embodiment 1~6 final product, Fig. 2 b
1~b
5Be respectively the X-ray powder diffraction spectrogram of embodiment 7~11 final products.From Fig. 1 a
0Adopting thiocarbamide as can be seen is sulphur source gained true yellow copper mine and CuFeS
2Base peak fit like a glove (JCPDS No. 35-0752).Mix after a small amount of Al and the Se element, the crystalline structure of chalcopyrite material still remains unchanged, but when Al and Se element are excessive, also some impurity can occur in the product except chalcopyrite, as Fig. 1 a
4With 2 b
4By Scherrer formula D=K λ/β cos θ, wherein K is the Scherrer constant, and its value is 0.89; D is particle size (nm); β is the diffraction peak peak width at half height; θ is diffraction angle; λ=0.154nm calculates the particle size (as shown in table 1) between 25.3~38.7 nm of product, and the sample that proves gained is nano-scale yellow copper.Above test analysis has confirmed that the finished product that experiment obtains are the successful nanometer chalcopyrites that mix, and the energy gap value size of different embodiment products has nothing in common with each other, and is as shown in table 1.As seen from Table 1, different along with Al and Se element doping amount, the energy gap of chalcopyrite is adjustable in 1.2~2.2 eV scopes, thereby has satisfied the requirement of desirable solar cell material, therefore the application of having widened the chalcopyrite material.
Energy gap and the size of the different embodiment products of table 1
Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 |
Band gap (eV) | 2.0 | 1.8 | 1.7 | 1.7 | 1.6 | 1.5 | 1.2 | 1.3 | 1.5 | 1.5 | 2.2 |
Particle diameter (nm) | 38.7 | 31.2 | 38.6 | 28.0 | 29 | 30.1 | 35.3 | 33.8 | 32.0 | 25.4 | 27.1 |
Description of drawings
Fig. 1 is the XRD figure spectrum of the embodiment of the invention 1~6 product.
Fig. 2 is the XRD figure spectrum of the embodiment of the invention 7~11 products.
Embodiment
Embodiment 1
Taking by weighing 0.6819 g copper chloride dihydrate, 1.0812 g Iron trichloride hexahydrates and 0.9134 g thiocarbamide joins respectively in the beaker that contains 15 mL dehydrated alcohols, ultrasound procedure mixed it in 3 minutes, continued ultrasonic 6 minutes to wherein adding 15 mL distilled water again, then the solution that mixes is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to room temperature afterwards, centrifugation goes out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtains nanometer chalcopyrite a
0, its particle size is 38.7 nm, energy gap is 2.0 eV.
Embodiment 2
Step is with embodiment 1, different is to take by weighing 0.6819 g copper chloride dihydrate, 1.0812 g Iron trichloride hexahydrates, 0.8678 g thiocarbamide and 0.0474 g selenium powder to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Se nanometer chalcopyrite a
1, its particle size is 31.2 nm, energy gap is 1.8 eV.
Embodiment 3
Step is with embodiment 1, different is to take by weighing 0.6819 g copper chloride dihydrate, 1.0812 g Iron trichloride hexahydrates, 0.8221 g thiocarbamide and 0.0948 g selenium powder to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Se nanometer chalcopyrite a
2, its particle size is 38.6 nm, energy gap is 1.7 eV.
Embodiment 4
Step is with embodiment 1, different is to take by weighing 0.6819 g copper chloride dihydrate, 1.0812 g Iron trichloride hexahydrates, 0.7764 g thiocarbamide and 0.1421 g selenium powder to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Se nanometer chalcopyrite a
3, its particle size is 28.0 nm, energy gap is 1.7 eV.
Embodiment 5
Step is with embodiment 1, different is to take by weighing 0.6819 g copper chloride dihydrate, 1.0812 g Iron trichloride hexahydrates, 0.7308 g thiocarbamide and 0.1895 g selenium powder to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Se nanometer chalcopyrite a
4, its particle size is 29.0 nm, energy gap is 1.6 eV.
Embodiment 6
Step is with embodiment 1, different is to take by weighing 0.6819 g copper chloride dihydrate, 1.0812 g Iron trichloride hexahydrates, 0.6394 g thiocarbamide and 0.2842 g selenium powder to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Se nanometer chalcopyrite a
5, its particle size is 30.1 nm, energy gap is 1.5 eV.
Embodiment 7
Step is with embodiment 1, different is to take by weighing 0.5114 g copper chloride dihydrate, 0.6757 g Iron trichloride hexahydrate, 0.6851 g thiocarbamide and 0.0666 g Aluminum chloride anhydrous to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Al nanometer chalcopyrite b
1, its particle size is 35.3 nm, energy gap is 1.2 eV.
Embodiment 8
Step is with embodiment 1, different is to take by weighing 0.5114 g copper chloride dihydrate, 0.5068 g Iron trichloride hexahydrate, 0.6851 g thiocarbamide and 0.2000 g Aluminum chloride anhydrous to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Al nanometer chalcopyrite b
2, its particle size is 33.8 nm, energy gap is 1.3 eV.
Embodiment 9
Step is with embodiment 1, different is to take by weighing 0.5114 g copper chloride dihydrate, 0.4054 g Iron trichloride hexahydrate, 0.6851 g thiocarbamide and 0.1500 g Aluminum chloride anhydrous to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Al nanometer chalcopyrite b
3, its particle size is 32.0 nm, energy gap is 1.5 eV.
Embodiment 10
Step is with embodiment 1, different is to take by weighing 0.5114 g copper chloride dihydrate, 0.3041 g Iron trichloride hexahydrate, 0.6851 g thiocarbamide and 0.2500 g Aluminum chloride anhydrous to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Al nanometer chalcopyrite b
4, its particle size is 25.4 nm, energy gap is 1.5 eV.
Embodiment 11
Step is with embodiment 1, different is to take by weighing 0.5114 g copper chloride dihydrate, 0.1351 g Iron trichloride hexahydrate, 0.6851 g thiocarbamide and 0.3333 g Aluminum chloride anhydrous to join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, sustained reaction is 24 hours under the condition that constant temperature is 200 ℃, be cooled to after the room temperature centrifugation and go out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtain mixing Al nanometer chalcopyrite b
5, its particle size is 27.1 nm, energy gap is 2.2 eV.
Claims (2)
1. the synthetic method of the adjustable nanometer chalcopyrite of energy gap, it is characterized in that 0.5114~0.6819 g copper chloride dihydrate, 0.1351~1.0812 g Iron trichloride hexahydrates, 0.6394~0.9134 g thiocarbamide, 0.0666~0.3333 g Aluminum chloride anhydrous and 0.2842~0.0474 g selenium powder join respectively in the beaker that contains 15 mL dehydrated alcohols, evenly mix to wherein adding under the 15 mL distilled water ultrasound conditions again, then mixing solutions is transferred in the autoclave, reaction is 24 hours under 200 ℃ of constant temperatures, after finishing, reaction treats that the temperature of system is down to room temperature, centrifugation goes out that product is washed 3 times with distilled water and dehydrated alcohol respectively and after under 80 ℃ of conditions dry 12 hours, obtains nanometer chalcopyrite and doping chalcopyrite product.
2. the energy gap of the prepared nanometer chalcopyrite sample of the present invention is adjustable in 1.2~2.2 eV scopes.
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Cited By (5)
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CN107381623A (en) * | 2017-06-22 | 2017-11-24 | 中国科学院上海硅酸盐研究所 | A kind of middle carrying semiconductor material and its preparation method and application |
CN108085746A (en) * | 2017-12-20 | 2018-05-29 | 中国地质科学院地球物理地球化学勘查研究所 | The polymeric method of nano-micrometer sheet chalcopyrite crystallite is prepared under hydrothermal condition |
CN109545981A (en) * | 2018-11-27 | 2019-03-29 | 江苏拓正茂源新能源有限公司 | A kind of organic solar batteries and preparation method thereof |
CN110451574A (en) * | 2019-08-30 | 2019-11-15 | 东北大学 | The synthetic method of chalcopyrite nano-micrometer crystal spheroidal aggravation |
CN110590020A (en) * | 2019-10-17 | 2019-12-20 | 兰州大学 | Method for treating laver processing wastewater |
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CN101468398A (en) * | 2007-12-28 | 2009-07-01 | 财团法人工业技术研究院 | Method for producing nano-scale yellow copper structure powder and polymer thin-film solar cell |
CN102603008A (en) * | 2012-04-09 | 2012-07-25 | 济南大学 | Method for synthesizing nanoscale copper pyrites |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN107381623A (en) * | 2017-06-22 | 2017-11-24 | 中国科学院上海硅酸盐研究所 | A kind of middle carrying semiconductor material and its preparation method and application |
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CN108085746A (en) * | 2017-12-20 | 2018-05-29 | 中国地质科学院地球物理地球化学勘查研究所 | The polymeric method of nano-micrometer sheet chalcopyrite crystallite is prepared under hydrothermal condition |
CN109545981A (en) * | 2018-11-27 | 2019-03-29 | 江苏拓正茂源新能源有限公司 | A kind of organic solar batteries and preparation method thereof |
CN110451574A (en) * | 2019-08-30 | 2019-11-15 | 东北大学 | The synthetic method of chalcopyrite nano-micrometer crystal spheroidal aggravation |
CN110451574B (en) * | 2019-08-30 | 2021-03-26 | 东北大学 | Synthetic method of chalcopyrite nano-micron crystal spherical aggregate |
CN110590020A (en) * | 2019-10-17 | 2019-12-20 | 兰州大学 | Method for treating laver processing wastewater |
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