CN109638102B - Graphene heterojunction solar cell and preparation method thereof - Google Patents
Graphene heterojunction solar cell and preparation method thereof Download PDFInfo
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Abstract
A solar cell structure of a graphene heterojunction comprises a silicon wafer substrate layer, a graphene mixing layer, a ZnO nanorod layer, a plurality of silver colloids and a pair of Ti/Au electrodes; the preparation method comprises a silicon wafer substrate preparation step, a graphene microchip reduction step, a spin-coating mother liquor preparation step, a film preparation step and a ZnO nanorod generation step.
Description
Technical Field
The invention relates to the technical field of graphene batteries, in particular to a graphene heterojunction solar battery and a preparation method thereof.
Background
Solar cells are of great interest because of their excellent performance. Graphene, as a representative of new materials, is very strong in the improvement capability of solar cells, and is a subject of general consideration in new cell materials. The graphene is widely applied to be used as a transparent conductive electrode of an organic solar cell and a dye-sensitized solar cell, and is also combined with a semiconductor to form a Schottky junction photovoltaic device; various solar cells based on silicon nanostructures have also been extensively studied and advanced. The Schottky junction photovoltaic device based on the graphene/silicon nanostructure can fully combine the advantages of the graphene and the silicon nanostructure in the aspect of photovoltaic energy conversion, is low in cost and convenient to realize, and is expected to be an outstanding character in a new-generation solar cell. At present, schottky junction photovoltaic devices based on graphene/silicon nano structures have been reported, but compared with other photovoltaic devices based on silicon nano structures, the energy conversion efficiency of the photovoltaic devices is still insufficient, and the practical application is influenced.
In the prior art, Haixin Chang of hong kong physic university in 2011 finds that a material containing a ZnO nanorod has high responsivity to ultraviolet light and is a relatively good cell structure, and after graphene is found, graphene is used as a good conductor which is easy to process, so that the ZnO nanorod/graphene composite material becomes a relatively realistic solar cell structure choice.
However, in the prior art, no indication and thought are given for how to improve the ultraviolet responsivity of the ZnO nanorod material, and in the prior art, no research and analysis are carried out for how to improve the regularity of the ZnO nanorod and how to improve the conductive property of graphene in the whole material, and how to further improve the photovoltaic performance of the surface of the graphene/ZnO nanorod is needed to be further researched and analyzed.
Disclosure of Invention
The invention aims to provide a graphene/ZnO nanorod solar cell structure to solve the problems of nonuniform performance and insufficient photovoltaic performance of a ZnO nanorod/graphene material in the prior art. The method disclosed by the invention is greatly improved, and tests show that the photovoltaic performance is actually further improved, and the uniformity of the material performance is greatly improved.
In order to achieve the purpose, the invention provides the following technical scheme: a graphene heterojunction solar cell structure, comprising: the device comprises a silicon wafer substrate layer, a graphene mixing layer, a ZnO nanorod layer, a plurality of silver colloids and a pair of Ti/Au electrodes.
The silver glues are respectively coated on two opposite side edges of the silicon chip substrate layer, and a pair of Ti/Au electrodes are oppositely led out from the silver glues on the two opposite side edges; the main body of the graphene mixing layer is a large-radial-size reduced graphene microchip, and ZnO quantum dots are attached to an aggregate of the large-radial-size reduced graphene microchip; the ZnO nanorod layer is located above the graphene mixing layer, and all ZnO nanorods are formed by growing ZnO quantum dots on the upper surface of the graphene mixing layer.
Furthermore, the pair of Ti/Au electrodes are used as terminal electrodes and are in a narrow strip shape with the size similar to that of two opposite side edges of the silicon chip substrate layer, silver colloid is adhered to the outer sides of the pair of Ti/Au electrodes, and a lead is led out from the silver colloid adhered to the outer sides.
The preparation method of the graphene heterojunction solar cell structure is used for preparing the graphene heterojunction solar cell structure, and is characterized by comprising the following steps: 1) a silicon wafer substrate preparation step: polishing to remove an oxide layer of the silicon wafer substrate, loading absolute ethyl alcohol in a spray can, cleaning for multiple times, continuously cleaning with sufficient amount of double distilled water-absolute ethyl alcohol-double distilled water-absolute ethyl alcohol at 35-45 ℃, and airing to obtain a clean silicon wafer substrate.
2) The preparation method of the graphene nanoplatelets comprises the following steps: taking a large number of prefabricated expanded graphite sheets as raw materials, and ultrasonically stripping the raw materials in absolute ethyl alcohol for more than 1-2h to generate graphene microchip dispersion liquid; taking out the upper layer dispersion liquid through low-frequency ultrasound, and keeping the graphite which is not stripped in the container.
The process of abandoning: supplementing the solvent absolute ethyl alcohol of the upper layer dispersion liquid to more than 200-300ml, carrying out high-intensity ultrasonic oscillation for 3-5min, standing for 5-10s, immediately discarding the upper half of the dispersion liquid, and supplementing the absolute ethyl alcohol to the volume of more than 200-300 ml; repeating the winnowing process for at least 10-20 times until the average radial size of the graphene nanoplatelets is higher than 5m as confirmed by AFM or SEM; and (3) evaporating most of the solvent in a spinning mode, and drying at normal temperature under the condition of discontinuously using weak nitrogen for blowing so as to obtain the graphene oxide micro-sheets with large radial sizes.
3) And (3) graphene nanoplatelets reduction: taking a four-mouth bottle with the volume of more than 2L, adding 180 parts by weight of double distilled water, inserting a stirring rod from the first mouth of the four-mouth bottle, stirring at 3-10 r/s, and keeping the temperature to be 35-45 ℃ for continuous stirring; 0.2-0.4 weight part of PVA superfine powder which is subjected to repeated freeze-drying powder grinding until the average particle size is below 60um is slowly added from the second opening of the four-opening bottle; slowly adding 20 parts by weight of graphene oxide micro-sheets with large radial dimension from the second port of the four-port bottle, after all the graphene oxide micro-sheets are added, dissolving 5-10 parts by weight of ascorbic acid with double-distilled water at 35-45 ℃, keeping the solution of ascorbic acid under magnetic stirring at 35-45 ℃, and adding the ascorbic acid solution from the third port of the four-port bottle by using a dropper at the speed of 20-30 drops/min until the addition is finished; stirring for 10-15min, adding dropwise ammonia water from the third port, measuring pH value, and stopping adding ammonia water when pH value is stably higher than 7 and is kept for more than 5 min; and stirring for 10-15min, pouring out the mixture in the four-mouth bottle, removing supernatant, and continuously washing for 6 times by using excess absolute ethyl alcohol, double distilled water, absolute ethyl alcohol and double distilled water at about 40 ℃ to obtain the completely reduced large-radial-size reduced graphene nanoplatelets.
4) The preparation method of the spin coating mother solution comprises the following steps: taking a large beaker, holding 220ml of anhydrous methanol with 180 ml, placing on a magnetic stirring table with a heating function, heating to 35-45 ℃ and keeping, and continuously stirring at the speed of 3-10 r/s by using a polytetrafluoroethylene rotor.
0.05-0.1g of PVA (polyvinyl alcohol) ultrafine powder which is crushed into powder with the average particle size below 60um by freeze-drying for many times is slowly added into a big beaker; weighing 3-5g of ZnO quantum dot powder and 8-10g of reduced graphene micro-sheets, and respectively putting the ZnO quantum dot powder and the reduced graphene micro-sheets into a ZnO quantum dot sieve barrel and a reduced graphene micro-sheet sieve barrel, wherein microporous filter membranes with average pore diameters of 20-40um are arranged on the lower surfaces of the ZnO quantum dot sieve barrel and the reduced graphene micro-sheet sieve barrel; and (3) slowly sieving the two substances into a big beaker by using a ZnO quantum dot sieve barrel and a reduced graphene microchip sieve barrel for about the same time, heating the mixture in the big beaker to 60 ℃ under the continuous stirring at the speed of 3-10 r/s, and slowly evaporating the mixture to about 1/4 volumes to obtain a concentrated dispersion liquid.
5) The preparation method of the film comprises the following steps: placing a clean silicon wafer substrate at the center of the upper surface of a spin coating table, and continuously keeping the concentrated dispersion liquid in an ultrasonic dispersion state; spin coating process: dripping the silicon wafer substrate surface within 10s of ultrasonic treatment by a dropper until the surface is covered with a layer of dispersion liquid, sequentially rotating the silicon wafer substrate on a spin coating platform at low speed of 300-; repeating the spin coating process for 20-30 times to obtain the quantum dot silicon wafer.
6) And (3) ZnO nanorod generation: taking a big beaker to contain 200 plus 300ml of 1.2-0.8mol/L double-distilled aqueous solution of zinc nitrate, adding 0.3-0.6g of hexamethylenetetramine under the rotary stirring at 35-45 ℃, stopping stirring after stirring for 15-25min to obtain long-rod mixed solution, reversely clamping the quantum dot silicon wafer by using a clamping device to ensure that a thin film layer on the quantum dot silicon wafer is just completely immersed into the long-rod mixed solution, standing for at least 12h, circularly cleaning the surface of the quantum dot silicon wafer for at least 3 times by using low-pressure deionized water spray and absolute ethyl alcohol spray, and airing until the surface is completely dried to obtain the solar cell structure.
Compared with the prior art, the invention has the following beneficial effects: 1) the performance is improved, through tests, the responsivity of the ZnO nanorod/graphene prepared by the dropping coating method in the prior art to ultraviolet light can reach 22.7A/W under 20V bias, but the dropping coating method causes very unstable performance of products, more than 10 times of experiments are repeated, the numerical value of some dropping coated devices is only 2.XA/W which is far lower than the highest numerical value, the instability in performance is mainly caused by dropping coating, and the prior art is also far away from device formation, the method uses the selected large-size graphene, and uses a mode of simultaneously adding and existing PVA insulating powder in dispersion, so that the prepared material has more stable performance, through tests, the responsivity of the device in the application to ultraviolet light is within a narrow interval between 26 and 28.5A/W under 20V bias, compared with the prior art, the method has the advantages of obvious improvement and stable performance. This prior art does not suggest. The technology is expected to provide stable ultraviolet photovoltaic devices and push the performance of the devices to a new height.
Drawings
FIG. 1 is a schematic diagram of a method of making a cell structure according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A graphene heterojunction solar cell structure, comprising: the device comprises a silicon wafer substrate layer, a graphene mixing layer, a ZnO nanorod layer, a plurality of silver colloids and a pair of Ti/Au electrodes; the silver glues are respectively coated on two opposite side edges of the silicon chip substrate layer, and a pair of Ti/Au electrodes are oppositely led out from the silver glues on the two opposite side edges; the main body of the graphene mixing layer is a large-radial-size reduced graphene microchip, and ZnO quantum dots are attached to an aggregate of the large-radial-size reduced graphene microchip; the ZnO nanorod layer is located above the graphene mixing layer, and all ZnO nanorods are formed by growing ZnO quantum dots on the upper surface of the graphene mixing layer. The silicon chip substrate layer is in a square sheet shape, the surface of the silicon chip substrate layer is required to be repeatedly cleaned by water and organic solvent, furthermore, the pair of Ti/Au electrodes are used as terminal electrodes and are in a narrow strip shape similar to the two opposite side edges of the silicon chip substrate layer in size, silver colloid is adhered to the outer sides of the pair of Ti/Au electrodes, and a lead is led out from the silver colloid adhered to the outer sides. The narrow strip-shaped lead-out adapts to the shape of a silicon device, and the cell structure can generate current when the ZnO nanorod surface receives ultraviolet light.
Example 2
The preparation method of the graphene heterojunction solar cell structure is used for preparing the graphene heterojunction solar cell structure in the embodiment 1, and is characterized by comprising the following steps: 1) a silicon wafer substrate preparation step: and polishing to remove an oxide layer of the silicon wafer substrate, loading absolute ethyl alcohol in a spray can, cleaning for multiple times, continuously cleaning with sufficient amount of double distilled water at 40 ℃, absolute ethyl alcohol, double distilled water and absolute ethyl alcohol, and airing to obtain a clean silicon wafer substrate.
2) The preparation method of the graphene nanoplatelets comprises the following steps: taking a large number of prefabricated expanded graphite sheets as raw materials, and ultrasonically stripping the raw materials in absolute ethyl alcohol for more than 1.5 hours to generate graphene microchip dispersion liquid; taking out the upper-layer dispersion liquid through low-frequency ultrasound, and leaving the graphite which is not stripped in the container; the process of abandoning: supplementing absolute ethanol as solvent of upper layer dispersion liquid to above 220ml, high intensity ultrasonic oscillating for 4min, standing for 6s, immediately discarding half of upper layer dispersion liquid, and supplementing absolute ethanol to above 220ml volume; repeating the lifting process for at least 15 times until the average radial size of the graphene nanoplatelets is higher than 5m as confirmed by AFM or SEM; and (3) evaporating most of the solvent in a spinning mode, and drying at normal temperature under the condition of discontinuously using weak nitrogen for blowing so as to obtain the graphene oxide micro-sheets with large radial sizes.
3) And (3) graphene nanoplatelets reduction: taking a four-mouth bottle with the volume of more than 2L, adding 180 parts by weight of double distilled water, inserting a stirring rod from the first mouth of the four-mouth bottle, stirring at 3-5 revolutions per second, and keeping the temperature and stirring continuously at 40 ℃; taking 0.2 weight part of PVA (polyvinyl acetate) ultrafine powder which is subjected to repeated freeze-drying powder crushing until the average particle size is below 60 mu m, and slowly adding the PVA ultrafine powder from the second opening of the four-opening bottle; slowly adding 20 parts by weight of graphene oxide micro-sheets with large radial dimension from the second port of the four-port bottle, after all the graphene oxide micro-sheets are added, dissolving 5 parts by weight of ascorbic acid with double-distilled water at 40 ℃, keeping the solution at 40 ℃, magnetically stirring the ascorbic acid solution, and adding the ascorbic acid solution from the third port of the four-port bottle by using a dropper at the speed of 24 drops/min until the addition is finished; stirring for 12min, dropwise adding ammonia water from the third port, measuring pH value while dropwise adding, and stopping dropwise adding ammonia water when the pH value is stably higher than 7 and is kept for more than 5 min; and stirring for 12min, pouring out the mixture in the four-mouth bottle, removing supernatant, and continuously washing for 6 times by using excessive absolute ethyl alcohol, double distilled water, absolute ethyl alcohol and double distilled water at about 40 ℃ to obtain the completely reduced large-radial-size reduced graphene nanoplatelets.
4) The preparation method of the spin coating mother solution comprises the following steps: taking a big beaker, holding 190ml of anhydrous methanol, placing on a magnetic stirring table with a heating function, heating to 40 ℃ and keeping, and continuously stirring at the speed of 3-5 revolutions per second by using a polytetrafluoroethylene rotor; 0.06g of PVA ultrafine powder which is crushed into 60um below average particle size by freeze-drying powder for many times is slowly added into a big beaker; weighing 4g of ZnO quantum dot powder and 9g of reduced graphene micro-sheets, and respectively putting the ZnO quantum dot powder and the reduced graphene micro-sheets into a ZnO quantum dot sieve barrel and a reduced graphene micro-sheet sieve barrel, wherein microporous filter membranes with the average pore diameter of 25um are arranged on the lower surfaces of the ZnO quantum dot sieve barrel and the reduced graphene micro-sheet sieve barrel; and (3) slowly sieving the two substances into a big beaker by using a ZnO quantum dot sieve barrel and a reduced graphene microchip sieve barrel for about the same time, heating the mixture in the big beaker to 60 ℃ under the continuous stirring at the speed of 3-5 r/s, and slowly evaporating the mixture to about 1/4 volumes to obtain a concentrated dispersion liquid.
5) The preparation method of the film comprises the following steps: placing a clean silicon wafer substrate at the center of the upper surface of a spin coating table, and continuously keeping the concentrated dispersion liquid in an ultrasonic dispersion state; spin coating process: dripping the silicon wafer substrate surface by a dropper within 10s from ultrasonic wave till the surface is covered with a layer of dispersion liquid, sequentially rotating the silicon wafer substrate on a spin-coating platform at a low speed of 400r/min for 6-10s and at a high speed of 1200r/min for 10-15s, and naturally drying; repeating the spin coating process for 25 times to obtain the quantum dot silicon wafer.
6) And (3) ZnO nanorod generation: taking a big beaker to contain 220ml of 0.9mol/L double-distilled water solution of zinc nitrate, adding 0.4g of hexamethylenetetramine under the rotary stirring at 40 ℃, stirring for 15-25min, stopping stirring to obtain long-rod mixed solution, reversely clamping the quantum dot silicon wafer by using a clamping device, enabling a thin film layer on the quantum dot silicon wafer to be just completely immersed into the long-rod mixed solution, standing for at least 12h, circularly cleaning the surface of the quantum dot silicon wafer for at least 3 times by using low-pressure deionized water spray and absolute ethyl alcohol spray, and airing until the surface is completely dried to obtain the solar cell structure.
Example 3
The preparation method of the graphene heterojunction solar cell structure is used for preparing the graphene heterojunction solar cell structure in the embodiment 1, and is characterized by comprising the following steps: 1) a silicon wafer substrate preparation step: and polishing to remove an oxide layer of the silicon wafer substrate, loading absolute ethyl alcohol in a spray can, cleaning for multiple times, continuously cleaning with sufficient double distilled water at 45 ℃, absolute ethyl alcohol, double distilled water and absolute ethyl alcohol, and airing to obtain a clean silicon wafer substrate. A clean, contaminant-free substrate is necessary here, otherwise various effects can occur.
2) The preparation method of the graphene nanoplatelets comprises the following steps: taking a large number of prefabricated expanded graphite sheet layers as raw materials, and ultrasonically stripping in absolute ethyl alcohol for more than 2 hours to generate graphene microchip dispersion liquid; taking out the upper-layer dispersion liquid through low-frequency ultrasound, and leaving the graphite which is not stripped in the container; the process of abandoning: supplementing the solvent absolute ethyl alcohol of the upper layer dispersion liquid to more than 270ml, carrying out high-intensity ultrasonic oscillation for 5min, standing for 9s, immediately discarding the upper half dispersion liquid, and supplementing the absolute ethyl alcohol to the volume of more than 220 ml; repeating the lifting process for at least 20 times until the average radial size of the graphene nanoplatelets is higher than 5m as confirmed by AFM or SEM; and (3) evaporating most of the solvent in a spinning mode, and drying at normal temperature under the condition of discontinuously using weak nitrogen for blowing so as to obtain the graphene oxide micro-sheets with large radial sizes. The graphene microchip with the large radial size is selected to ensure that the prepared film is more uniform, the vertical upward tendency of the ZnO nanorod generated on the surface is stronger, and after all, the size distribution of the stripped graphene is very wide.
3) And (3) graphene nanoplatelets reduction: taking a four-mouth bottle with the volume of more than 2L, adding 180 parts by weight of double distilled water, inserting a stirring rod from the first mouth of the four-mouth bottle, stirring at 5-8 r/s, and keeping the temperature and stirring continuously at 45 ℃; taking 0.3 weight part of PVA (polyvinyl acetate) ultrafine powder which is subjected to repeated freeze-drying powder crushing until the average particle size is below 60 mu m, and slowly adding the PVA ultrafine powder from the second opening of the four-opening bottle; slowly adding 20 parts by weight of graphene oxide micro-sheets with large radial dimension from the second port of the four-port bottle, after all the graphene oxide micro-sheets are added, dissolving 8 parts by weight of ascorbic acid by using double-distilled water at 45 ℃, keeping the solution at 45 ℃, magnetically stirring the ascorbic acid solution, and adding the ascorbic acid solution from the third port of the four-port bottle by using a dropper at the speed of 28 drops/min until the addition is finished; stirring for 14min, dropwise adding ammonia water from the third port, measuring pH value while dropwise adding, and stopping dropwise adding ammonia water when the pH value is stably higher than 7 and is kept for more than 5 min; and stirring for 14min, pouring out the mixture in the four-mouth bottle, removing supernatant, and continuously washing with excess absolute ethyl alcohol, double distilled water, absolute ethyl alcohol and double distilled water at about 40 ℃ for 6 times to obtain the completely reduced large-radial-size reduced graphene nanoplatelets. Through comparison tests, the reduced graphene and the unreduced graphene have better surface adhesion condition and good electrical property after being obviously reduced, so that a special reduction step is performed.
4) The preparation method of the spin coating mother solution comprises the following steps: taking a big beaker, holding 210ml of anhydrous methanol in the beaker, placing the beaker on a magnetic stirring table with a heating function, heating the beaker to 45 ℃ and keeping the temperature, and continuously stirring the beaker at the speed of 5-8 revolutions per second by using a polytetrafluoroethylene rotor; 0.08g of PVA (polyvinyl alcohol) ultrafine powder which is crushed into 60um or less in average particle size through repeated freeze-drying is slowly added into a big beaker; weighing 5g of ZnO quantum dot powder and 10g of reduced graphene micro-sheets, and respectively putting the ZnO quantum dot powder and the reduced graphene micro-sheets into a ZnO quantum dot sieve barrel and a reduced graphene micro-sheet sieve barrel, wherein microporous filter membranes with the average pore diameter of 30um are arranged on the lower surfaces of the ZnO quantum dot sieve barrel and the reduced graphene micro-sheet sieve barrel; and (3) slowly sieving the two substances into a big beaker by using a ZnO quantum dot sieve barrel and a reduced graphene microchip sieve barrel for about the same time, heating the mixture in the big beaker to 60 ℃ under the continuous stirring at the speed of 5-8 r/s, and slowly evaporating the mixture to about 1/4 volumes to obtain a concentrated dispersion liquid. The method has the key points that firstly, in order to prevent the ZnO quantum dots from being unevenly adhered and easily agglomerating, insulating PVA fine powder is added in the solution in advance and exists like isolated islands, so that the dispersity is higher, and secondly, the quantum dots and graphene are slowly added into the solution at a very slow speed, so that better conditions are provided for uniform dispersion.
5) The preparation method of the film comprises the following steps: placing a clean silicon wafer substrate at the center of the upper surface of a spin coating table, and continuously keeping the concentrated dispersion liquid in an ultrasonic dispersion state; spin coating process: dripping the silicon wafer substrate surface by a dropper within 10s from ultrasonic wave till the surface is covered with a layer of dispersion liquid, sequentially rotating the silicon wafer substrate on a spin-coating platform at a low speed of 500r/min for 6-10s and at a high speed of 1300r/min for 10-15s, and naturally drying; repeating the spin coating process for 30 times to obtain the quantum dot silicon wafer, sequentially cleaning with double distilled water and absolute ethyl alcohol, and air drying for later use. The spin coating process adopts the arrangement of first slow speed and then medium speed, so that not only is the material spread, but also too fast throwing-out is avoided, and the method is a mode which is more favorable for preparing the material.
6) And (3) ZnO nanorod generation: taking a big beaker to contain 270ml of 1.2mol/L double-distilled aqueous solution of zinc nitrate, adding 0.6g of hexamethylenetetramine under the rotary stirring at 45 ℃, stirring for 25min, stopping stirring to obtain long-rod mixed solution, reversely clamping the quantum dot silicon wafer by using a clamping device, enabling a thin film layer on the quantum dot silicon wafer to be just completely immersed in the long-rod mixed solution, standing for at least 12h, circularly cleaning the surface of the quantum dot silicon wafer for at least 3 times by using low-pressure deionized water spray and absolute ethyl alcohol spray, and drying till the surface is completely dried to obtain the solar cell structure.
Tests prove that the responsivity of the ZnO nanorod/graphene prepared by the dropping coating method in the prior art to ultraviolet light can be as high as 22.7A/W under 20V bias, but the dropping coating method causes very unstable product performance, more than 10 times of experiments are repeated, the numerical value of some dropping coated devices is only 2.XA/W which is far lower than the highest numerical value, the instability in performance is mainly caused by dropping coating, and the surface of the prior art is far away from device formation, the method uses the selected large-size graphene, and uses a mode of simultaneously adding and PVA insulating powder in dispersion, so that the prepared material has more stable performance, and the responsivity of the device in the prior art to the ultraviolet light is obviously improved in a narrow interval between 26 and 28.5A/W under 20V bias compared with the prior art, and the performance is stable.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (1)
1. A preparation method of a graphene heterojunction solar cell structure is used for preparing the following graphene heterojunction solar cell structure:
the device comprises a silicon wafer substrate layer, a graphene mixing layer, a ZnO nanorod layer, a plurality of silver colloids and a pair of Ti/Au electrodes; the plurality of silver glues are respectively coated on two opposite side edges of the silicon chip substrate layer, and a pair of Ti/Au electrodes are oppositely led out from the silver glues on the two opposite side edges; the main body of the graphene mixing layer is a large-radial-size reduced graphene microchip, and ZnO quantum dots are attached to an aggregate of the large-radial-size reduced graphene microchip; the ZnO nanorod layer is positioned on the graphene mixing layer, and all ZnO nanorods are formed by growing ZnO quantum dots on the upper surface of the graphene mixing layer;
the preparation method is characterized by comprising the following steps:
1) preparing a silicon wafer substrate layer: polishing to remove an oxide layer on the silicon wafer substrate layer, cleaning for multiple times by using absolute ethyl alcohol loaded in a spray can, continuously cleaning by using sufficient double distilled water-absolute ethyl alcohol-double distilled water-absolute ethyl alcohol at the temperature of 35-45 ℃, and airing to obtain a clean silicon wafer substrate layer;
2) the preparation method of the graphene nanoplatelets comprises the following steps: taking a large number of prefabricated expanded graphite sheets as raw materials, and ultrasonically stripping the raw materials in absolute ethyl alcohol for more than 1-2h to generate graphene microchip dispersion liquid; taking out the upper-layer dispersion liquid through ultrasonic treatment, and keeping the graphite which is not stripped in a container;
the process of abandoning: supplementing the solvent absolute ethyl alcohol of the upper layer dispersion liquid to more than 200 plus 300ml, ultrasonically oscillating for 3-5min, standing for 5-10s, immediately discarding the upper half dispersion liquid, and supplementing the absolute ethyl alcohol to the volume of more than 200 plus 300 ml; repeating the winnowing process for at least 10-20 times until the average radial size of the graphene nanoplatelets is higher than 5m as confirmed by AFM or SEM; most of the solvent is removed by rotary evaporation, and the graphene oxide micro-sheets with large radial sizes are obtained by drying at normal temperature under the condition of discontinuously purging with nitrogen;
3) and (3) graphene nanoplatelets reduction: taking a four-mouth bottle with the volume of more than 2L, adding 180 parts by weight of double distilled water, inserting a stirring rod from the first mouth of the four-mouth bottle, stirring at 3-10 r/s, and keeping the temperature to be 35-45 ℃ for continuous stirring;
0.2-0.4 weight part of PVA superfine powder which is subjected to repeated freeze-drying powder grinding until the average particle size is below 60um is slowly added from the second opening of the four-opening bottle;
slowly adding 20 parts by weight of graphene oxide micro-sheets with large radial dimension from the second port of the four-port bottle, after all the graphene oxide micro-sheets are added, dissolving 5-10 parts by weight of ascorbic acid with double-distilled water at 35-45 ℃, keeping the solution of ascorbic acid under magnetic stirring at 35-45 ℃, and adding the ascorbic acid solution from the third port of the four-port bottle by using a dropper at the speed of 20-30 drops/min until the addition is finished;
stirring for 10-15min, adding dropwise ammonia water from the third port, measuring pH value, and stopping adding ammonia water when pH value is stably higher than 7 and is kept for more than 5 min;
stirring for 10-15min, pouring out the mixture in the four-mouth bottle, removing supernatant, and continuously washing with excessive 40 ℃ absolute ethyl alcohol, double distilled water, absolute ethyl alcohol and double distilled water for 6 times to obtain fully-reduced large-radial-size reduced graphene nanoplatelets;
4) the preparation method of the spin coating mother solution comprises the following steps: taking a large beaker, carrying 180 ml of anhydrous methanol and 220ml of anhydrous methanol, placing the beaker on a magnetic stirring table with a heating function, heating the beaker to 35-45 ℃, keeping the temperature, and continuously stirring the beaker at the speed of 3-10 revolutions per second by using a polytetrafluoroethylene rotor;
0.05-0.1g of PVA (polyvinyl alcohol) ultrafine powder which is crushed into powder with the average particle size below 60um by freeze-drying for many times is slowly added into a big beaker;
weighing 3-5g of ZnO quantum dot powder and 8-10g of reduced graphene micro-sheets, and respectively putting the ZnO quantum dot powder and the reduced graphene micro-sheets into a ZnO quantum dot sieve barrel and a reduced graphene micro-sheet sieve barrel, wherein microporous filter membranes with average pore diameters of 20-40um are arranged on the lower surfaces of the ZnO quantum dot sieve barrel and the reduced graphene micro-sheet sieve barrel;
slowly screening the two substances into a big beaker by using a ZnO quantum dot sieve barrel and a reduced graphene microchip sieve barrel at the same time, heating the mixture in the big beaker to 60 ℃ under the continuous stirring at the speed of 3-10 r/s, and slowly evaporating the mixture to 1/4 volumes to obtain a concentrated dispersion liquid;
5) the preparation method of the film comprises the following steps: placing a clean silicon wafer substrate layer at the center of the upper surface of a spin coating table, and continuously keeping the concentrated dispersion liquid in an ultrasonic dispersion state;
spin coating process: dripping the silicon wafer substrate layer surface within 10s from ultrasonic by using a dropper until the surface is covered with a layer of dispersion liquid, sequentially rotating the silicon wafer substrate layer surface on a spin coating platform at low speed of 300-;
repeating the spin coating process for 20-30 times to obtain a quantum dot silicon wafer;
6) and (3) ZnO nanorod generation: taking a big beaker to contain 200-300ml of 1.2-0.8mol/L double-distilled aqueous solution of zinc nitrate, adding 0.3-0.6g of hexamethylenetetramine under the rotary stirring at 35-45 ℃, stopping stirring after stirring for 15-25min to obtain long-rod mixed solution, reversely clamping the quantum dot silicon wafer by using a clamping device to ensure that a thin film layer on the quantum dot silicon wafer is just completely immersed into the long-rod mixed solution, standing for at least 12h, circularly cleaning the surface of the quantum dot silicon wafer for at least 3 times by using deionized water spray and absolute ethyl alcohol spray, and airing until the surface is completely dried to obtain the solar cell structure.
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