CN113755164A - Green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process - Google Patents
Green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 35
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- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 33
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
- C09K11/562—Chalcogenides
- C09K11/565—Chalcogenides with zinc cadmium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract
The invention discloses a green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process, which relates to the technical field of nano material preparation and comprises the following steps: s1: placing peeled plant tubers containing starch in a crushing device, starting the crushing device to crush the plant tubers to obtain plant fragments; s2: the pulverized plant debris of S1 was placed in a clean beaker, and deionized water was added to the beaker. According to the green and environment-friendly preparation and manufacturing process of the cadmium sulfide quantum dots, the plant tubers containing the starch are used as the preparation raw materials of the leaching liquor, the green and environment-friendly preparation raw materials are pollution-free, no harm is brought to preparation personnel in the preparation process, the raw materials are easy to obtain, the manufacturing cost is low, the preparation process is suitable for mass production, the operation process is simple, the condition requirement required by the preparation process is not high, the required equipment requirement is low, the prepared quantum dots are uniform in size, small in surface defect and excellent in photoelectric performance.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation and manufacturing process of a green and environment-friendly cadmium sulfide quantum dot.
Background
Quantum dots are semiconductor nanostructures which bind excitons in three spatial directions, sometimes called "artificial atoms", "superlattices", "superatoms" or "quantum dot atoms", and are a new concept proposed in the 90 s of the 20 th century, cadmium sulfide quantum dots, which are the most important group II-IV semiconductors, have the characteristics of narrow band gap of 2.42eV, quantum confinement, surface area and the like, and are endowed with good optical, electrochemical and fluorescent properties, so that the cadmium sulfide quantum dots are widely applied in the detection fields of metals, drugs and the like, and the performance of cadmium sulfide nanomaterials depends on the size and spatial structure to a great extent, so in recent years, people are dedicated to preparing cadmium sulfide nanomaterials with required size and structure by different methods.
The existing common preparation methods of the cadmium sulfide quantum dots are high-temperature pyrolysis, sol-gel method, microemulsion method, precipitation method and hydrothermal method, wherein some preparation methods need to be prepared at high temperature, conditions do not allow mass preparation, the cost is high, and raw materials needed in some preparation methods can bring harm to the environment and the body of a preparation worker and cannot meet the requirements of the existing use, so that the preparation process of the cadmium sulfide quantum dots is green and environment-friendly.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a green and environment-friendly preparation process of cadmium sulfide quantum dots, and solves the problems in the background art.
In order to achieve the purpose, the invention is realized by the following technical scheme: a green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process comprises the following steps:
s1: placing peeled plant tubers containing starch in a crushing device, starting the crushing device to crush the plant tubers to obtain plant fragments;
s2: putting the crushed plant debris in the S1 into a clean beaker, and adding deionized water into the beaker;
s3: heating the beaker filled with the plant debris and the deionized water, and continuously stirring by using a stirrer;
s4: cooling the plant solution obtained after heating and stirring in the beaker to room temperature;
s5: placing the cooled plant solution in a centrifugal filter to obtain an initial plant leaching liquor containing starch, adding deionized water into the centrifugal filter after primary centrifugal filtration, performing centrifugal filtration again, and adding the filtrate into the initial plant leaching liquor to obtain a plant leaching liquor with a required volume;
s6: sequentially and slowly adding thioacetamide and cadmium sulfate into the plant leaching liquor obtained in the step S5, and continuously stirring the plant leaching liquor when adding the thioacetamide and the cadmium sulfate;
s7: placing the plant leaching liquor, thioacetamide and cadmium sulfate mixed solution into an electronic steam pressure sterilization pot for reaction;
s8: and (4) cooling the mixed solution subjected to pressure sterilization in the S7 to room temperature to obtain a uniformly dispersed aqueous cadmium sulfide quantum dot solution.
Optionally, the starch-containing plant tuber in S1 is selected from one of potato, taro, yam, pachyrhizus and purple sweet potato.
Alternatively, the starch-containing tubers of S1 are clean and free of impurities on the surface and rot on the inside.
Optionally, the amount of the plant debris placed in the beaker in the step S2 is 100 g.
Optionally, the heating temperature in S3 is 100 ± 3 ℃, and the heating time is 30 ± 3 minutes after boiling.
Optionally, the amount of thioacetamide added in S6 is 2.8 g, and the amount of cadmium sulfate added in S6 is 135 g.
Optionally, the reaction condition of the electronic steam pressure sterilizing pot in the step S7 is 125 +/-3 ℃, the reaction pressure is 105 +/-3 kPa, and the reaction time is 20 +/-3 minutes.
The invention provides a green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process, which has the following beneficial effects:
1. according to the green and environment-friendly preparation and manufacturing process of the cadmium sulfide quantum dots, the plant tubers containing the starch are used as the preparation raw materials of the leaching liquor, the green and environment-friendly preparation raw materials are pollution-free, no harm is brought to preparation personnel in the preparation process, the raw materials are easy to obtain, the manufacturing cost is low, the preparation process is suitable for mass production, the operation process is simple, the condition requirement required by the preparation process is not high, the required equipment requirement is low, the prepared quantum dots are uniform in size, small in surface defect and excellent in photoelectric performance.
2. The green and environment-friendly preparation and manufacturing process of the cadmium sulfide quantum dots has the advantages that the plant tubers containing the starch are crushed into chips during preparation, the starch-containing plant tubers are convenient to heat and dissolve, the preparation speed of the leaching liquor is increased, in addition, after the initial plant leaching liquor containing the starch is obtained from plant solution through primary centrifugation, deionized water is added into the centrifugal filter again and centrifugal filtration is continued, the plant leaching liquor with the required volume is obtained, the situation that the concentration of chemical substances in the initial plant leaching liquor is reduced too much by directly adding water into the initial plant leaching liquor to influence the quality of the leaching liquor is avoided, and in addition, the residual chemical substances in the centrifuged plant waste residues can be fully utilized.
Drawings
FIG. 1 is a graph showing the absorption spectrum of cadmium sulfide quantum dot solution prepared from potato extract according to the present invention on fluorescence;
FIG. 2 is a fluorescence absorption and emission spectrum of a cadmium sulfide quantum dot solution prepared from a potato extract of the present invention;
FIG. 3 is a fluorescence emission spectrum of leaching liquor prepared by using potatoes, taros, yams, sweet potatoes and purple potatoes as materials;
FIG. 4 is a comparison chart of X-ray diffraction tests of cadmium sulfide quantum dot solution prepared from the potato leach liquor and a standard substance;
FIG. 5 is a diagram of a cadmium sulfide quantum dot solution prepared from a potato extract of the present invention under a transmission electron microscope;
FIG. 6 is a diagram of a high resolution TEM image of a cadmium sulfide quantum dot solution prepared from a potato extract of the present invention;
FIG. 7 is an infrared spectrum of cadmium sulfide quantum dots prepared from potato extract of 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.
Referring to fig. 1 to 7, the present invention provides a technical solution: a green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process comprises the following steps:
s1: placing peeled plant tubers containing starch in a crushing device, starting the crushing device to crush the tubers to obtain plant fragments, and accelerating the speed of dissolving the plant fragments in deionized water;
s2: putting the crushed plant debris in the S1 into a clean beaker, and adding deionized water into the beaker;
s3: heating the beaker filled with the plant debris and the deionized water, and continuously stirring by using a stirrer to accelerate the mixing speed of the plant debris dissolved substance and the deionized water;
s4: cooling the plant solution obtained after heating and stirring in the beaker to room temperature;
s5: placing the cooled plant solution in a centrifugal filter to obtain an initial plant leaching liquor containing starch, adding deionized water into the centrifugal filter after primary centrifugal filtration, performing centrifugal filtration again, and adding the filtrate into the initial plant leaching liquor to obtain a plant leaching liquor with a required volume;
s6: sequentially and slowly adding thioacetamide and cadmium sulfate into the plant leaching liquor obtained in the step S5, and continuously stirring the plant leaching liquor when adding thioacetamide and cadmium sulfate to fully and uniformly mix the thioacetamide and the cadmium sulfate with the plant leaching liquor;
s7: placing the plant leaching liquor, thioacetamide and cadmium sulfate mixed solution into an electronic steam pressure sterilization pot for reaction;
s8: and (4) cooling the mixed solution subjected to pressure sterilization in the S7 to room temperature to obtain a uniformly dispersed aqueous cadmium sulfide quantum dot solution.
It is understood by those skilled in the art that, firstly, more than 120 g of potatoes are weighed and washed, peeled, then the peeled potatoes are placed in a crushing device for crushing, then 100 g of potato scraps are weighed and placed in a clean beaker, 250 ml of deionized water is added into the beaker, the beaker filled with the potato scraps and the deionized water is heated, the heating is continued for 30 minutes after the potato scraps and the deionized water are boiled, the stirrer is used for stirring during the heating process, the beaker is taken down after the heating, so that the potato solution is naturally cooled to the room temperature, then the potato solution is placed in a centrifugal filter to obtain an initial potato leaching solution containing starch, 250 ml of deionized water is added into the centrifugal filter after one centrifugal filtration, the centrifugal filtration is carried out again, and the filtrate is added into the initial potato leaching solution to obtain a total amount of 500 ml of potato leaching solution, then slowly adding 2.8 g of thioacetamide into 500 ml of potato extract, stirring the potato extract while adding the thioacetamide, then slowly adding 135 g of cadmium sulfate into the potato extract, stirring the potato extract while adding the cadmium sulfate in the same way, subpackaging the uniformly stirred potato extract, thioacetamide and cadmium sulfate mixed solution into six 120 ml conical flasks, sealing the conical flasks, then placing the conical flasks into an electronic steam pressure sterilizing pot, reacting for 20 minutes at 121 ℃ under the pressure of 102 kilopascals, and finally taking out the conical flasks to cool the potato extract, the thioacetamide and the cadmium sulfate mixed solution in the conical flasks to room temperature to obtain the uniformly dispersed cadmium sulfide quantum dot solution.
Performing fluorescence performance test analysis on the prepared cadmium sulfide quantum dot solution through a fluorescence spectrometer to obtain that the prepared cadmium sulfide quantum dot solution has different degrees of absorption of light with a wave band of 200-470 nm, wherein a wider and stronger absorption section is arranged in the wave band of 300-400 nm, and the absorption intensity of the aqueous cadmium sulfide quantum dot is highest at the position of lambda of 350nm, so that the lambda of 350nm is determined as the excitation wavelength of the cadmium sulfide quantum dot, under the condition that the excitation wavelength lambda of 350nm, a pure potato leaching solution is used as a reference to perform fluorescence spectrum test with aqueous cadmium sulfide, the potato leaching solution has no obvious fluorescence excitation in the test wavelength range, the aqueous cadmium sulfide quantum dot solution has an obvious emission peak at the position of lambda of 490nm, and finally the fluorescence emission wavelength of the aqueous cadmium sulfide quantum dot prepared in a laboratory is determined to be 490 nm;
testing the prepared cadmium sulfide quantum dot solution through X-ray diffraction to obtain that the prepared cadmium sulfide quantum dot sample is of a hexagonal crystal form, except for a characteristic peak of the cubic crystal form, no diffraction peak of other impurities exists, and the product is proved to be well crystallized;
observing the appearance of the prepared cadmium sulfide quantum dots by a transmission electron microscope and a transmission high-resolution electron microscope, observing that the cadmium sulfide quantum dots are in a spherical shape with uniform dispersion in a region, and observing that the particle size is about 5nm by the transmission high-resolution electron microscope;
the conditions of the surface binding molecules and groups of the cadmium sulfide quantum dots in the solution are measured through infrared spectroscopy, and the main effect of chemical substances (protein, mineral substances, vitamins, amino acid and the like) in the potato leaching liquor on the generation and the stabilization of the quantum dots is determined.
Wherein, the plant tuber containing starch in S1 is selected from one of potato, taro, rhizoma Dioscoreae, radix Pachyrhizi Erosi and purple sweet potato.
As can be understood by those skilled in the art, when the cadmium sulfide quantum dots are prepared, the cadmium sulfide quantum dots can be prepared by using plant tubers of potatoes, taros, yams, pachyrhizus and purple potatoes, and 100 g of taro chips, yam chips, pachyrhizus chips and purple potato chips can be respectively used for preparing taro extract, yam extract, pachyrhizus extract and purple potato extract according to the same method, so as to prepare similar cadmium sulfide quantum dots.
Wherein, the surface of the plant tuber containing starch in S1 is clean and has no impurities and no rot inside.
As can be understood by those skilled in the art, impurities outside the plant tuber and rotting bacteria inside the plant tuber are prevented from affecting the preparation of the cadmium sulfide quantum dots.
In S2, the amount of the plant debris placed in the beaker is 100 g.
It will be appreciated by those skilled in the art that a selected amount of plant debris is placed in a beaker to prepare the leach liquor, wherein the weight of the plant debris can be varied.
Wherein the heating temperature in S3 is 100 +/-3 ℃, and the heating time is 30 +/-3 minutes after boiling.
As will be understood by those skilled in the art, the plant debris in the beaker and the DI water are heated to 100 degrees Celsius so that the plant debris is melted into the plasma water, and the heating of the DI water is continued for another 30 minutes after boiling.
Wherein, the thioacetamide added in S6 is 2.8 g, and the cadmium sulfate added in S6 is 135 g.
It will be understood by those skilled in the art that when 100 grams of plant debris is weighed, 2.8 grams of thioacetamide and 135 grams of cadmium sulfate are added, and when the weight of the plant debris is changed, the adaptation of thioacetamide and cadmium sulfate changes.
Wherein, the reaction condition of the electronic steam pressure sterilizing pot in the S7 is 125 plus or minus 3 ℃, the reaction pressure is 105 plus or minus 3 kilopascals, and the reaction time is 20 plus or minus 3 minutes.
As can be understood by those skilled in the art, when the temperature inside the electronic steam pressure sterilization pot is 125 +/-3 ℃, the reaction pressure is 105 +/-3 kPa, and the reaction time is 20 +/-3 minutes, the sterilization effect on the conical flask which is placed inside the electronic steam pressure sterilization pot and filled with the plant leaching solution, the thioacetamide and the cadmium sulfate mixed solution is optimal.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A preparation and manufacturing process of green and environment-friendly cadmium sulfide quantum dots is characterized by comprising the following steps:
s1: placing peeled plant tubers containing starch in a crushing device, starting the crushing device to crush the plant tubers to obtain plant fragments;
s2: putting the crushed plant debris in the S1 into a clean beaker, and adding deionized water into the beaker;
s3: heating the beaker filled with the plant debris and the deionized water, and continuously stirring by using a stirrer;
s4: cooling the plant solution obtained after heating and stirring in the beaker to room temperature;
s5: placing the cooled plant solution in a centrifugal filter to obtain an initial plant leaching liquor containing starch, adding deionized water into the centrifugal filter after primary centrifugal filtration, performing centrifugal filtration again, and adding the filtrate into the initial plant leaching liquor to obtain a plant leaching liquor with a required volume;
s6: sequentially and slowly adding thioacetamide and cadmium sulfate into the plant leaching liquor obtained in the step S5, and continuously stirring the plant leaching liquor when adding the thioacetamide and the cadmium sulfate;
s7: placing the plant leaching liquor, thioacetamide and cadmium sulfate mixed solution into an electronic steam pressure sterilization pot for reaction;
s8: and (4) cooling the mixed solution subjected to pressure sterilization in the S7 to room temperature to obtain a uniformly dispersed aqueous cadmium sulfide quantum dot solution.
2. The preparation and manufacturing process of the green and environment-friendly cadmium sulfide quantum dot according to claim 1, characterized by comprising the following steps: the starch-containing plant tuber in the S1 is selected from one of potato, taro, yam, pachyrhizus and purple sweet potato.
3. The preparation and manufacturing process of the green and environment-friendly cadmium sulfide quantum dot according to claim 1, characterized by comprising the following steps: the starch-containing tubers in S1 were clean and free of impurities on the surface and rotten on the inside.
4. The preparation and manufacturing process of the green and environment-friendly cadmium sulfide quantum dot according to claim 1, characterized by comprising the following steps: the amount of the plant debris placed in the beaker in the S2 is 100 g.
5. The preparation and manufacturing process of the green and environment-friendly cadmium sulfide quantum dot according to claim 1, characterized by comprising the following steps: the heating temperature in the S3 is 100 +/-3 ℃, and the heating time is 30 +/-3 minutes after boiling.
6. The preparation and manufacturing process of the green and environment-friendly cadmium sulfide quantum dot according to claim 1, characterized by comprising the following steps: the thioacetamide added in S6 was 2.8 g, and the cadmium sulfate added in S6 was 135 g.
7. The preparation and manufacturing process of the green and environment-friendly cadmium sulfide quantum dot according to claim 1, characterized by comprising the following steps: the reaction condition of the electronic steam pressure sterilizing pot in the S7 is 125 +/-3 ℃, the reaction pressure is 105 +/-3 kPa, and the reaction time is 20 +/-3 minutes.
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| Publication number | Priority date | Publication date | Assignee | Title |
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