CN111122556A - Method for detecting chloroform in quantum dot solution - Google Patents
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- CN111122556A CN111122556A CN201811287432.XA CN201811287432A CN111122556A CN 111122556 A CN111122556 A CN 111122556A CN 201811287432 A CN201811287432 A CN 201811287432A CN 111122556 A CN111122556 A CN 111122556A
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Abstract
The invention discloses a method for detecting chloroform in a quantum dot solution, which comprises the following steps: providing an initial quantum dot solution, wherein the quantum dots in the initial quantum dot solution do not contain sulfur element; carrying out primary illumination treatment on the initial quantum dot solution; and inserting the test glass with the surface covered with silver nitrate into the initial quantum dot solution subjected to the first illumination treatment, and judging whether the initial sulfur-containing quantum dot solution contains chloroform or not. The method provided by the invention can intuitively, efficiently and accurately judge whether the chloroform exists in the initial quantum dot solution.
Description
Technical Field
The invention relates to the field of chloroform qualitative detection, in particular to a method for detecting chloroform in a quantum dot solution.
Background
In the process of preparing the quantum dot solution, usually, after the quantum dots are washed for the last time, chloroform is needed to wash the quantum dots down and transfer the quantum dots into a sample bottle, then the sample bottle is put into a vacuum drying oven to evaporate the chloroform to dryness to obtain quantum dot powder, and then a proper solvent (generally n-octane or n-hexane) is used for dissolving to obtain the quantum dot solution, wherein the components of the quantum dot solution comprise a large amount of n-octane solvent, the quantum dots and a small amount of washing solvent (chloroform, ethyl acetate, methanol, acetone and the like). The chloroform is remained in the quantum dot solution because of incomplete evaporation, and the bottle cap of the sample bottle made of plastic materials can be corroded; the purity of the quantum dot product and the performance of the quantum dot are greatly influenced; devices can be formed with corrosion on the device surface, resulting in reduced device lifetime and efficiency.
At present, chloroform detection methods comprise high performance liquid chromatography, gas chromatography, colorimetric titration and the like, wherein the chromatography needs to be analyzed by a large instrument, is not suitable for field detection, and has high cost and long detection time; the colorimetric titration method is difficult to control, has relatively large calculation error and is easily influenced by external factors.
In addition, chloroform, which is generally used as a solvent, an extractant, and a preservative, is chemically stable and is difficult to react with a substance to generate an obvious experimental phenomenon or convert into another substance to be detected. If a device is fabricated using a quantum dot solution in which chloroform remains, the chloroform corrodes the surface of the device, resulting in a decrease in the lifetime and luminous efficiency of the device, and therefore, the chloroform remaining in the quantum dot solution must be removed before the device is fabricated using the quantum dot solution. However, the preparation process of materials used for chloroform purification is tedious, high in price and large in dosage, and when the purification is completed during the purification cannot be accurately known, so that in order to save the investment of the purification cost, the prior art needs to develop a cheap, rapid and accurate method suitable for qualitatively detecting whether chloroform exists in a quantum dot solution.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide an intuitive, fast and accurate method for detecting the presence of chloroform in a quantum dot solution.
The technical scheme of the invention is as follows:
a method for detecting chloroform in a quantum dot solution comprises the following steps:
providing an initial quantum dot solution, wherein the quantum dots in the quantum dot solution do not contain sulfur element;
carrying out primary illumination treatment on the initial quantum dot solution;
and (3) placing one section or the whole of the part of the test glass, the surface of which is covered with the silver nitrate, in the initial quantum dot solution subjected to the first illumination treatment, and judging whether the initial sulfur-containing quantum dot solution contains chloroform or not.
Has the advantages that: the method comprises the steps of converting the detection of chloroform in a quantum dot solution into the detection of hydrogen chloride in the quantum dot solution by utilizing the principle that the chloroform generates phosgene and hydrogen chloride under the illumination condition, inserting test glass with the surface covered with silver nitrate into the initial quantum dot solution subjected to primary illumination treatment, and then detecting the surface of the test glass taken out to judge whether the chloroform exists in the initial quantum dot solution; if the glass surface for testing is detected to be colorless and transparent, determining that the initial quantum dot solution does not contain chloroform; and if the white substance on the surface of the glass for testing is detected to be present, carrying out secondary light irradiation treatment on the surface of the glass for testing, and if the white substance on the surface of the glass for testing is blackened, judging that the initial quantum dot solution contains chloroform. The method provided by the invention can simply, intuitively and efficiently make an accurate judgment on whether the chloroform exists in the sulfur-free quantum dot solution.
Drawings
FIG. 1 is a diagram of a preferred embodiment of the method for detecting chloroform in a quantum dot solution according to the invention.
Detailed Description
The invention provides a method for detecting chloroform in a quantum dot solution, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the process of preparing the quantum dot solution, a small amount of chloroform usually remains in the quantum dot solution because the chloroform cannot be completely evaporated, and the chloroform not only corrodes a bottle cap made of a plastic material, but also reduces the performance and purity of the quantum dot. If a device is fabricated using a quantum dot solution in which chloroform remains, the chloroform corrodes the surface of the device, resulting in a decrease in the lifetime and luminous efficiency of the device, and therefore, the chloroform remaining in the quantum dot solution must be removed before the device is fabricated using the quantum dot solution. However, the preparation process of the material used for removing the impurities from the chloroform is complicated, the price is high, the dosage is large, and when the impurities are removed, the time when the impurities are removed cannot be accurately known. Therefore, in order to save the investment of impurity removal cost, an intuitive, rapid and accurate method suitable for detecting whether chloroform exists in a quantum dot solution is urgently needed in the prior art.
Based on the problems in the prior art, the specific embodiment of the invention provides a method for detecting chloroform in a quantum dot solution, which comprises the following steps:
s10, providing an initial quantum dot solution, wherein the quantum dots in the quantum dot solution do not contain sulfur element;
s20, carrying out first illumination treatment on the initial quantum dot solution;
s30, placing one section or all of the part, covered with silver nitrate, of the surface of the glass for testing in the initial quantum dot solution subjected to the first illumination treatment, and judging whether the initial sulfur-containing quantum dot solution contains chloroform or not;
s40, if the surface of the glass for testing is detected to be colorless and transparent, the initial quantum dot solution does not contain chloroform;
and S50, if the white substance on the surface of the glass for testing is detected to exist, carrying out secondary light irradiation treatment on the surface of the glass for testing, and if the white substance on the surface of the glass for testing is blackened, enabling the initial quantum dot solution to contain chloroform.
The method provided by the embodiment can intuitively, efficiently and accurately judge whether the chloroform exists in the initial quantum dot solution, and the implementation principle is as follows:
this example utilizes the decomposition of chloroform to phosgene and hydrogen chloride (2 CHCl) under light conditions3+O2=2COCl2+2 HCl) converts the detection of chloroform in the initial quantum dot solution to the detection of hydrogen chloride in the initial quantum dot solution, the quantum dots in the initial quantum dot solution not containing elemental sulfur. Specifically, as shown in FIG. 1, when chloroform is present in the initial quantum dot solution, light is appliedUnder the irradiation condition, chloroform is decomposed, the generated phosgene is used as gas to leave the initial quantum dot solution, and residual hydrogen chloride is left in the initial quantum dot solution. Therefore, silver ions are added into the initial quantum dot solution subjected to the light irradiation treatment, and the existence of chloroform in the initial quantum dot solution can be judged by observing whether the reaction occurs and white precipitate AgCl is generated.
However, in a high concentration quantum dot solution, the formation of a minute amount of white precipitate is not easily observed. Therefore, in this embodiment, the test glass with the surface covered with silver nitrate is inserted into the initial quantum dot solution subjected to the first illumination treatment, and then the surface of the test glass taken out is detected to determine whether chloroform exists in the initial quantum dot solution; if the glass surface for testing is detected to be colorless and transparent, determining that the initial quantum dot solution does not contain chloroform; and if the white substance is detected to exist on the surface of the glass for testing, carrying out second illumination treatment on the surface of the glass, and if the white substance is changed into purple firstly and then changed into black, indicating that the white substance is AgCl (AgCl is unstable to light and is changed into purple firstly and then changed into black) so as to judge that the initial quantum dot solution contains chloroform.
In a preferred embodiment, the quantum dots in the initial quantum dot solution are free of elemental sulfur. Preferably, the quantum dots are selected from one or more of group II-VI compounds, group III-V compounds, and group IV-VI compounds, but not limited thereto. More preferably, the II-VI compound is selected from one or more of CdSe, ZnSe, CdTe, ZnTe, CdZnSe, CdZnTe, ZnSeTe, CdSeTe and CdZnSeTe, but not limited thereto. More preferably, the III-V compound is selected from one or more of InP, InAs and InAsP, but is not limited thereto. More preferably, the group IV-VI compound is selected from one or more of PbSe, PbTe and PbSeTe, but is not limited thereto.
In a preferred embodiment, in the present embodiment, instead of directly dropping a silver nitrate solution into an initial quantum dot solution, a test glass with a surface covered with silver nitrate is inserted into the initial quantum dot solution, so that whether the initial quantum dot solution contains chloroform can be determined by observing whether a white substance is generated on the glass, and thus, the problem of difficulty in observing experimental phenomena is effectively solved.
Preferably, in this embodiment, the preparation method of the glass for testing with the surface covered with silver nitrate includes the steps of: providing a test glass substrate; and coating a silver nitrate solution on the surface of the test glass substrate to obtain the test glass with the surface covered with silver nitrate. In an alternative embodiment, the glass surface is completely covered with silver nitrate, the glass can be completely placed in the sulfur-free quantum dot solution, or a part of the surface of the glass can be placed in the sulfur-free quantum dot solution. In an alternative embodiment, a part of the glass surface is covered with silver nitrate, the part of the glass surface covered with silver nitrate can be completely placed in the sulfur-free quantum dot solution, and a section of the glass surface covered with silver nitrate can also be placed in the sulfur-free quantum dot solution.
Because the surface of the glass is smooth, if the silver nitrate solution is directly coated on the surface of the glass, the situation that the silver nitrate is not tightly combined with the glass is easy to occur, and in order to avoid the situation, the embodiment also provides another method for preparing the glass for testing with the surface covered with the silver nitrate, which comprises the following steps: providing a colorless and transparent adhesive; and after the adhesive is coated on the surface of the glass substrate for testing, coating a silver nitrate solution on the surface of the adhesive to obtain the glass for testing with the surface covered with silver nitrate. In this embodiment, silver nitrate can be tightly bonded to the test glass surface by coating the test glass surface with a layer of adhesive in advance.
Preferably, the adhesive is reactive with neither silver nitrate nor quantum dots. More preferably, the adhesive is selected from one or two of urea-formaldehyde resin and phenol-formaldehyde resin, but is not limited thereto.
In a preferred embodiment, the present example further provides a method for preparing a test glass with a surface covered with silver nitrate, comprising the steps of: providing a colorless and transparent adhesive; and coating the adhesive on the surface of the glass substrate for testing, drying, and coating a silver nitrate solution on the surface of the adhesive to obtain the glass for testing with the surface covered with silver nitrate.
Specifically, this example illustrates the preparation of a test glass with a surface covered with silver nitrate by spin coating: fixing the glass substrate for testing on a spin coater, dropwise adding a colorless and transparent adhesive on the surface of the glass substrate for testing, controlling the glass substrate for testing to rotate at the rotating speed of 5000-.
Further, dropwise adding a prepared silver nitrate solution on the adhesive film of the glass substrate for testing, and continuously controlling the glass substrate for testing to rotate at the rotating speed of 5000-; and drying the silver nitrate solution on the adhesive film to obtain the glass for testing with the surface covered with silver nitrate. Preferably, the test glass with the silver nitrate coated on the surface is placed in a vacuum drying oven to be dried for 6 hours, so that the test glass with the silver nitrate covered on the surface is prepared.
Preferably, the silver nitrate solution has a concentration of 1-50mg/ml, and is prepared by dissolving 10-500nm silver nitrate in 10ml ethanol.
Preferably, the glass substrate for testing is FTO glass or ITO glass. Because the FTO glass surface is provided with the tin oxide film, and the ITO glass surface is provided with the indium tin oxide film, uneven ravines can be observed on the tin oxide film and the indium tin oxide film under microscopic conditions, which is more favorable for the silver nitrate to be firmly bonded on the FTO glass or the ITO glass surface.
In a preferred embodiment, a sample bottle containing an initial quantum dot solution is placed under a light source in an open manner, a first illumination treatment is carried out for 10-30min, then a test glass with the surface covered with silver nitrate is inserted into the initial quantum dot solution, after a reaction is carried out for 8-15min, the test glass is taken out and the state of the surface of the test glass is observed, and if the surface of the test glass is detected to be colorless and transparent, the initial quantum dot solution is judged to be free of chloroform; and if the white substance on the surface of the glass for testing is detected to be present, carrying out secondary illumination treatment on the surface of the glass for testing, and if the white substance on the surface of the glass for testing is changed into purple firstly and then is changed into black, judging that the initial quantum dot solution contains chloroform.
The following is a further explanation of the method for detecting chloroform in a quantum dot solution according to the present invention by specific examples:
example 1
1) Respectively performing ultrasonic treatment on the common glass in acetone, ethanol and water for 20 min, and drying for later use;
2) dissolving 10 mg of silver nitrate in 10ml of ethanol to prepare 1 mg/ml of silver nitrate solution for later use;
3) fixing common glass on a spin coater, dripping 200 microliters of adhesive on the common glass, rotating at a high speed of 5000 r/min for 20 s to uniformly spread the adhesive into a film, and standing at room temperature to naturally dry the film; dripping 200 microliters of silver nitrate solution on the glass, rotating at a high speed of 10000r/min for 20 s to uniformly spread the silver nitrate solution into a film, standing at room temperature to naturally dry the film, and then putting the film into a vacuum drying oven to dry for 6 hours to obtain silver nitrate glass;
4) placing the sample bottle filled with the A quantum dot solution under a light source in an open manner, and irradiating for 10-30 min;
5) putting silver nitrate glass into a sample bottle, reacting for 10 min, taking out and observing a white substance on the surface of the glass, changing the white substance into purple after illumination, and then changing into black, and judging that the A quantum dot solution contains chloroform.
Example 2
1) Respectively performing ultrasonic treatment on the FTO glass in acetone, ethanol and water for 20 min, and drying for later use;
2) dissolving 100 mg of silver nitrate in 10ml of ethanol to prepare 10 mg/ml of silver nitrate solution for later use;
3) dripping 200 microliters of silver nitrate solution on glass, rotating at a high speed of 10000r/min for 20 s to uniformly spread the silver nitrate solution into a film, standing at room temperature to naturally dry the film, and then putting the film into a vacuum drying oven to dry for 6 hours to obtain silver nitrate glass;
4) placing the sample bottle filled with the B quantum dot solution under a light source in an open manner, and irradiating for 10-30 min;
5) and putting silver nitrate glass into a sample bottle, reacting for 10 min, taking out the sample bottle, observing the surface of the glass, wherein the glass is still colorless and transparent, no white substance exists, and the glass is still colorless and transparent after illumination, and judging that the B quantum dot solution does not contain chloroform.
Example 3
1) Carrying out ultrasonic treatment on the ITO glass in acetone, ethanol and water for 20 min respectively, and drying for later use;
2) dissolving 500 mg of silver nitrate in 10ml of ethanol to prepare 50mg/ml of silver nitrate solution for later use;
3) dripping 200 microliters of silver nitrate solution on glass, rotating at a high speed of 8000 r/min for 20 s to uniformly spread the silver nitrate solution into a film, standing at room temperature to naturally dry the film, and then putting the film into a vacuum drying oven to dry for 6 hours to obtain silver nitrate glass;
4) placing the sample bottle filled with the C quantum dot solution under a light source in an open manner, and irradiating for 10-30 min;
5) putting silver nitrate glass into a sample bottle, reacting for 10 min, taking out and observing a white substance on the surface of the glass, changing the white substance into purple after illumination, and then changing into black, and judging that the C quantum dot solution contains chloroform.
Example 4
1) Respectively performing ultrasonic treatment on the FTO glass in acetone, ethanol and water for 20 min, and drying for later use;
2) dissolving 100 mg of silver nitrate in 10ml of ethanol to prepare 10 mg/ml of silver nitrate solution for later use;
3) dripping 200 microliters of silver nitrate solution on glass, rotating at a high speed of 10000r/min for 20 s to uniformly spread the silver nitrate solution into a film, standing at room temperature to naturally dry the film, and then putting the film into a vacuum drying oven to dry for 6 hours to obtain silver nitrate glass;
4) placing the sample bottle filled with the D quantum dot solution under a light source in an open manner, and irradiating for 10-30 min;
5) and putting silver nitrate glass into a sample bottle, reacting for 10 min, taking out the glass, observing the surface of the glass to obtain a white substance, changing the white substance into purple after illumination, and then changing the white substance into black, and judging that the D quantum dot solution contains chloroform.
In summary, the invention utilizes the principle that chloroform generates phosgene and hydrogen chloride under the illumination condition, the detection of chloroform in the quantum dot solution is converted into the detection of hydrogen chloride in the quantum dot solution, the test glass with the surface covered with silver nitrate is inserted into the initial quantum dot solution subjected to the first illumination treatment, and then the surface of the test glass taken out is detected to judge whether the chloroform exists in the initial quantum dot solution; if the glass surface for testing is detected to be colorless and transparent, determining that the initial quantum dot solution does not contain chloroform; and if the white substance on the surface of the glass for testing is detected to be present, carrying out secondary light irradiation treatment on the surface of the glass for testing, and if the white substance on the surface of the glass for testing is blackened, judging that the initial quantum dot solution contains chloroform. The method provided by the invention can simply, intuitively and efficiently make an accurate judgment on whether the chloroform exists in the sulfur-free quantum dot solution.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for detecting chloroform in a quantum dot solution is characterized by comprising the following steps:
providing an initial quantum dot solution, wherein the quantum dots in the initial quantum dot solution do not contain sulfur element;
carrying out primary illumination treatment on the initial quantum dot solution;
and (3) placing one section or the whole of the part of the test glass, the surface of which is covered with the silver nitrate, in the initial quantum dot solution subjected to the first illumination treatment, and judging whether the initial sulfur-containing quantum dot solution contains chloroform or not.
2. The method for detecting chloroform in a quantum dot solution as claimed in claim 1, wherein a part or all of a portion of the test glass, the surface of which is covered with silver nitrate, is placed in the initial quantum dot solution subjected to the first light irradiation,
if the test glass surface is detected to be colorless and transparent, the initial quantum dot solution does not contain chloroform;
and if the white substance on the surface of the glass for testing is detected to be present, carrying out secondary light irradiation treatment on the surface of the glass for testing, and if the white substance on the surface of the glass for testing is blackened, enabling the initial quantum dot solution to contain chloroform.
3. The method for detecting chloroform in a quantum dot solution according to claim 1, wherein the quantum dots in the initial quantum dot solution are selected from one or more of group II-VI compounds, group III-V compounds and group IV-VI compounds.
4. The method for detecting chloroform in a quantum dot solution as claimed in claim 1, wherein the test glass with the surface covered with silver nitrate is prepared by the method comprising the steps of:
providing a test glass substrate;
and coating the silver nitrate solution on the surface of the test glass substrate to obtain the test glass with the surface covered with silver nitrate.
5. The method for detecting chloroform in a quantum dot solution as claimed in claim 1, wherein the test glass with the surface covered with silver nitrate is prepared by the method comprising the steps of:
providing a colorless and transparent adhesive;
and after the adhesive is coated on the surface of the glass substrate for testing, coating a silver nitrate solution on the surface of the adhesive to obtain the glass for testing with the surface covered with silver nitrate.
6. The method for detecting chloroform in a quantum dot solution according to claim 5, wherein the adhesive is one or two of urea resin and phenolic resin.
7. The method for detecting chloroform in a quantum dot solution as claimed in claim 5, wherein the method for preparing the glass with the surface covered with silver nitrate comprises the following steps:
providing a colorless and transparent adhesive;
and coating the adhesive on the surface of the glass substrate for testing, drying, and coating a silver nitrate solution on the surface of the adhesive to obtain the glass for testing with the surface covered with silver nitrate.
8. The method for detecting chloroform in a quantum dot solution according to any one of claims 4 to 7, wherein the glass substrate for testing is FTO glass or ITO glass.
9. The method for detecting chloroform in a quantum dot solution according to any one of claims 4 to 7, wherein the concentration of the silver nitrate solution is 1 to 50 mg/ml.
10. The method for detecting chloroform in a quantum dot solution as claimed in claim 1, wherein in the step of performing the first light irradiation treatment on the initial quantum dot solution, the first light irradiation treatment time is 10-30 min.
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Address after: 516006 TCL science and technology building, No. 17, Huifeng Third Road, Zhongkai high tech Zone, Huizhou City, Guangdong Province Applicant after: TCL Technology Group Co.,Ltd. Address before: 516006 Guangdong province Huizhou Zhongkai hi tech Development Zone No. nineteen District Applicant before: TCL RESEARCH AMERICA Inc. |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |