CN114752377B - Large-scale preparation method of high-temperature-resistant yellow-light carbon dots for LEDs - Google Patents
Large-scale preparation method of high-temperature-resistant yellow-light carbon dots for LEDs Download PDFInfo
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Abstract
The invention belongs to the technical field of luminescent materials, and particularly relates to a large-scale preparation method of a high-temperature-resistant yellow-light carbon dot for an LED. The method comprises the following steps: (1) Grinding the raw materials uniformly by using citric acid as a carbon source and boric acid, silicic acid and urea as doping agents, and dissolving the raw materials in deionized water; (2) Pyrolyzing the mixture obtained in the step (1) at 200-250 ℃, and then grinding to obtain yellow carbon dots. The yellow carbon dots prepared by the preparation method disclosed by the invention are high in yield, stable in luminescence and free of quenching in a solid aggregation state of the prepared carbon dots, and have a good high-temperature resistance characteristic. The preparation of the yellow LED device with low cost, low color temperature and strong penetration capability can be realized, and the preparation method has great market prospect in the field of yellow LED devices.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to a large-scale preparation method of a high-temperature-resistant yellow-light carbon dot for an LED.
Background
As a fourth generation lighting technology, LEDs are receiving wide attention in the industry due to their low power consumption and long service life. Light pollution has become a considerable problem in our daily lives, and artificial light sources of high color temperature are considered to be a major source of such pollution, which has adverse effects on human health. Compared with white light LEDs, yellow light LEDs with low color temperature have certain application prospects in certain special industrial and medical fields. In addition, yellow light has longer wavelength, better penetrability and stronger dispersion intensity, and is friendly to human eyes in dark environment. It is reported in the literature that indoor illumination using LEDs of gold yellow light can promote the secretion of melatonin and glutamic acid, protect eyes, accelerate healing and hair regeneration, and improve sleep quality by evaluating some biological changes in human (152 people in total) and mouse models (Scientfic Reports,2019, 7560). In addition, the golden yellow LED outdoor street lamp has the advantages of low color temperature, strong penetrating power, high lighting effect and long service life of the traditional high-pressure sodium lamp and the fluorescent LED street lamp. The emergence of yellow LEDs with high luminous efficiency will provide a new technical path for achieving LED illumination with no or little blue light, and will bring new vitality to LED illumination. Therefore, the yellow LED device with low cost and high luminous efficiency has wide application prospect (Acta Physica, 2019, 68-16).
The carbon dots are small-sized zero-dimensional carbon-based nano materials, most of which have the size below 10nm, and have potential application in the fields of industry, medical treatment, agriculture and the like. The carbon dot has the advantages of multicolor fluorescence, biocompatibility, water solubility, low toxicity and the like. Compared with rare earth luminescent materials, the photoluminescent carbon dots have the advantages of easily available raw materials, lower preparation cost, environmental friendliness and biological friendliness. There are various methods for synthesizing carbon dots, including a hydrothermal method (CN 202110695392.8), a solvothermal method, a microwave method, an ultrasonic method, a plasma method, a laser firing method, and the like, and the prepared carbon dots often exhibit excellent photoluminescence properties when dispersed in a liquid, and often exhibit luminescence quenching when aggregated as a solid (Journal of Colloid and Interface Science,2021, 598. Carbon dots are generally not refractory and often exhibit fluorescence quenching at high temperatures. However, the LED devices often have high temperature during operation, and the common practice is as follows: the application of the Carbon dots on the LED device is realized by coating other high-temperature resistant materials on the surfaces of the Carbon dots or manufacturing a composite film (Carbon, 2022, 190.
Disclosure of Invention
The invention aims to provide a method for quickly, efficiently and massively synthesizing yellow carbon dots, wherein the single yield can reach more than 4g, and the highest yield can reach more than 47%.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a preparation method of high-temperature-resistant yellow light carbon dots, which comprises the following steps:
(1) Grinding the raw materials uniformly by using citric acid as a carbon source and boric acid, silicic acid and urea as doping agents, and dissolving the raw materials in deionized water;
(2) Pyrolyzing the mixture obtained in the step (1) at 200-250 ℃, and then grinding to obtain yellow carbon dots.
In the above technical solution, further, the mass ratio of citric acid, boric acid, silicic acid, urea and deionized water in the step (1) is 1:3:0.2: (0.025-0.5): 50.
in the above technical solution, further, the pyrolysis time in the step (2) is 4 to 6 hours.
In the above technical scheme, further, the yellow emission color temperature is regulated and controlled by regulating and controlling the doping concentration of silicon element and nitrogen element in the carbon dots.
The invention also provides a yellow carbon dot prepared by the preparation method.
The invention further provides application of the carbon dots to preparation of a yellow light-emitting diode (LED) device, and the carbon dots and a 470nm emitting LED chip are packaged to obtain the yellow LED device.
The invention has the beneficial effects that:
the yellow carbon dots prepared by the preparation method disclosed by the invention are high in yield, stable in luminescence and free of quenching in a solid aggregation state of the prepared carbon dots, and have a good high-temperature resistance characteristic. The preparation of the yellow LED device with low cost, low color temperature and strong penetration capability can be realized, and the preparation method has great market prospect in the field of yellow LED devices.
Drawings
FIG. 1 is a graph showing the emission spectra (excitation wavelength: 470 nm) of the yellow carbon dots obtained in examples 1 to 4;
FIG. 2 is a graph showing the variation of the photoluminescence intensity of a yellow carbon dot obtained in example 2 with temperature (excitation wavelength: 470 nm);
FIG. 3 is a graph showing the change of luminous intensity with time (excitation wavelength is 470 nm) of the yellow carbon dots prepared in example 2 when placed in a natural environment;
FIG. 4 is an XRD pattern of yellow carbon dots made in example 2;
FIG. 5 is a FI-IR spectrum of a yellow carbon dot from example 2;
FIG. 6 is a TEM image of a yellow carbon spot obtained in example 2;
FIG. 7 is a mass balance diagram of a single preparation of carbon dot 2 of example 2;
FIG. 8 is a schematic diagram of a yellow carbon dot LED prepared in example 2;
FIG. 9 is a color coordinate diagram of a yellow carbon dot made in example 2.
Detailed Description
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
2g of citric acid, 6g of boric acid, 0.2g of silicic acid and 0.1g of urea are accurately weighed, mixed and ground, then placed in a beaker, added into 100ml of deionized water, stirred for 2 hours through a magnetic device until the solute is completely dissolved, the prepared solution is placed in an oven at 210 ℃ for pyrolysis for 5 hours, and then ground for 30 minutes by a mortar, so that yellow carbon dots 1 are obtained.
Example 2
2g of citric acid, 6g of boric acid, 0.2g of silicic acid and 0.2g of urea are accurately weighed, mixed and ground, then placed in a beaker, added into 100ml of deionized water, stirred for 2 hours through a magnetic device until the solute is completely dissolved, the prepared solution is placed in an oven at 210 ℃ for pyrolysis for 5 hours, and then ground for 30 minutes by a mortar, so that yellow carbon dots 2 are obtained.
FIG. 7 is a mass scale chart of carbon dots 2 of example 2 prepared in a single pass, with an empty bottle mass of 11.5410g and a bottle weight of 15.8746g containing carbon dots prepared in a single pass, so that the carbon dots prepared in a single pass have a mass of 4.3336g.
The color coordinates of the carbon dot 2 obtained in example 2 are shown in FIG. 9, and the color coordinates are (0.40, 0.55), the color temperature is 4274.46K, and the color rendering index is 37.
Example 3
Accurately weighing 2g of citric acid, 6g of boric acid, 0.2g of silicic acid and 0.5g of urea, mixing and grinding, then placing the mixture into a beaker, adding 100ml of deionized water, stirring by a magnetic device for 2 hours until the solute is completely dissolved, placing the prepared solution into an oven at 210 ℃ for pyrolysis for 5 hours, and then grinding for 30 minutes by using a mortar to obtain yellow carbon dots 3.
Example 4
Accurately weighing 2g of citric acid, 6g of boric acid, 0.2g of silicic acid and 1g of urea, mixing and grinding, then placing the mixture into a beaker, adding 100ml of deionized water, stirring by a magnetic device for 2 hours until the solute is completely dissolved, placing the prepared solution into an oven at 210 ℃ for pyrolysis for 5 hours, and then grinding for 30 minutes by using a mortar to obtain yellow carbon dots 4.
The yields of yellow dots produced by the methods of preparation described in examples 1-4 are shown in Table 1.
TABLE 1 yield of yellow carbon dot samples
| Sample (I) | Yield of |
| Example 1 | 35.40％ |
| Example 2 | 34.33％ |
| Example 3 | 36.80％ |
| Example 4 | 47.10％ |
The color temperatures of the yellow carbon dots prepared by the methods of examples 1-4 are shown in Table 2.
TABLE 2 color temperature of yellow carbon dot samples
| Sample(s) | Color temperature |
| Example 1 | 3566.60K |
| Example 2 | 4274.46K |
| Example 3 | 4437.77K |
| Example 4 | 4209.91K |
Example 5
The yellow carbon dot 2 prepared in example 2 was packaged with a commercially available 470nm emitting LED chip to obtain a yellow LED device:
LED packaging: weigh 0.05g of carbon dots on an electronic balance and weigh 0.25g of glue A and 1g of glue B. And stirring the weighed glue A for 2min, then adding CDs, and stirring and mixing uniformly. Adding the weighed B glue into the mixture of the A glue and the CDs, and stirring and mixing the mixture uniformly for 5min; then, defoaming was performed by using low-frequency ultrasonic waves. Dipping the defoamed mixture, dispensing the mixture on an LED substrate support, putting the dispensed LED into an oven, baking for 40min at 60 ℃, and then baking for 110min at 135 ℃ to obtain the packaged yellow LED device.
A schematic diagram of a yellow carbon dot LED is shown in FIG. 8.
Claims (4)
1. A preparation method of high-temperature-resistant yellow carbon dots is characterized by comprising the following steps:
(1) The method comprises the following steps of taking citric acid as a carbon source, taking boric acid, silicic acid and urea as doping agents, uniformly grinding the raw materials, and dissolving the raw materials in deionized water, wherein the mass ratio of the citric acid to the boric acid to the silicic acid to the urea to the deionized water is 1:3:0.2: (0.025-0.5): 50;
(2) Pyrolyzing the mixture obtained in the step (1) at 200-250 ℃ for 4-6 h, and then grinding to obtain yellow carbon dots.
2. The preparation method according to claim 1, wherein the yellow emission color temperature is controlled by controlling the doping concentrations of the silicon element and the nitrogen element in the carbon dots.
3. A yellow carbon dot produced by the production method according to any one of claims 1 to 2.
4. The use of the yellow carbon dot of claim 3, wherein the carbon dot is packaged with a 470nm emitting LED chip to obtain a yellow LED device.
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