CN114752377A - Large-scale preparation method of high-temperature-resistant yellow-light carbon dots for LED - Google Patents
Large-scale preparation method of high-temperature-resistant yellow-light carbon dots for LED 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) the mixture obtained in the step (1) is pyrolyzed at the temperature of 200-250 ℃ and then ground 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 the main source of such pollution, which has an adverse effect 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 by evaluating some biological changes in human (152 total) and mouse models, indoor lighting using LEDs of golden yellow light can promote melatonin and glutamic acid secretion, protect eyes, accelerate healing and hair regeneration, improve sleep quality (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 the carbon dots are below 10nm in size, and the carbon dots 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 the rare earth luminescent material, the photoluminescent carbon dot has the advantages of easily available raw materials, lower preparation cost, environmental friendliness and biological friendliness. There are various methods for synthesizing carbon dots, including hydrothermal method (CN202110695392.8), solvothermal method, microwave method, ultrasonic method, plasma method, laser firing method, etc., 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: 274-. Carbon dots are generally not refractory and often exhibit fluorescence quenching at high temperatures. However, the LED device often has a high temperature when operating, and it is common practice to: the application of the Carbon dots on the LED devices is realized by coating other high-temperature resistant materials on the surfaces of the Carbon dots or manufacturing composite films (Carbon, 2022, 190: 22-31).
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) and (2) pyrolyzing the mixture obtained in the step (1) at the temperature of 200 ℃ and 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 step (1) is 1: 3: 0.2: (0.025-0.5): 50.
in the above technical scheme, further, the pyrolysis time in the step (2) is 4-6 h.
In the above technical scheme, further, the yellow emission color temperature is regulated and controlled by regulating and controlling the doping concentration of the silicon element and the nitrogen element in the carbon dots.
The invention also provides a yellow carbon dot prepared by the preparation method.
In another aspect, the invention provides an application of the carbon dots in preparing a yellow light LED device, and the carbon dots are encapsulated with a 470nm emitting LED chip to obtain the yellow light 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 spectrum of an emission spectrum (excitation wavelength: 470nm) of a yellow carbon dot 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 470nm) 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 from example 2;
FIG. 5 is a FI-IR spectrum of a yellow carbon dot obtained in 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 by a magnetic device until the solute is completely dissolved, the prepared solution is placed in a 210 ℃ oven for pyrolysis for 5 hours, and then ground for 30 minutes by a mortar, so that the yellow carbon dots 1 are obtained.
Example 2
Accurately weighing 2g of citric acid, 6g of boric acid, 0.2g of silicic acid and 0.2g of urea, mixing and grinding, then placing the mixture into a beaker, adding 100ml of deionized water, stirring for 2h through a magnetic device until the solute is completely dissolved, placing the prepared solution into an oven at 210 ℃ for pyrolysis for 5h, and then grinding for 30min by using a mortar to obtain the yellow carbon dot 2.
FIG. 7 is a mass balance diagram of carbon dot 2 prepared in one time in example 2, wherein the mass of an empty bottle is 11.5410g, and the weight of a bottle filled with carbon dot prepared in one time is 15.8746g, so that the mass of carbon dot prepared in one time is 4.3336 g.
The color coordinates of the carbon dot 2 obtained in example 2 are (0.40,0.55), the color temperature is 4274.46K, and the color rendering index is 37, as shown in FIG. 9.
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 for 2 hours through a magnetic device 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 the yellow carbon dot 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 for 2 hours through a magnetic device 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 carbon dots produced by the methods described in examples 1-4 are shown in Table 1.
TABLE 1 yield of yellow carbon dot samples
| Sample (I) | Yield of the product |
| 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 described in examples 1-4 are shown in Table 2.
TABLE 2 color temperature of yellow carbon dot samples
| Sample (I) | 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 5 min; 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 physical diagram of a yellow carbon dot LED is shown in FIG. 8.
Claims (6)
1. A preparation method of high-temperature-resistant yellow carbon dots is characterized by comprising 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) and (2) pyrolyzing the mixture obtained in the step (1) at the temperature of 200 ℃ and 250 ℃, and then grinding to obtain yellow carbon dots.
2. The preparation method according to claim 1, wherein the mass ratio of the citric acid, the boric acid, the silicic acid, the urea and the deionized water in the step (1) is 1: 3: 0.2: (0.025-0.5): 50.
3. the preparation method according to claim 1, wherein the pyrolysis time in the step (2) is 4-6 h.
4. The preparation method according to claim 1, wherein the yellow emission color temperature is controlled by controlling the doping concentrations of silicon and nitrogen in the carbon dots.
5. A yellow carbon dot produced by the production method according to any one of claims 1 to 4.
6. The use of the yellow carbon dot of claim 5, wherein the carbon dot is packaged with a 470nm emitting LED chip to obtain a yellow LED device.
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| CN116285973A (en) * | 2023-02-27 | 2023-06-23 | 大连海事大学 | Purple light carbon dot and preparation method and application thereof |
| CN116285973B (en) * | 2023-02-27 | 2024-02-20 | 大连海事大学 | Purple light carbon dot and preparation method and application thereof |
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