CN104531146B - The preparation method of the adjustable BCNO fluorescent powder of a kind of orange red light emission - Google Patents
The preparation method of the adjustable BCNO fluorescent powder of a kind of orange red light emission Download PDFInfo
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Abstract
The present invention is the preparation method of the adjustable BCNO fluorescent powder of a kind of orange red light emission, the method comprises the following steps: step 1: boric acid and α-alanine are put into baking oven and carries out heat pre-treatment, Heating temperature is 110 ~ 130 DEG C, heat-up time is 4-6 hour, naturally cools to room temperature after having heated; Step 2: the boric acid after heat pre-treatment and α-alanine are put into reactor immediately, then add deionized water then 40 ~ 60 DEG C stir 4 ~ 6 hours; Then solution temperature is increased to 110 ~ 130 degree, until by water evaporate to dryness, obtains the precursor of BCNO; Step 3: sinter 8 ~ 24 hours at the BCNO precursor upper step prepared is warming up to 600 ~ 700 DEG C, naturally cool to room temperature and namely obtain the adjustable BCNO fluorescent powder of orange red light emission.This invention only needs two kinds of raw materials, by liquid phase method synthesis BCNO precursor, then adopts low-temperature sintering to prepare orange red light emission BCNO fluorescent powder.
Description
Technical field
The invention belongs to technical field of function materials, more particularly, relate to the preparation method that low-temperature sintering prepares the adjustable BCNO of orange red light emission (boron carbon nitrogen oxygen) fluorescent material.
Background technology
Current phosphor material powder is mostly with rare earth element (Eu
2+, Ce
3+deng) luminous as activator; not only expensive, synthesis temperature higher (more than 900 DEG C), needs protective atmosphere (nitrogen or argon gas) or reducing atmosphere (hydrogen) sintering; and the toxicity of rare earth chloride is comparatively large, serious environment pollution.Red-light fluorescent powder has widespread use in fields such as white light LEDs, display, biomedicines, and the fluorescent material of current red emission mostly is the sulfide (Ca/SrS:Eu of Eu doping
2+), not only price is held high, and has certain toxicity, and the sulfide very easily moisture absorption, unstable properties.BCNO is a kind of fluorescent material of non-rear-earth-doped luminescence, because it does not need rare earth element to cause the extensive concern of people as activator.BCNO fluorescent powder has preparation temperature lower (700 ~ 900 DEG C), the many merits such as (visible-ranges) that do not need that protective atmosphere sinters (namely realizing sintering in atmosphere), energy-conserving and environment-protective, excitation spectrum wide ranges (from ultraviolet to blue light), emmission spectrum is adjustable, has broad application prospects in fields such as White-light LED illumination and display, fluorescein, bioluminescence imaging, DNA marker and medical science.At present, people have prepared blue emission and yellowish green photoemissive BCNO fluorescent powder, and the report of orange red light emission BCNO fluorescent powder is little, unique report is also that we adopt boric acid, trimeric cyanamide and glycerol to be raw material, adopts liquid phase method to synthesize the BCNO fluorescent powder of wide excitation and emission spectra (emission peak is adjustable at 450 to 630nm).In addition, the preparation of BCNO fluorescent powder mostly needs three kinds of raw materials, and general boric acid or the boron trioxide of adopting does boron source, and nitrogenous source made by urea or trimeric cyanamide, the organism of carbon containing prepares BCNO fluorescent powder as carbon source, and needs to regulate emmission spectrum scope by changing carbon source content.Only use the emmission spectrum of the BCNO fluorescent powder of boron source and nitrogenous source two kinds of Material synthesis substantially at blue wave band at present, yet there are no the report of the orange red light emission BCNO fluorescent powder of employing two kinds of Material synthesis.In addition, people generally adopt urea combustion, and (sintering temperature is 700 ~ 900 DEG C, sintering time is 30 ~ 120 minutes) synthesis BCNO fluorescent powder, although the method technique is simple, but the controllability of the method is poor, and sintering time has a significant impact emmission spectrum, sintering time difference several minutes can cause the deviation of emmission spectrum tens nanometer, can ammonia be produced during Urea simultaneously, thus can environmental pollution be caused.Therefore, urea combustion is unfavorable for green syt and the industrial application of BCNO fluorescent powder.
Summary of the invention
The object of the invention is to for comparing shortage in current phosphor material powder system, and be substantially all rear-earth-doped and problem that is that glow, the preparation method of the adjustable BCNO fluorescent powder of a kind of orange red light emission is provided, the method only adopts boric acid and L-Ala (α-alanine) two kinds of raw materials, utilize the chemical structure of L-Ala, special chemical key forms, and suitable carbon, nitrogen ratio, first the precursor of BCNO is synthesized by liquid phase method, then orange red photoemissive BCNO fluorescent powder is prepared at the retort furnace low temperature sintering precursor of unprotect atmosphere, overcome in current techniques and use three kinds of raw materials to synthesize BCNO fluorescent powder (if only go to regulate emmission spectrum without carbon source with two kinds of raw materials, its emmission spectrum is substantially at blue wave band.), both avoided the use of urea, raw material type is few, there is good controllability, be applicable to batch production and industrial application, and adopt L-Ala to be that carbon nitrogen source has synthesized the adjustable BCNO fluorescent powder of orange red light emission first, further expand orange red light emission phosphor material powder system.
Technical scheme of the present invention is:
A preparation method for BCNO fluorescent powder that orange red light emission is adjustable, comprises the following steps:
Step 1: boric acid and α-alanine are put into baking oven in proportion and carries out heat pre-treatment, Heating temperature is 110 ~ 130 DEG C, and heat-up time is 4-6 hour, naturally cools to room temperature after having heated; Wherein, molar ratio of material is boric acid: α-alanine=1:1 ~ 10;
Step 2: the boric acid after heat pre-treatment and α-alanine are put into reactor immediately, then add deionized water boric acid and α-alanine are dissolved, then 40 ~ 60 DEG C are stirred 4 ~ 6 hours; Then solution temperature is increased to 110 ~ 130 degree, until by water evaporate to dryness, obtains the precursor of BCNO;
Step 3: sinter at the BCNO precursor upper step prepared is warming up to 600 ~ 700 DEG C, temperature rise rate is per minute 5 degree, and sintering time is 8 ~ 24 hours, naturally cools to room temperature after terminating; Finally the product taken out is ground 30 ~ 60 minutes, obtain the adjustable BCNO fluorescent powder of orange red light emission.
Described solution stirring is induction stirring or mechanical stirring, stirring at low speed, and rotating speed is 50 ~ 100 revs/min.
Utilize BCNO fluorescent powder prepared by technical scheme of the present invention, carry out X-ray diffraction (X-ray diffractometer (RigakuUltimaIV), sweep limit is 10 – 80 degree, scanning speed is 2 degree/point, scanning step is 0.02 degree), scanning electron microscope (scanning electron microscope (Hitachi, S-4800)), x-ray photoelectron power spectrum (x-ray photoelectron spectroscopy (PHI1600EXCA)), infrared spectra (Fourier transform infrared spectroscopy (Bruker, WQF-410), test specification is 400 to 2000 wave numbers) and emmission spectrum (fluorescence spectrophotometer (Hitachi, F-7000), exciting light is the monochromatic ray of 370nm, emmission spectrum test specification is 390-720nm) performance test, known: the structure of BCNO fluorescent powder is staggered floor BN hexagonal structure, and containing a small amount of boron trioxide in sample.The pattern of sample is irregular, and particle size at several microns to 100 microns, and exists B, C, N, O tetra-kinds of elements, containing chemical bonds such as B-N, B-N-B, B-O, B-C, C-C, C-H.The emmission spectrum of the BCNO fluorescent powder of preparation, in orange red optical band, can make the emmission spectrum of BCNO fluorescent powder adjustable in orange red optical band by regulating material rate.
The invention provides a kind of preparation method of orange red light emission BCNO fluorescent powder, can supplement and substitute current red-light fluorescent powder (as Ca/SrS:Eu as a kind of orange red-light fluorescent powder newly
2+deng).This invention only needs two kinds of raw materials, first by liquid phase method synthesis BCNO precursor, then adopts low-temperature sintering precursor (600-700 degree) to prepare orange red light emission BCNO fluorescent powder.The synthesis of current BCNO fluorescent powder substantially all needs three kinds of raw materials, boron source, nitrogenous source and carbon source respectively, if the emission wavelength of the BCNO fluorescent powder not having carbon source to synthesize is at blue wave band, and by regulating carbon source kind and content to regulate the emission wavelength of BCNO fluorescent powder also can only be adjusted to yellow green light wave band, there be limited evidence currently of has the report of red emission BCNO fluorescent powder, unique report is that we adopt boric acid to be boron source, trimeric cyanamide is nitrogenous source, and glycerol is that the wide of carbon source synthesis excites the BCNO fluorescent powder with wide emmission spectrum.The present invention adopts α-alanine simultaneously as nitrogenous source and carbon source, and boric acid is that the adjustable BCNO fluorescent powder of orange red light emission has been synthesized in boron source.The raw materials used cheap and nontoxic pollution-free of this invention, equipment used and processing method simple.In addition, this method avoid the use of urea, more energy-conserving and environment-protective.This orange red light emission BCNO fluorescent powder does not need rare earth doped and luminous, has enriched red-light fluorescent powder material system further, compensate for the present situation that current red-light fluorescent powder lacks.BCNO fluorescent powder emission peak positions prepared by the present invention can regulate in orange red optical band along with material rate, through the test of follow-up thermal treatment process and repeated experiment research, find that orange red light emission BCNO fluorescent powder prepared by the present invention has good thermostability and process repeatability, be very beneficial for industrial mass manufacture.
Accompanying drawing explanation
The X-ray diffractogram of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that Fig. 1 is embodiment 3 and 13 mesoboric acid and α-alanine when being 1:1 and 1:10.
The scanning electron microscope (SEM) photograph of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that Fig. 2 is embodiment 3 mesoboric acid and α-alanine when being 1:1.
The x-ray photoelectron energy spectrogram of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that Fig. 3 is embodiment 3 mesoboric acid and α-alanine when being 1:1.
The infrared absorpting light spectra of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that Fig. 4 is embodiment 3 and 13 mesoboric acid and α-alanine when being 1:1 and 1:10.
Fig. 5 is embodiment 1-4 mesoboric acid and α-alanine when being 1:1, and differing temps sinters the utilizing emitted light spectrogram of the BCNO fluorescent powder of preparation in 12 hours.
The utilizing emitted light spectrogram of BCNO fluorescent powder prepared by 650 degree of sintering different times that Fig. 6 is embodiment 5-8 mesoboric acid and α-alanine when being 1:1.
The utilizing emitted light spectrogram of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that Fig. 7 is embodiment 9-13 mesoboric acid and α-alanine when being different ratios.
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1: prepare orange light emission BCNO fluorescent powder under different sintering temperature.
Step 1: weigh boric acid (0.02mol) and α-alanine (0.02mol) according to chemical mol ratio 1:1, load weighted boric acid and α-alanine are put into baking oven and carries out heat pre-treatment, Heating temperature is 120 degree, heat-up time is 4 hours, naturally cools to room temperature after having heated;
Step 2: the boric acid after heat pre-treatment and α-alanine are put into beaker, then (amount of deionized water is for can make boric acid and α-alanine dissolve completely to add 30 ml deionized water, here for convenience of experiment, choose 30 milliliters, and (induction stirring, rotating speed is 80 revs/min to carry out heated and stirred.), Heating temperature is 50 DEG C, and the Keep agitation time is 4 hours; Then solution temperature is increased to 120 degree, until by complete for water evaporate to dryness, obtain the precursor of BCNO;
Step 3: the BCNO precursor upper step prepared puts into alumina crucible, alumina crucible is put into retort furnace and sinters, retort furnace rises to 600 DEG C with the temperature rise rate of per minute 5 degree.Sinter 12 hours at such a temperature.Terminate rear closedown retort furnace and naturally cool to room temperature.Finally the sample of taking-up is ground and within 40 minutes, namely obtain orange light emission BCNO fluorescent powder.
Embodiment 2,
Other steps are with embodiment 1, and difference is that the sintering temperature in step 3 changes 625 degree into by 600 degree.
Embodiment 3,
Other steps are with embodiment 1, and difference is that the sintering temperature in step 3 changes 650 degree into by 600 degree.
Embodiment 4,
Other steps are with embodiment 1, and difference is that the sintering temperature in step 3 changes 700 degree into by 600 degree.
Test result: adopt low-temperature sintering precursor to prepare BCNO fluorescent powder at different temperatures, X-ray diffraction, scanning electron microscope, x-ray photoelectron power spectrum, infrared spectra and emission spectroscopy measurements have been carried out to fluorescent material, test result respectively as shown in Figure 1, Figure 2, shown in Fig. 3, Fig. 4 and Fig. 5.The X-ray diffractogram of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that Fig. 1 is boric acid and α-alanine when being 1:1 and 1:10, there are two wider diffraction peaks in sample near 26 degree and 43 degree, by comparing (PDF#45-0895) with standard P DF card, show that the structure of BCNO fluorescent powder is staggered floor BN hexagonal structure; And sample exists sharp-pointed diffraction peak near 33,44 degree, 58 degree and 62 degree, by comparing (PDF#06-0634) with standard P DF card, show in the sample prepared containing a small amount of boron trioxide.The scanning electron microscope (SEM) photograph of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that Fig. 2 is boric acid and α-alanine when being 1:1, result shows that the pattern of sample is irregular, and particle size is at 5 microns to 100 microns.The x-ray photoelectron energy spectrogram of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that Fig. 3 is boric acid and α-alanine when being 1:1, result shows that sample exists B, C, N, O tetra-kinds of elements.The infrared absorpting light spectra of the BCNO fluorescent powder of 650 degree of sintering preparation in 12 hours that what Fig. 4 provided is boric acid and α-alanine when being 1:1 and 1:10, as seen from Figure 4, containing chemical bonds such as B-N, B-N-B, B-O, B-C, C-C, C-H in BCNO fluorescent powder.By analyzing above 4 figure, can show that the fluorescent material of preparation is made up of B, C, N, O, sample is staggered floor BN hexagonal structure, and there is chemical bond between each element.Fig. 5 is boric acid the utilizing emitted light spectrogram of BCNO fluorescent powder under 370nm excites that prepared by different sintering temperature when being 1:1 with α-alanine, as shown in Figure 5, the emmission spectrum of fluorescent material is in yellow orange optical band, emission peak positions is near 570nm, and emission peak positions is along with the rising slightly red shift of sintering temperature, but intensity of emission spectra is along with the rising first increases and then decreases of sintering temperature, when sintering temperature is 650 degree, the intensity of emission spectra of BCNO fluorescent powder is the strongest, by changing 6 times that sintering temperature can make optimum transmit spectral intensity reach original.In addition, because our sample sintering time is all long, sintering time differs within 20 minutes and does not substantially have an impact to spectrum, and the BCNO fluorescent powder that therefore prepared by the method has satisfactory stability and repeatability.
Embodiment 5: prepare orange light emission BCNO fluorescent powder under different sintering time.
Step 1: weigh boric acid (0.02mol) and α-alanine (0.02mol) according to chemical mol ratio 1:1, load weighted boric acid and α-alanine are put into baking oven and carries out heat pre-treatment, Heating temperature is 120 degree, heat-up time is 5 hours, naturally cools to room temperature after having heated;
Step 2: the boric acid after heat pre-treatment and α-alanine are put into beaker, then adds 30 ml deionized water, and carries out heated and stirred, and Heating temperature is 60 DEG C, and the Keep agitation time is 5 hours; Then solution temperature is increased to 120 degree, until by complete for water evaporate to dryness, obtain the precursor of BCNO;
Step 3: the BCNO precursor upper step prepared puts into alumina crucible, alumina crucible is put into retort furnace and sinters, retort furnace rises to 650 DEG C with the temperature rise rate of per minute 5 degree.Sinter 8 hours at such a temperature.Terminate rear closedown retort furnace and naturally cool to room temperature.Finally the sample of taking-up is ground and within 40 minutes, namely obtain orange light emission BCNO fluorescent powder.
Embodiment 6,
Other steps are with embodiment 5, and difference is that the sintering time in step 3 changed 12 hours into by 8 hours.
Embodiment 7,
Other steps are with embodiment 5, and difference is that the sintering time in step 3 changed 16 hours into by 8 hours.
Embodiment 8,
Other steps are with embodiment 5, and difference is that the sintering time in step 3 changed 24 hours into by 8 hours.
Test result: utilize low-temperature sintering precursor to adopt different sintering time (650 DEG C of sintering) to prepare orange light emission BCNO fluorescent powder, X-ray diffraction, scanning electron microscope, x-ray photoelectron power spectrum, infrared spectra and emission spectroscopy measurements have been carried out to fluorescent material.Fig. 6 is boric acid and α-alanine the utilizing emitted light spectrograms of BCNO fluorescent powder under 370nm excites that prepared by 650 degree of sintering different times when being 1:1.As shown in Figure 6, in 8-24 hours window, the emmission spectrum of this fluorescent material is in yellow orange optical band, emission peak positions is near 570nm, and emission peak positions along with the increase of sintering time substantially constant, but intensity of emission spectra first raises rear reduction along with the increase of sintering time, when sintering time is 12 hours, the intensity of emission spectra of BCNO fluorescent powder is the strongest, by changing 3 times that sintering time can make optimum transmit spectral intensity reach original.
Embodiment 9: prepare orange red light emission BCNO fluorescent powder when the boric acid of different mol ratio and α-alanine.
Step 1: weigh boric acid and α-alanine according to chemical mol ratio 1:1, boric acid is fixed on 0.02mol, load weighted boric acid and α-alanine is put into baking oven and carries out heat pre-treatment, and Heating temperature is 120 degree, heat-up time is 6 hours, naturally cools to room temperature after having heated;
Step 2: the boric acid after heat pre-treatment and α-alanine are put into beaker, then adds 40 ml deionized water, and carries out heated and stirred, and Heating temperature is 60 DEG C, and the Keep agitation time is 5 hours; Then solution temperature is increased to 120 degree, until by complete for water evaporate to dryness, obtain the precursor of BCNO;
Step 3: the BCNO precursor upper step prepared puts into alumina crucible, alumina crucible is put into retort furnace and sinters, retort furnace rises to 650 DEG C with the temperature rise rate of per minute 5 degree.Sinter 12 hours at such a temperature.Terminate rear closedown retort furnace and naturally cool to room temperature.Finally the sample of taking-up is ground and within 40 minutes, namely obtain orange light emission BCNO fluorescent powder.
Embodiment 10,
Other steps are with embodiment 9, and difference is that the mol ratio of boric acid in step 1 and α-alanine makes 1:3 into by 1:1.
Embodiment 11,
Other steps are with embodiment 9, and difference is that the mol ratio of boric acid in step 1 and α-alanine makes 1:5 into by 1:1.
Embodiment 12,
Other steps are with embodiment 9, and difference is that the mol ratio of boric acid in step 1 and α-alanine makes 1:8 into by 1:1.
Embodiment 13,
Other steps are with embodiment 9, and difference is that the mol ratio of boric acid in step 1 and α-alanine makes 1:10 into by 1:1.
Test result: adopt the boric acid of different mol ratio and α-alanine (650 degree sintering 12 hours) to prepare orange red light emission BCNO fluorescent powder, X-ray diffraction, scanning electron microscope, x-ray photoelectron power spectrum, infrared spectra and emission spectroscopy measurements have been carried out to fluorescent material.Fig. 7 is the normalized emission spectrogram of BCNO fluorescent powder under 370nm excites adopting the boric acid of different mol ratio and α-alanine to prepare.As shown in Figure 7, mol ratio emmission spectrum scope of this fluorescent material within the scope of 1:1-1:10 of boric acid and α-alanine is adjustable in orange red optical range, and emission peak positions increases by 570nm red shift to 610nm along with the mol ratio of boric acid and α-alanine.From utilizing emitted light spectrogram, the emmission spectrum of the BCNO fluorescent powder that we prepare for raw material with boric acid and α-alanine really in orange red optical band, and can regulate the emmission spectrum scope of BCNO fluorescent powder easily by the mol ratio changing boric acid and α-alanine.
According to above result, can find out that method that the present invention proposes avoids the use of urea, at lower temperature (600 ~ 700 DEG C), adopt low-temperature sintering to prepare the adjustable BCNO fluorescent powder of orange red light emission, and overcome urea combustion and prepare the deficiency of BCNO fluorescent powder to sintering time sensitivity.In addition, raw material can be made fully to mix by liquid phase heated and stirred and improve the homogeneity and controllability of reacting, being easy to batch production.The present invention determines the processing condition of orange red light emission BCNO fluorescent powder by the mol ratio changing sintering temperature, sintering time and boric acid and α-alanine.
Above to invention has been exemplary description; should be noted that; when not departing from core of the present invention, any simple distortion, amendment or other those skilled in the art can not spend the equivalent replacement of creative work all to fall into protection scope of the present invention.
Unaccomplished matter of the present invention is known technology.
Claims (2)
1. a preparation method for BCNO fluorescent powder, is characterized by and comprise the following steps:
Step 1: boric acid and α-alanine are put into baking oven in proportion and carries out heat pre-treatment, Heating temperature is 110 ~ 130 DEG C, and heat-up time is 4-6 hour, naturally cools to room temperature after having heated; Wherein, molar ratio of material is boric acid: α-alanine=1:1 ~ 10;
Step 2: the boric acid after heat pre-treatment and α-alanine are put into reactor immediately, then add deionized water boric acid and α-alanine are dissolved, then 40 ~ 60 DEG C are stirred 4 ~ 6 hours; Then solution temperature is increased to 110 ~ 130 degree, until by water evaporate to dryness, obtains the precursor of BCNO;
Step 3: sinter at the BCNO precursor upper step prepared is warming up to 600 ~ 700 DEG C, temperature rise rate is per minute 5 degree, and sintering time is 8 ~ 24 hours, naturally cools to room temperature after terminating; Finally the product taken out is ground 30 ~ 60 minutes, obtain the adjustable BCNO fluorescent powder of orange red light emission.
2. the preparation method of BCNO fluorescent powder as claimed in claim 1, the stirring that it is characterized by described solution is induction stirring or mechanical stirring, stirring at low speed, and rotating speed is 50 ~ 100 revs/min.
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