CN103450876B - Inorganic oxide coated fluorescent powder and preparation method thereof - Google Patents
Inorganic oxide coated fluorescent powder and preparation method thereof Download PDFInfo
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- CN103450876B CN103450876B CN201310419671.7A CN201310419671A CN103450876B CN 103450876 B CN103450876 B CN 103450876B CN 201310419671 A CN201310419671 A CN 201310419671A CN 103450876 B CN103450876 B CN 103450876B
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Abstract
The invention discloses inorganic oxide coated fluorescent powder and a preparation method thereof. A surface coating layer of the inorganic oxide-coated fluorescent powder contains any one or two or three of silicon oxide, magnesium oxide and aluminum oxide, and is prepared by adopting the following method: (1), according to the type of an inorganic oxide, selecting tetraethyl orthosilicate, a soluble magnesium salt and a soluble aluminum salt to prepare liquor A; (2), firstly adjusting pH value to 1-2 by using strong acid, and then adjusting pH value to 5-7 by using weak base to obtain liquor B; (3), adding urea and fluorescent powder into the mixed liquor B, reacting to obtain slurry C containing the fluorescent powder, carrying out solid-liquid separation after cooling, washing and drying to obtain powder; (4), roasting the dried powder for 0.1 hour -6 hours to obtain the inorganic oxide-coated fluorescent powder. The coating layer is uniform, continuous, compact, firm, and small in thickness, and does not lose luminous intensity. Hydrolysis of the fluorescent powder can be restrained by utilizing tetraethyl orthosilicate, so that a defect that the fluorescent powder is easy to hydrolyze and becomes ineffective is overcome.
Description
Technical field
The invention belongs to field of material technology, be specifically related to a kind of inorganic oxide encapsulated phosphor and preparation method thereof.
Background technology
After certain material is excited (ray, high energy particle, electron beam, external electric field etc.), material will be in excited state, and the energy of excited state can be discharged by the form of light or heat.If this part energy is positioned at visible, ultraviolet or near infrared electromagnetic radiation, this process is luminescence process.The material that can realize luminescence process is called luminescent material, and a class pressed powder is wherein fluorescent material again.Fluorescent material is the high added value functional materials being widely used in the fields such as illumination, display, detection, mark.Along with popularizing of energy-conserving light source and large screen display device, fluorescent material industry achieves lasting high growth in recent years.The very big concern that research and development luminous efficiency is high, cause people with application matching is good, purity of color is high, physicochemical property are stable fluorescent material.
At present, in use mainly there is following problem in fluorescent material.(1) irradiation deterioration: refer to that fluorescent material is in use subject to the bombardment of energetic ray or particle, the microenvironment of internal structure and luminescence center changes, thus cause the phenomenon of fluorescent material performance degradation, be embodied in brightness decay, chroma offset etc., cause the decay in application life-span.(2) thermal degradation when: through high bake or calcining process, the luminescence center of part fluorescent material is oxidized or occur microstructure change, also the deterioration of fluorescent material performance can be caused, show as brightness decay, chroma offset etc. equally, reduce the performance of fluorescent material goods, and limit the range of application of fluorescent material.(3) chemical stability: refer to that some fluorescent material easily decompose in water or when being heated, cause brightness decay or inefficacy.(4) dispersed and screening characteristics: fluorescent material in water or slurrying time, due to surface electrical behavior, dispersed very poor, easily to assemble, sedimentation, cause coating homogeneity bad, have impact on optical homogeneity and the consistence of application device.
Carry out Surface coating to fluorescent material to be considered to solve or improve the effective way of the problems referred to above; regulate and control the surface electrical behavior of fluorescent material on the one hand, improve powder surface damage; improve dispersiveness and the coating homogeneity of fluorescent material; thus improve optical homogeneity and the consistence of device; on the other hand fluorescent material and the external world are kept apart; available protecting fluorescent material, reduces extraneous factor to the impact of fluorescent material, extends the work-ing life of fluorescent material.According to the chemical composition of coated rete, can be divided into Coated with Organic Matter and inorganics coated; According to cladding process method, physical package coating technique (dry method solid phase) and chemical packs coating technique (wet method liquid phase or gas phase) can be divided into.Although Coated with Organic Matter can significantly improve fluorescent material in water or slurrying time dispersiveness, but in the deterioration of reduction irradiation and thermal degradation when, raising chemical stability etc. DeGrain; Often there is coating layer and the defect of fluorescent material in conjunction with the fine and close coating layer of insecure, more difficult formation in physical package coating technique; The dependency of gas phase cladding to equipment and the energy is higher, and technique is more complicated; Usual liquid phase method easily causes coating to be reunited, and make coating layer uneven, or coating layer is too thick, causes luminescent properties to decline, and aqueous medium also can cause the hydrolysis of some fluorescent material.
Summary of the invention
The present invention seeks to for the deficiencies in the prior art, adopt chemical process at phosphor surface coated inorganic oxide compound, the out-phase homogeneous nucleation of coating is utilized to realize evenly coated, realize controlled coated and reduce coating thickness by controlling speed of response, the hydrolysis of Fluorophotometry powder simultaneously, coating layer evenly, continuously, fine and close, firm, thickness is thin, do not lose luminous intensity.
For achieving the above object, adopt technical scheme as follows:
A kind of inorganic oxide encapsulated phosphor, its surface coating layer containing silica, magnesium oxide, aluminum oxide any one or any two or three, adopt and prepare with the following method:
1) kind of inorganic oxide contained by above-mentioned coating layer, select tetraethoxy, solubility magnesium salts, aluminum soluble salt to prepare solution A, solvent is the mixed solution of water or water and ethanol;
2) first use strong acid adjust ph to 1 ~ 2, then obtain solution B with weak base adjust ph to 5 ~ 7; Described strong acid is sulfuric acid, hydrochloric acid or nitric acid; Described weak base is ammoniacal liquor, volatile salt or bicarbonate of ammonia;
3) in mixing solutions B, add urea and fluorescent material, at the temperature of 80 ~ 120 DEG C, reaction 0.1 ~ 6 hour, obtains the slurry C containing fluorescent material, solid-liquid separation after cooling, washs and dry to obtain powder;
4) within 0.1 ~ 6 hour, inorganic oxide encapsulated phosphor is obtained by drying the temperature lower calcination of powder at 300 ~ 700 DEG C.
By such scheme, when solvent is the mixed solution of water and ethanol, water: ethanol contend is than being 20:1 ~ 1:3.
By such scheme, described tetraethoxy, solubility magnesium salts, aluminum soluble salt are by the Mass Calculation of corresponding metal oxide, and corresponding silicon oxide, magnesium oxide, aluminum oxide consumption are 0 ~ 15% of fluorescent material consumption; The total mass of three kinds of oxide compounds is 0.1 ~ 15% of fluorescent material quality.
By such scheme, the consumption of described urea is 3 ~ 20 times of metallic element integral molar quantity in solution A.
By such scheme, in described calcination process, the fluorescent material bad or easily oxidized for thermostability in oxidizing atmosphere, selects to calcine in reducing atmosphere; Reducing atmosphere uses carbon heat or uses nitrogen and hydrogen mixture.
By such scheme, for the fluorescent material that hydrolysis easily occurs, during preparation solution A, add tetraethoxy.
By such scheme, the preparation method of described inorganic oxide encapsulated phosphor, comprises the following steps:
1) kind of inorganic oxide contained by above-mentioned coating layer, select tetraethoxy, solubility magnesium salts, aluminum soluble salt to prepare solution A, solvent is the mixed solution of water or water and ethanol;
2) first use strong acid adjust ph to 1 ~ 2, then obtain solution B with weak base adjust ph to 5 ~ 7; Described strong acid is sulfuric acid, hydrochloric acid or nitric acid; Described weak base is ammoniacal liquor, volatile salt or bicarbonate of ammonia;
3) in mixing solutions B, add urea and fluorescent material, at the temperature of 80 ~ 120 DEG C, reaction 0.1 ~ 6 hour, obtains the slurry C containing fluorescent material, solid-liquid separation after cooling, washs and dry to obtain powder;
4) within 0.1 ~ 6 hour, inorganic oxide encapsulated phosphor is obtained by drying the temperature lower calcination of powder at 300 ~ 700 DEG C.
By such scheme, when solvent is the mixed solution of water and ethanol, water: ethanol contend is than being 20:1 ~ 1:3; Described tetraethoxy, solubility magnesium salts, aluminum soluble salt are by the Mass Calculation of corresponding metal oxide, and corresponding silicon oxide, magnesium oxide, aluminum oxide consumption are 0 ~ 15% of fluorescent material consumption; The total mass of three kinds of oxide compounds is 0.1 ~ 15% of fluorescent material quality; The consumption of described urea is 3 ~ 20 times of metallic element integral molar quantity in solution A.
By such scheme, in described calcination process, the fluorescent material bad or easily oxidized for thermostability in oxidizing atmosphere, selects to calcine in reducing atmosphere; Reducing atmosphere uses carbon heat or uses nitrogen and hydrogen mixture.
By such scheme, for the fluorescent material that hydrolysis easily occurs, during preparation solution A, add tetraethoxy.
When hydrolysis easily occurs prepared fluorescent material, add the technique effect that tetraethoxy can produce the hydrolysis of Fluorophotometry powder.Reason is that tetraethoxy is hydrolyzed in acid condition, then aggregates into the network-like polymkeric substance with hydroxyl and oxyethyl group in the basic conditions.First the pH value of the mixing solutions of tetraethoxy and water, alcohol is adjusted to 1 ~ 2, impels tetraethoxy to be hydrolyzed fast, fully; Again pH value is adjusted to the slightly acidic of 5 ~ 7, the acidolysis of fluorescent material when avoiding it to mix with fluorescent material; Add fluorescent material and urea in reaction system after; the even hydrolysis reaction of urea is utilized pH value to be adjusted to the weakly alkaline of 7 ~ 8; promote the polymerization of teos hydrolysis product; according to heterogeneous nucleation principle; network-like polymerisate is wrapped in phosphor surface; form layer protecting film, the hydrolysis of Fluorophotometry powder.
Utilize urea even hydrolysis reaction under certain condition and the heterogeneous nucleation principle of precipitation, obtain the inorganic oxide rete of uniformly continous, compact and firm at phosphor surface, the rete overcoming general Physical coating technology and fluorescent material to distribute discontinuous uneven defect in conjunction with insecure, other chemical method coating technology retes.
Beneficial effect of the present invention:
1) the present invention is by the control to conditions such as reaction times, covering amount, initial concentration, amount of urea, the effective control to thicknesses of layers can be realized, while acquisition uniformly continous, the coated rete of compact and firm, coating film layer thickness can also be reduced, to avoid the luminous intensity loss caused because coating layer is too thick;
2) technical solution of the present invention is carried out in aqueous phase, by utilizing hydrolysis, the polymerization of tetraethoxy, first the network-like polymkeric substance of one deck is generated at phosphor surface, can the hydrolysis of Fluorophotometry powder, therefore the present invention is also applicable to carry out coated to facile hydrolysis fluorescent material, overcomes the defect that its fluorescent material facile hydrolysis of other coating technologies carried out in aqueous phase lost efficacy;
3) ethanol contained in the initial action solution of technical solution of the present invention, not only as the solvent of tetraethoxy, also because it has volatility, can play dissemination in reaction process, is conducive to obtaining more uniform coated rete;
4) in technical solution of the present invention raw materials used cheap, be easy to get, technique is simple, and the reaction times is short, and low to the dependency of equipment, the energy, process is pollution-free.
Accompanying drawing explanation
Fig. 1 is SiO
2coated SrAl
2o
4: Eu
2+, Dy
3+the stereoscan photograph of fluorescent material.
Fig. 2 is not coated SrAl
2o
4: Eu
2+, Dy
3+the stereoscan photograph of fluorescent material.
Embodiment
Following instance is further illustrating present invention process, and the present invention is including but not limited to following instance.
Embodiment 1
5.357g tetraethoxy is dissolved in 300ml water: ethanol contend, than in the mixed solution for 1:1, stirs and makes it dissolve.By nitric acid adjust ph to 1, then use ammoniacal liquor adjust ph to 6.Add the SrAl of 11.3584g urea and 30g facile hydrolysis
2o
4: Eu
2+, Dy
3+yellow-green colour long persistence luminescent powder, reaction 1 hour in 95 DEG C and under the condition constantly stirred, now pH value is 8.Reaction system is cooled to room temperature, and suction filtration is separated, and washs 2 times respectively, then in 80 DEG C of dried overnight with distilled water and ethanol.Powder will be dried at 400 DEG C, 10%H
2/ 90%N
2reducing atmosphere under insulation within 1 hour, namely obtain SiO
2coated SrAl
2o
4: Eu
2+, Dy
3+fluorescent material, its luminescent properties non-coating fluorescent powder relative to afterglow property does not have significantly sacrificing.
Accompanying drawing 1 is shown in by the SEM photo of coating fluorescent powder, and accompanying drawing 2 is shown in by the SEM photo of non-coating fluorescent powder.
Contrast accompanying drawing 1 and accompanying drawing 2 visible, sharply clearly, surface is comparatively coarse, and coated rear fluorescent powder grain angular edge comparatively relaxes, and surface is comparatively smooth, shows successfully at SrAl for coated front fluorescent powder grain corner angle
2o
4: Eu
2+, Dy
3+phosphor surface is coated has gone up even, the fine and close rete of one deck.
Embodiment 2
1.071g tetraethoxy is dissolved in 200ml water: ethanol contend, than in the mixed solution for 3:1, stirs and makes it dissolve.Add 2.230g Al (NO
3)
39H
2o, stirs and makes it dissolve.With salt acid for adjusting pH value to 2, then use sal volatile adjust ph to 5.Add the SrAl of 6.673g urea and 30g facile hydrolysis
2o
4: Eu
2+, Dy
3+yellow-green colour long persistence luminescent powder, reaction 2 hours in 100 DEG C and under the condition constantly stirred, now pH value is 8.Reaction system is cooled to room temperature, centrifugation, washs 3 times respectively with distilled water and ethanol, then in 90 DEG C of dried overnight.By oven dry powder 500 DEG C, under carbothermic reduction atmosphere insulation within 0.5 hour, namely obtain SiO
2and Al
2o
3the SrAl of compound coating
2o
4: Eu
2+, Dy
3+fluorescent material, its luminescent properties non-coating fluorescent powder relative to afterglow property is not obviously decayed.
In atmosphere in 800 DEG C of SrAl to coated front and back
2o
4: Eu
2+, Dy
3+after fluorescent material carries out the thermal degradation when process of 5 minutes, the original intensity after coating fluorescent powder irradiates 5 minutes in the sunlight and time of persistence are 2 times and 3 times of non-coating fluorescent powder respectively, show that the thermostability of coating fluorescent powder is improved.
Embodiment 3
By 4.820g Mg (NO
3)
26H
2o is dissolved in 400ml water: ethanol contend, than in the mixed solution for 9:1, stirs and makes it dissolve.By sulfuric acid adjust ph to 2, then use ammonium bicarbonate soln adjust ph to 6.Add 16.932g urea and 30gBaMgAl
10o
17: Eu
2+blue colour fluorescent powder, reaction 3 hours in 110 DEG C and under the condition constantly stirred, now pH value is 8.Reaction system is cooled to room temperature, filtering separation, washs 2 times respectively with distilled water and ethanol, then in 100 DEG C of dried overnight.Powder will be dried at 600 DEG C, 5%H
2/ 95%N
2reducing atmosphere under insulation within 2 hours, namely obtain the coated BaMgAl of MgO
10o
17: Eu
2+fluorescent material, its luminescent properties relatively non-coating fluorescent powder is not obviously decayed.
In atmosphere in 600 DEG C of BaMgAl to coated front and back
10o
17: Eu
2+fluorescent material carries out the thermal degradation when process of 30 minutes, and the luminous intensity of coating fluorescent powder under 254nm excites is 130% of non-coating fluorescent powder, shows that the thermostability of coating fluorescent powder is improved.
Embodiment 4
By 1.115g Al (NO
3)
39H
2o and 0.9639gMg (NO
3)
26H
2o is dissolved in 200ml water, stirs and makes it dissolve.By nitric acid adjust ph to 1, then use ammoniacal liquor adjust ph to 6.Add 6.062g urea and 30g Sr
2mgSi
2o7:Eu
2+, Dy
3+sky blue long persistence luminescent powder, reaction 3 hours in 85 DEG C and under the condition constantly stirred, now pH value is 8.Reaction system is cooled to room temperature, and suction filtration is separated, and washs 2 times respectively, then in 110 DEG C of dried overnight with distilled water and ethanol.Oven dry powder is incubated 1 hour at 500 DEG C and namely obtains Al
2o
3with the Sr of MgO compound coating
2mgSi
2o7:Eu
2+, Dy
3+fluorescent material, its luminescent properties non-coating fluorescent powder relative to afterglow property is not obviously decayed, and in air, irradiate 1.5 times and 2 times that the original intensity of 5 minutes and time of persistence are non-coating fluorescent powder respectively after the thermal treatment of 800 DEG C, 5 minutes in the sunlight.
Embodiment 5
0.5357g tetraethoxy is dissolved in 300ml water: ethanol contend, than in the mixed solution for 2:1, stirs and makes it dissolve.Add 1.115g Al (NO
3)
39H
2o and 0.9639gMg (NO
3)
26H
2o, stirs and makes it dissolve.By nitric acid adjust ph to 1, then use ammonium bicarbonate soln adjust ph to 6.Add 8.334g urea and 30gY
2o
2s:Eu
3+red fluorescence powder, reaction 1 hour in 90 DEG C and under the condition constantly stirred, now pH value is 8.Reaction system is cooled to room temperature, and suction filtration is separated, and washs 2 times respectively, then in 80 DEG C of dried overnight with distilled water and ethanol.Namely oven dry powder is obtained SiO in 1 hour 500 DEG C of insulations
2, Al
2o
3with the Y of MgO compound coating
2o
2s:Eu
3+fluorescent material, its luminescent properties relatively non-coating fluorescent powder is not obviously decayed, and the luminance loss in air after the thermal treatment of 180 DEG C, 20 minutes is 25%, is better than 35% of non-coating fluorescent powder.
Embodiment 6
By 11.1492g Al (NO
3)
39H
2o is dissolved in 300ml water, stirs and makes it dissolve.By nitric acid adjust ph to 1, then use sal volatile adjust ph to 6.Add 13.3765g urea and 30g (Y, Gd)
3(Al, Ga)
5o
12: Ce
3+yellow fluorescent powder, reaction 0.5 hour in 95 DEG C and under the condition constantly stirred, now pH value is 8.Reaction system is cooled to room temperature, and suction filtration is separated, and washs 2 times respectively, then in 80 DEG C of dried overnight with distilled water and ethanol.Oven dry powder is incubated 0.5 hour at 500 DEG C and namely obtains Al
2o
3coated (Y, Gd)
3(Al, Ga)
5o
12: Ce
3+fluorescent material, its luminescent properties relatively non-coating fluorescent powder is not obviously decayed, and the luminance loss in air after the thermal treatment of 180 DEG C, 20 minutes is 20%, is better than 25% of non-coating fluorescent powder.
Embodiment 7
0.0536g tetraethoxy is dissolved in 210ml water: ethanol contend, than in the mixed solution for 20:1, stirs and makes it dissolve.Add 0.0954g Mg (NO
3)
26H
2o, stirs and makes it dissolve.With salt acid for adjusting pH value to 2, then use sal volatile adjust ph to 6.Add 20 times of GOLD FROM PLATING SOLUTION and belong to the urea of element molar weight and the SrAl of 30g facile hydrolysis
2o
4: Eu
2+, Dy
3+yellow-green colour long persistence luminescent powder, reaction 6 hours in 80 DEG C and under the condition constantly stirred, now pH value is 8.Reaction system is cooled to room temperature, centrifugation, washs 3 times respectively with distilled water and ethanol, then in 90 DEG C of dried overnight.By oven dry powder 700 DEG C, under carbothermic reduction atmosphere calcining within 0.1 hour, namely obtain SiO
2and Al
2o
3the SrAl of compound coating
2o
4: Eu
2+, Dy
3+fluorescent material, its luminescent properties non-coating fluorescent powder relative to afterglow property is not obviously decayed, and the luminance loss in air after the thermal treatment of 180 DEG C, 20 minutes is 20%, is better than 25% of non-coating fluorescent powder.
Embodiment 8
5.3571g tetraethoxy is dissolved in 300ml water: ethanol contend, than in the mixed solution for 1:3, stirs and makes it dissolve.Add 11.0375g Al (NO
3)
39H
2o and 9.5426gMg (NO
3)
26H
2o, stirs and makes it dissolve.By nitric acid adjust ph to 1, then use ammonium bicarbonate soln adjust ph to 5.Add urea and 30gY that 3 times of GOLD FROM PLATING SOLUTION belong to element molar weight
2o
2s:Eu
3+red fluorescence powder, reaction 0.1 hour in 120 DEG C and under the condition constantly stirred, now pH value is 8.Reaction system is cooled to room temperature, and suction filtration is separated, and washs 2 times respectively, then in 80 DEG C of dried overnight with distilled water and ethanol.Namely oven dry powder is obtained SiO in 6 hours 300 DEG C of insulations
2, Al
2o
3with the Y of MgO compound coating
2o
2s:Eu
3+fluorescent material, the luminance loss in air after the thermal treatment of 180 DEG C, 20 minutes is 20%, is better than 25% of non-coating fluorescent powder.
Claims (3)
1. a preparation method for inorganic oxide encapsulated phosphor, its surface coating layer containing silica, magnesium oxide, aluminum oxide any one or any two or three, it is characterized in that comprising the following steps:
1) kind of inorganic oxide contained by above-mentioned coating layer, select tetraethoxy, solubility magnesium salts, aluminum soluble salt to prepare solution A, solvent is the mixed solution of water or water and ethanol;
2) first use strong acid adjust ph to 1 ~ 2, then obtain solution B with weak base adjust ph to 5 ~ 7; Described strong acid is sulfuric acid, hydrochloric acid or nitric acid; Described weak base is ammoniacal liquor, volatile salt or bicarbonate of ammonia;
3) in mixing solutions B, add urea and fluorescent material, at the temperature of 80 ~ 120 DEG C, reaction 0.1 ~ 6 hour, obtains the slurry C containing fluorescent material, solid-liquid separation after cooling, washs and dry to obtain powder;
4) within 0.1 ~ 6 hour, inorganic oxide encapsulated phosphor is obtained by drying the temperature lower calcination of powder at 300 ~ 700 DEG C;
Wherein, fluorescent material is the fluorescent material that hydrolysis easily occurs, and adds tetraethoxy during preparation solution A.
2. the preparation method of inorganic oxide encapsulated phosphor described in claim 1, when it is characterized in that described solvent is the mixed solution of water and ethanol, water: ethanol contend is than being 20:1 ~ 1:3; Described tetraethoxy, solubility magnesium salts, aluminum soluble salt are by the Mass Calculation of corresponding metal oxide, and corresponding silicon oxide, magnesium oxide, aluminum oxide consumption are 0 ~ 15% of fluorescent material consumption; The total mass of three kinds of oxide compounds is 0.1 ~ 15% of fluorescent material quality; The consumption of described urea is 3 ~ 20 times of metallic element integral molar quantity in solution A.
3. the preparation method of inorganic oxide encapsulated phosphor described in claim 1, is characterized in that in described calcination process, the fluorescent material bad or easily oxidized for thermostability in oxidizing atmosphere, selects to calcine in reducing atmosphere; Reducing atmosphere uses carbon heat or uses nitrogen and hydrogen mixture.
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| KR20170141706A (en) | 2015-04-27 | 2017-12-26 | 메르크 파텐트 게엠베하 | Silicate phosphor |
| CN106866034A (en) * | 2017-03-22 | 2017-06-20 | 佛山市蓝瑞欧特信息服务有限公司 | A kind of fluorescent artificial stone diamond stone sheet material and preparation method thereof |
| CN107163940A (en) * | 2017-06-26 | 2017-09-15 | 南京工业大学 | Preparation and surface modification method of zinc oxide green fluorescent powder |
| CN109133878B (en) | 2017-06-28 | 2021-11-30 | 深圳光峰科技股份有限公司 | Composite ceramic and preparation method thereof |
| CN107446084A (en) * | 2017-07-24 | 2017-12-08 | 南京师范大学 | A kind of water-fast luminous hydrogel and preparation method thereof |
| CN108059953B (en) * | 2017-11-24 | 2020-05-22 | 中国林业科学研究院木材工业研究所 | Long-afterglow luminous flexible nano-cellulose material, and preparation method and application thereof |
| CN109400158A (en) * | 2018-12-29 | 2019-03-01 | 北京雷生强式科技有限责任公司 | Mix the preparation method of ytterbium luteium oxide laser ceramics |
| CN111334281B (en) * | 2020-03-06 | 2023-07-04 | 英特美光电（苏州）有限公司 | Preparation method of composite coated yellow fluorescent powder special for COB |
| CN113789169B (en) * | 2021-10-29 | 2024-01-26 | 重庆文理学院 | Fluorescent powder and preparation method thereof |
| CN116042069A (en) * | 2022-11-03 | 2023-05-02 | 中建工程产业技术研究院有限公司 | Single-component polyurea waterproof coating with refrigeration function and preparation method thereof |
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