CN1052745C - Micro-wave thermosynthesizing of fluorescent powder - Google Patents
Micro-wave thermosynthesizing of fluorescent powder Download PDFInfo
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- CN1052745C CN1052745C CN95106117A CN95106117A CN1052745C CN 1052745 C CN1052745 C CN 1052745C CN 95106117 A CN95106117 A CN 95106117A CN 95106117 A CN95106117 A CN 95106117A CN 1052745 C CN1052745 C CN 1052745C
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- 239000000843 powder Substances 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000011541 reaction mixture Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000012856 packing Methods 0.000 claims description 8
- 239000011229 interlayer Substances 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 6
- 238000002203 pretreatment Methods 0.000 claims description 5
- 238000003746 solid phase reaction Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- 238000010671 solid-state reaction Methods 0.000 claims description 2
- 150000002736 metal compounds Chemical class 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 238000005303 weighing Methods 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 230000003407 synthetizing effect Effects 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical class OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 229910052693 Europium Inorganic materials 0.000 description 3
- 229910052771 Terbium Inorganic materials 0.000 description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000004110 Zinc silicate Substances 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000013626 chemical specie Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- LQFNMFDUAPEJRY-UHFFFAOYSA-K lanthanum(3+);phosphate Chemical compound [La+3].[O-]P([O-])([O-])=O LQFNMFDUAPEJRY-UHFFFAOYSA-K 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- -1 no sintering Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- GFKJCVBFQRKZCJ-UHFFFAOYSA-N oxygen(2-);yttrium(3+);trisulfide Chemical compound [O-2].[O-2].[O-2].[S-2].[S-2].[S-2].[Y+3].[Y+3].[Y+3].[Y+3] GFKJCVBFQRKZCJ-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229940071182 stannate Drugs 0.000 description 1
- 125000005402 stannate group Chemical group 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
- 235000019352 zinc silicate Nutrition 0.000 description 1
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Abstract
The present invention relates to a new synthesis method of fluorescent powder, which utilizes microwave heat effect to synthesize fluorescent powder. A solid reaction mixture is obtained after raw materials are preprocessed; the solid reaction mixture is loaded in a specific reaction device, and then is arranged in a microwave device; the solid reaction mixture is firstly preheated at low power, and then is heated for a certain time at high power to obtain the target product. In the method of the present invention, the reaction is thorough and has high speed; the target product has favorable performance; the particle size conforms to use requirements. The devices have the advantages of simplicity and easy operation; the working environment is clean; the applicable kind of the synthetic fluorescent powder is wide. Therefore, the method of the present invention has the advantages of reliability, high efficiency, energy saving, environmental protection, etc.
Description
The present invention relates to a kind of new synthetic method of fluorescent material, i.e. applied microwave heat effect synthetizing phosphor powder.
The synthetic method of fluorescent material, mainly be high-temperature solid phase reaction method at present, raw material is with the solid-state certain hour that at high temperature reacts, obtain target product, because at first being the point of contact place between the solid-phase reactant component, reaction process sends out the biophase boundary response, react inside mutually by diffusing into thing then, and along with the carrying out that reacts, diffusion path is more and more longer, speed of response is more and more slower, therefore, reaction must at high temperature be carried out for a long time, according to the difference of various fluorescent material, temperature of reaction is generally 1000～1600 ℃ high temperature, requirement to heating installation is very high, and the reaction times generally must 3～5 hours, and energy consumption is big; Some special reaction is needed certain protection atmosphere, as contain lower valency ionic fluorescent material, need at specific reaction atmosphere such as H
2-N
2Carry out under mixed atmosphere or the carbon reduction atmosphere, must be heating installation with silicon molybdenum electric furnace or carbon silicon electric furnace for this reason; Simultaneously, because long reaction time, temperature distributing disproportionation, differ before and after the speed of response, be difficult to obtain to form uniform product, often product easy-sintering crystal grain is also thicker, do not meet service requirements, must first ball mill pulverizing during use to particle diameter less than 10 μ m, and the ball mill pulverizing process has been destroyed the crystal habit of fluorescent material to a certain extent, so that influences its use properties.
The purpose of this invention is to provide a kind of method of new synthetizing phosphor powder, its equipment is simple, and is easy and simple to handle, chemical reaction thoroughly and time-saving energy-saving, and product crystal grain meets service requirements.
Method of the present invention is to utilize microwave heating effect to come synthetizing phosphor powder, is about to suitable proportion raw material after pre-treatment, the reaction unit of packing into, put into microwave equipment, through the low power preheating, again under higher-wattage the heating certain hour after, obtain target product, its concrete steps are:
1. the pre-treatment of raw material: adopt dry method or wet processing, raw material is reacted with the solid mixt form;
2. charging: reaction mixture is packed in the reaction unit, reaction unit is the double seal container, and interlayer is filled the microwave absorbing medium, and reactant is contained in the inner jar, for the reaction mixture that must under reducing atmosphere, react, also have a dividing plate that reactant and reducing medium are separated in the inner jar;
3. microwave thermal preheating: charged reaction unit is put into microwave equipment, earlier with the preheating of low power short period of time, for the amount of target product be the reaction raw materials amount of 0.02～0.05mol, pre-thermal power at 100～200W, the time is 30～120 seconds;
4. microwave thermal reaction: after the preheating, strengthening microwave power and make reaction mixture reaction certain hour, obtain target product, is the reaction raw materials amount of 0.02～0.05mol for the amount of target product, and reaction power is 480～800W, and the reaction times is 20～60min.
Microwave heating effect is to utilize the microwave radiation of frequency for 2450MHz, act in the component of solid state reaction mixture, the dipole that orders about in its molecule is made vibration at high speed, owing to be subjected to the obstruction and the interference of molecule on every side, thereby acquisition energy, form with heat shows, and medium temperature is risen rapidly, drives chemical reaction and carries out.Therefore, during with the microwave thermal synthetizing phosphor powder, the chemical species of start material must be a dipole molecule, and is higher to the assimilated efficiency of microwave, and the chemically reactive of itself is higher, and be difficult for bringing into foreign ion or reaction back removal of contamination ion easily, the selection of raw material should be as prerequisite, and the method for pre-treatment also should satisfy this condition, for the raw material that can directly react, adopt dry process, obtain reaction mixture with mechanically mixing, ball milling; And some raw material must be used wet processing, and promptly raw material is placed in the solution, and mechanically mixing or chemical reaction are dried crushing screening again and obtained satisfactory reaction mixture.
For making reaction more fully with quick; thereby obtain even-grained single-phase product; fill a kind of microwave absorbing medium at the interlayer of reaction unit double container; the microwave absorbing medium is the big compound of dielectric loss; utilize the synthetic reaction process of microwave thermal; it plays and absorbs the hot unlikely effect of distributing rapidly that microwave produces heat and protection inner jar, and transition metal oxide can serve as the microwave absorbing medium, as CaO, Fe
2O
3, Fe
3O
4, V
2O
5, WO
3, NiO, Co
2O
3Deng, can select person cheap and easy to get, as Fe
2O
3The microwave absorbing medium is higher than the height of reactant in the inner jar at least in the packing height of container interlayer, and it is better that whole interlayer is all filled microwave absorbing medium effect.
During micro-wave thermosynthesizing of fluorescent powder, the power of its preheating and reaction is relevant with material quantity, and is also relevant to the ability of microwave absorbing with start material, as using power excessive, overlong time, the easy sintering of product, even become non-target product, also can bring more impurity phase simultaneously into, as use power too small, time is too short, can make reaction not exclusively, and impurity is mutually more.
Utilize microwave thermal to come synthetizing phosphor powder, because the thermal source of microwave heating is evenly distributed on the inside of object, make temperature of reaction even, and heat-up rate is very fast, therefore, micro-wave thermosynthesizing of fluorescent powder has following characteristics:
1. compare to conventional high-temperature solid phase reaction method synthetizing phosphor powder, speed of response is fast, and shortens the reaction times greatly, has energy-efficient advantage;
2. equipment is simple, and is easy and simple to handle, the Working environment cleaning, and the common household microwave oven of synthetic use of a small amount of fluorescent material can be finished;
3. method is reliable: the composition phase structure of the synthetic target fluorescent powder product that obtains is simple, is generally single-phasely, and impurity is seldom (≤1%) mutually, shows that chemical reaction is thorough, and is efficient; In addition, the excitation spectrum of product, emmission spectrum, parameters such as chromaticity coordinates all meet service requirements, and relatively luminosity is also higher, and is can be with commercially available fluorescent material comparable and granular size is suitable, generally in 10 μ m, as Y
2O
3: Eu
3+D
50Be 3.90 μ m, (LaCeTb) PO
4Be 6.09 μ m, can ball mill pulverizing can use.
4. the suitable synthetic fluorescent material kind of the inventive method is wider, comprises oxide system, oxysulfide system, phosphate system, borate salt system, silicate systems, aluminates system, vanadate system, tungstate system, stannate system and sulfide system etc.
Below be embodiments of the invention:
(used microwave oven is the E22E-3 type household microwave oven that Shuande a species of small clam living in fresh water China microwave oven factory produces among the embodiment) embodiment 1: yttrium oxide is mixed the synthetic of europium fluorescent material
Take by weighing Y respectively
2O
35.14194g, Eu
2O
30.3519g, use dissolving with hydrochloric acid, heating evaporation is removed excessive hydrochloric acid, with the less water dissolving, adjusts PH=2, and add saturated oxalic acid and extremely precipitate fully, ageing 3 hours, filtration washing is to there not being Cl
-Ion, oven dry gets reaction mixture, reaction mixture is packed in the crucible, put into big crucible after adding a cover, interlayer is filled ferric oxide powder (device is seen Fig. 1), put into microwave oven, with 160W preheating 1 minute, continue with 720W heating 28 minutes earlier, reaction finishes, cold slightly, taking-up is chilled to room temperature, and products therefrom is white powder, and the X ray powder diffraction analysis result of product shows the d value and the relative intensity I/I of product
1Variation tendency and (Y
0.95Eu
0.05)
2O
3Card value basically identical (table 1) calculates according to experimental data, and product is an isometric system, and it is 1.0606nm that its structure cell ginseng is imitated a, with (Y
0.95Eu
0.05)
2O
3Card value a
0=1.0604nm is very consistent, in addition, also records the chromaticity coordinates value X=0.646 of product, Y=0.350, and luminosity is 70% relatively, the particle size dispersion of product is as shown in table 2.
Among Fig. 1,1 is inner jar, and 2 is outer container, and 3 is reaction mixture, and 4 is the microwave absorbing medium.Embodiment 2: yttrium oxysulfide is mixed the synthetic of europium fluorescent material
Take by weighing Y respectively
2O
39.1748g, Eu
2O
20.8253g, after the mixing, remove excessive hydrochloric acid with the dissolving with hydrochloric acid evaporation, about PH2, use oxalic acid precipitation, washing is to there not being Cl
-Ion filters, and oven dry is with Na
2CO
33.000g, sulphur 3.000g, (NH
4)
2HPO
40.5000g after mixed grinding was even, the reaction unit of packing into (with embodiment 1, seeing Fig. 1) placed microwave to protect, and earlier with 160W preheating 1 minute, continued with 720W heating 28 minutes, vulcanization reaction finishes, and taking-up is chilled to room temperature, with the boiling water washing, filters, and oven dry is again with Na
2CO
33.000g, sulphur 3.000g, (NH
4)
2HPO
40.5000g mix, grind evenly, carry out the vulcanization reaction second time,, continue after 1 minute with the 160W preheating with 720W heating 17 minutes, cold slightly, taking-up is chilled to room temperature, pours in the boiling water, stirs, washing is to neutral, filter, oven dry, products therefrom are white powder crystal shape, and uniform particles is tiny, the performance test data of product shows, the d value of product and relative intensity variation tendency and Y
2O
3S card value basically identical (table 3), product are hexagonal system, its unit cell parameters a=0.3785nm, and c=0.6590nm is with Y
2O
2S card value a
0=0.3784mm, c
0=0.6585 ten minute is approaching, wherein, and Y
2O
3Dephasign only 0.9%.Embodiment 3: lanthanum orthophosphate, cerium, terbium fluorescent material synthetic
By La: Ce: Tb is that 0.55: 0.10: 0.05 stoichiometric takes by weighing La respectively
2O
3, CeO
2, Tb
4O
7, be converted into oxide solution, with the saturated oxalic acid precipitation, washing is to there not being Cl about PH2
-Ion filters, and takes by weighing (La, Ce, Tb) after the oven dry
2(C
2O
4)
32.7204g with (NH
4)
2HPO
41.4527g, H
3BO
30.1252g mixed grinding is even; pack in the reaction unit as Fig. 2; 1 is inner jar among the figure, and 2 is outer container, and 3 is reaction mixture; 4 is the microwave absorbing medium; 5 is the inner jar median septum, and 6 is reducing medium, and the microwave absorbing medium is the ferric oxide powder in the present embodiment; reducing medium is a grain active carbon; reaction unit is put into microwave oven,, continues with 720W heating 28 minutes after 1 minute with the 160W preheating earlier; reaction finishes; cold slightly, take out and be cooled to room temperature, product is white powder; particle is thin, no sintering.The The performance test results of product, its particle size dispersion such as table 4.Embodiment 4: positive zinc silicate is mixed the synthetic of manganese fluorescent material.
Take by weighing ZnO 3.2552g respectively, SiO
21.2018g, MnCO
30.0460g and H
3BO
30.1351g mixed grinding is even, the reaction unit of packing into (, seeing Fig. 2) with embodiment 3, and device is put into microwave oven, with 160W preheating 1 minute, continue with 720W heating 40 minutes earlier, reaction finishes, and is cold slightly, taking-up is chilled to room temperature, and product is white powder, and particle is tiny, no sintering.Embodiment 5: yttrium oxide is mixed the synthetic of europium fluorescent material
Take by weighing Y respectively
2O
34.3358g, Eu
2O
30.2825g be ground to mix after, take by weighing above-mentioned mixed oxide 3.000g again, Ne
2C
2O
4Mix 0.15g be ground to, reaction mixture, with the reaction mixture reaction unit (device is seen Fig. 1) of packing into, put into microwave oven, earlier with 160W preheating 2 minutes, continuation was heated 39 minutes with 720W, and reaction finishes, and is cold slightly, taking-up is chilled to room temperature, products therefrom is white powder, no sintering, and product property is with embodiment 1.
Table 1 Y
2O
3: Eu
3+Microwave thermal method synthetic X ray diffracting data
| Experimental value 2 θ d (nm) inten. I/I 1 | PDF 25-1011 card value d (nm) I/I 1 hk1 |
| 20.470 0.4334 1188 12.3 29.126 0.3063 9633 100.0 31.516 0.2836 115 1.2 33.766 0.2652 2411 25.0 35.882 0.2500 514 5.3 37.908 0.2371 168 1.7 39.828 0.2261 553 5.7 41.662 0.2165 129 1.3 43.472 0.2079 791 8.2 46.860 0.1937 271 2.8 48.514 0.1874 3773 39.2 50.113 0.1818 238 2.5 51.628 0.1768 98 1.0 53.189 0.1720 486 5.0 54.702 0.1575 138 1.4 56.146 0.1636 393 4.1 57.593 0.1599 273 23.6 59.016 0.1563 495 5.1 60.413 0.1530 426 4.4 61.793 0.1500 219 2.3 63.133 0.1471 148 1.5 64.508 0.1443 263 2.7 65.815 0.1417 168 1.7 69.772 0.1346 185 1.9 | 0.4321 10 211 0.3058 100 222 0.2834 ＜1 321 0.2649 25 400 0.2498 6 411 0.2371 1 420 0.2260 6 332 0.2184 1 422 0.2079 8 431 0.1935 3 521 0.1874 50 440 0.1818 3 433 0.1767 1 600 0.1720 8 611 0.1677 1 620 0.16360 5 541 0.15990 30 622 0.15640 8 631 0.15310 6 444 0.15000 2 543 0.14700 1 640 0.14430 4 721 0.14170 2 642 0.13470 2 732 |
Table 2 Y
2O
3: Eu
3+Microwave thermal method synthetic particle size dispersion
| Diameter accumulative total changes (μ m) (%) (%) | Diameter accumulative total changes (μ m) (%) (%) |
| 40.00 100.0 30.00 97.6 2.4 20.00 92.4 5.3 15.00 87.1 5.3 10.00 75.9 11.2 8.00 68.3 7.6 6.00 60.6 7.7 5.00 55.3 5.4 4.00 50.7 4.5 3.00 43.8 6.9 | 2.00 36.7 1.50 34.6 2.1 1.00 26.5 8.1 0.80 21.4 5.1 0.60 14.9 6.5 0.50 11.7 3.2 0.40 8.1 3.6 0.30 5.6 2.5 0.20 4.2 1.4 0 4.2 |
Table 3 Y
2O
2: Eu
3+Microwave thermal method synthetic X ray diffracting data
| Experimental value 2 θ d (nm) inten I/I 1 | PDF244-1424 card value d (nm) I/I 1 hk1 |
| 13.384 0.6607 201 3.0 27.083 0.3289 1794 27.0 29.120 0.3064 59 0.9 30.408 0.2936 6646 100.0 38.708 0.2323 2178 32.8 41.063 0.2196 741 11.1 48.017 0.1893 2064 31.1 49.947 0.1824 1289 19.4 55.976 0.1641 849 12.8 57.919 0.1590 784 11.8 63.214 0.1469 525 7.9 64.988 0.1433 471 7.1 | 0.656 2 001 0.328 35 002,100 0.293 100 101 0.232 60 102 0.219 16 003 0.1892 65 110 0.1824 45 103,111 0.1642 30 12,200 0.1591 25 201 0.1468 12 104 0.1434 20 113 |
Table 4 (La, Ce, Tb) PO
4Microwave thermal method synthetic particle size dispersion
| Diameter accumulative total changes (μ m) (%) (%) | Diameter accumulative total changes (μ m) (%) (%) |
| 40.00 100.0 30.00 96.5 3.5 20.00 89.3 7.2 15.00 81.7 7.6 10.00 65.6 18.1 8.00 57.7 7.9 6.00 49.8 7.9 5.00 44.2 5.6 4.00 38.4 5.8 3.00 31.6 6.8 | 2.00 26.7 1.50 24.3 2.4 1.00 18.4 5.8 0.80 13.0 5.4 0.60 7.6 5.4 0.50 5.0 2.6 0.40 3.8 1.2 0.30 3.0 0.8 0 3.0 |
Claims (6)
1. method for preparing fluorescent material, be with by the fluorescent powder product proportion raw material after pre-treatment, the reaction unit of packing into is put into microwave equipment, through the low power preheating, behind the heating certain hour, obtains target product again under higher-wattage, it is characterized in that:
1. the pre-treatment of raw material is dry method or wet method, gets the solid state reaction mixture after the processing;
2. the reaction mixture reaction unit of packing into, add the microwave absorbing medium after, place microwave equipment to react, the microwave absorbing medium does not contact with reaction mixture;
When 3. the amount of target product was 0.02～0.05mol, microwave preheating power was 100～200W, and the time is 30～120 seconds;
When 4. the amount of target product was 0.02～0.05mol, microwave heating power was 480～800W, and the time is 20～60 minutes.
2. method according to claim 1 is characterized in that said microwave absorbing medium is transistion metal compound CuO, Fe
2O
3, Fe
3O
4, V
2O
5, WO
3, NiO, Co
2O
3
3. method according to claim 2 is characterized in that said microwave absorbing medium is Fe
2O
3
4. a reaction unit that is used for the described method of claim 1 is characterized in that device is the double seal container, and reaction mixture is contained in the inner jar, and interlayer is filled the microwave absorbing medium.
5. reaction unit according to claim 4 is characterized in that said microwave absorbing medium is not less than the height of reactant in the inner jar in the packing height of reaction unit interlayer.
6. according to claim 4 or 5 described reaction units, it is characterized in that also having a dividing plate in the said inner jar, reactant and required reducing medium are separated.
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| Application Number | Priority Date | Filing Date | Title |
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| CN95106117A CN1052745C (en) | 1995-05-19 | 1995-05-19 | Micro-wave thermosynthesizing of fluorescent powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN95106117A CN1052745C (en) | 1995-05-19 | 1995-05-19 | Micro-wave thermosynthesizing of fluorescent powder |
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| CN1141946A CN1141946A (en) | 1997-02-05 |
| CN1052745C true CN1052745C (en) | 2000-05-24 |
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| CN95106117A Expired - Fee Related CN1052745C (en) | 1995-05-19 | 1995-05-19 | Micro-wave thermosynthesizing of fluorescent powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1306005C (en) * | 2004-11-15 | 2007-03-21 | 王兵 | Aluminate-base rare earth long afterglow luminous material synthesizing method |
| CN100369862C (en) * | 2005-06-24 | 2008-02-20 | 深圳大学 | Microwave hydrothermal synthesis device and method for synthesizing tetragonal barium titanate |
| CN100334181C (en) * | 2005-07-08 | 2007-08-29 | 中国科学院新疆理化技术研究所 | Microwave heating method for one-step synthesis of rare earth doped fluorescence material |
| CN102998166A (en) * | 2012-11-27 | 2013-03-27 | 天津师范大学 | Microwave sample pretreatment method applied to organic carbon detection |
| CN107723027A (en) * | 2017-11-06 | 2018-02-23 | 南昌大学 | A kind of method of microwave radiation technology dual bed quick catalysis stalk with the common vaporizing system of fine coal for combustion gas |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064301A (en) * | 1991-12-28 | 1992-09-09 | 上海跃龙有色金属有限公司 | High quality red fluorescent powder and manufacturing process thereof |
| CN1064472A (en) * | 1991-02-26 | 1992-09-16 | 通用电气公司 | Adopt hydroxide coprecipitation step to prepare the method for yttrium oxide-gadolinium sesquioxide ceramic scintillator |
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1995
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064472A (en) * | 1991-02-26 | 1992-09-16 | 通用电气公司 | Adopt hydroxide coprecipitation step to prepare the method for yttrium oxide-gadolinium sesquioxide ceramic scintillator |
| CN1064301A (en) * | 1991-12-28 | 1992-09-09 | 上海跃龙有色金属有限公司 | High quality red fluorescent powder and manufacturing process thereof |
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| CN1141946A (en) | 1997-02-05 |
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