CN1363643A - Process for preparing nano yttrium aluminate as fluorescent powder - Google Patents
Process for preparing nano yttrium aluminate as fluorescent powder Download PDFInfo
- Publication number
- CN1363643A CN1363643A CN 01138218 CN01138218A CN1363643A CN 1363643 A CN1363643 A CN 1363643A CN 01138218 CN01138218 CN 01138218 CN 01138218 A CN01138218 A CN 01138218A CN 1363643 A CN1363643 A CN 1363643A
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- sol
- fluorescent powder
- yttrium aluminate
- rare earth
- solution
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Links
- 239000000843 powder Substances 0.000 title claims abstract description 24
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title description 8
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000003980 solgel method Methods 0.000 claims abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 8
- 150000002910 rare earth metals Chemical class 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 6
- 239000011259 mixed solution Substances 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- 239000000463 material Substances 0.000 description 13
- 238000001354 calcination Methods 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 12
- 230000007704 transition Effects 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000005284 excitation Effects 0.000 description 5
- 238000000695 excitation spectrum Methods 0.000 description 4
- -1 rare earth yttrium aluminate Chemical class 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000003836 solid-state method Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
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Abstract
A nano fluorescent yttrium aluminate powder is prepared by the combination of sol-gel method with microwave method. Its advantages include low temp for preparing it, short preparing temp. and high uniformity, purify and luminous nature of product. It can be used for plasma display panel, field-luminous display screen, etc.
Description
Technical field
The present invention relates to the nano rare earth yttrium aluminate as fluorescent powder, particularly prepare the method for nano yttrium aluminate as fluorescent powder.
Background technology
Because the relative luminous intensity of nano rare earth fluorescent material has been compared with micron fluorescent material and has been significantly improved, and the frequency displacement phenomenon can appear in emission wavelength, therefore, the nano rare earth luminescent material becomes a new and developing branch of luminescent material research field, and nano rare earth high-efficiency fluorescence powder has important application prospects on plasma display panel (PDP) (PDP), el display panel (EL).At present, preparation fluorescent RE powder method is a lot, as high temperature solid-state method etc., the fluorescent material of these method preparations all is micron order, and the sintering temperature that this producing and manufacturing technique requires is than higher, generally more than 1200 ℃, production cycle is longer, and the cost height is unfavorable for scale operation.
Summary of the invention
Technical problem to be solved by this invention is: the method for preparing nano yttrium aluminate as fluorescent powder, the sintering temperature that this method requires is lower than the temperature of high temperature solid-state method preparation micron fluorescent material, production cycle is shorter, and the product that makes chemistry good uniformity, purity height, luminescent properties significantly improve.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: its method steps is:
(1), rare earth oxide is obtained the mixed polymer colloidal sol of Citrate trianion with sol-gel method;
(2), step (1) gained colloidal sol is put in the microwave oven heating and obtained gelinite;
(3), gelinite is obtained xerogel by drying;
(4), xerogel is heat-treated under differing temps, and carry out the product particle surface and modify, just obtain nano yttrium aluminate as fluorescent powder (Y
4Al
2O
9: Eu
3+).
The present invention combines sol-gel method and forms new prepared route with microwave method, preparation nano rare earth yttrium aluminate as fluorescent powder (Y
4Al
2O
9: Eu
3+).In preparation process, impel doping with rare-earth ions evenly and promptly to spread by microwave heating and form the soluble chelating thing with citric acid, thereby, by microwave action colloidal sol is transformed also to gel again and shortened the production cycle greatly for the preparation of twinkler provides the presoma of forming and being evenly distributed.After 800 ℃～1200 ℃ calcinations, its product particle surface is modified, just can obtain nano rare earth yttrium aluminate as fluorescent powder (Y
4Al
2O
9: Eu
3+).
The sintering temperature that the inventive method requires obviously reduces than the temperature of high temperature solid-state method preparation micron fluorescent material, generally at 800 ℃～1200 ℃; Shorten the production cycle; The product chemical uniformity, purity, the luminescent properties that make all significantly improve; Product cost is low, is beneficial to scale operation.This novel red nano-phosphor can be applicable to PDP, EL, luminescent lamp, onboard instruments, mobile video telephone, game machine and ceramic scintillator etc.
Description of drawings
Fig. 1 is an embodiment of the invention schema
Fig. 2 is the powder crystal diffractogram of the inventive method nano yttrium aluminate as fluorescent powder that calcination obtains under differing temps
Fig. 3 is the transmission electron microscope high resolution pattern picture of the inventive method gained nano yttrium aluminate as fluorescent powder
Fig. 4 is the inventive method gained nano yttrium aluminate as fluorescent powder transmission electron microscope high resolving electron diffraction picture
Fig. 5 is the excitation spectrum of the inventive method gained nano yttrium aluminate as fluorescent powder
Fig. 6 is the emmission spectrum of the inventive method calcination gained nano yttrium aluminate as fluorescent powder under non-reduced atmosphere
Fig. 7 is the emmission spectrum of the inventive method calcination gained nano yttrium aluminate as fluorescent powder under reducing atmosphere
Specific embodiments
As shown in Figure 1, production craft step of the present invention is: take by weighing Y by certain stoichiometric ratio
2O
3(99.99%) is 4.5200 grams, Al (NO
3)
39H
2O (AR) is 7.5000 grams, and citric acid (AR) is 48.2600 grams, HNO
3(AR) be 1.8900 grams, Eu
2O
3(99.99%) is 0.3520 gram.Control weighing citric acid amount of substance is between 1.5～6.5 times of total amount of metal ion species such as rare earth.With Eu
2O
3, Y
2O
3Dissolve in 0.1-1N HNO respectively
3Can obtain nitrate solution, will be by the Al (NO of stoichiometric ratio weighing
3)
39H
2O and citric acid dissolve, and mix the mixed polymer solution that can obtain Citrate trianion with the nitrate solution that contains rare earth that obtains previously.In said process, note controlling amount of water.How many general mole ratio R=[H that use of amount of water
2O]: [M (OR)] expression.Amount of water and prepared dissolved adhesiveness and gelation time have substantial connection, and R need be controlled between 2～8.The excessive then viscosity degradation of R, gelation time prolongs, because too much water has watered down the concentration of inner complex.The too small dissolving that then is unfavorable for nitrate and citric acid of R, thus can not form uniform solution and precipitating metal nitrate.Simultaneously, too much water also can make prolong time of drying.PH is also very crucial in preparation process, and PH should be controlled at 2～8 scopes.PH value is unfavorable for the stable of inner complex too greatly, and crystallization and precipitation can occur.Just obtain colloidal sol behind the regulation and control mixing solutions pH value, insert that heating obtains gelinite in the microwave oven.Gelinite inserted drying obtains xerogel in the microwave oven.Xerogel is heat-treated under 800～1200 ℃.Then the product particle surface is modified, promptly used the immersion of 0.01～0.5M gelatin solution, stirring, separation, drying, just obtain nano rare earth fluorescent material Y
4Al
2O
9: Eu
3+
Y
2O
3-Al
2O
3There are three different thing phases: YA1O in two component system
3, Y
3Al
5O
12And Y
4Al
2O
9, this was studied in existing relevant document, three kinds of things of yttrium aluminate mutually in, preceding two kinds of matrix as fluorescent material were widely studied, and Y
4Al
2O
9As luminous host but be studied few.In the research, I find just can obtain fluorescent material Y with sol-gel processing at 800 ℃
4Al
2O
9The thing phase, 900 ℃ of following calcinations can obtain its pure thing phase, and the gained powder is observed down at transmission electron microscope (TEM), and the granular size of fluorescent material is at nano level (as Fig. 3).
Determining of calcination temperature: xerogel is put into the calcination under different temperature of high temperature cabinet-type electric furnace, the sample that obtains is carried out X ray powder crystal diffraction (XRD) analysis, found that in the time of 800 ℃, to begin to occur nanometer crystalline phase Y
4Al
2O
9Product has been Y when (YAO), reaching 900 ℃
4Al
2O
9Pure phase, then respectively 1000 ℃, 1200 ℃ following calcinations, the product that obtains still is Y
4Al
2O
9, the XRD of series of samples such as Fig. 2.The pattern of product and particle diameter are observed with transmission electron microscope (TEM), Figure 3 shows that the pattern picture (BF) of the nano-phosphor that obtains after 900 ℃ of following calcinations, Figure 4 shows that electron diffraction picture (ED).As can be seen from Figure 3 between 20nm～50nm, the statistical study median size is 30nm to grain diameter basically.By transmission electron microscope observation, most of particulates of the nano-phosphor of synthetic preparation are spherical or subsphaeroidal.Discover the raising along with calcination temperature, it is big that the particle diameter of YAO fluorescent powder grain can become gradually.When sintering temperature reaches 1200 ℃, the particle diameter of YAO is basically more than 1um.In addition, compare with a high temperature solid-state method preparation micron fluorescent material temperature with temperature shown in the phasor of Fig. 2 and relevant bibliographical information, the method that adopts sol-gel method to combine with microwave method prepares nanocrystalline Y
4Al
2O
9The thing phase, it burns temperature can be reduced to 800 ℃, and the production cycle has also shortened greatly.
The present invention adopts direct calcination xerogel and calcination under activity charcoal powder reductive atmosphere respectively, finds that the nanometer crystalline phase that obtains is same thing phase YAO.
The present invention studies exciting with emmission spectrum of gained nano-phosphor.Be illustrated in figure 5 as the excitation spectrum of gained under emmission spectrum 598nm monitoring, spectrogram 1 is the excitation spectrum of the sample for preparing under the non-reduced atmosphere, and peak value is respectively 394.3nm, 438.5nm, 470.8nm; Spectrogram 2 is the excitation spectrum of the sample of preparation under the reducing atmosphere, and the peak value of appearance is respectively 340.1nm, 395.7nm, 471.2nm.Both difference are 340.1nm and 438.5nm two excitation peaks, and the major cause that these different peaks occur is Eu
3+The fine difference of residing crystallographic site causes in the YAO nanocrystalline structure.Above-mentioned excitation peak is because Eu
3+The transition of f-f absorb and to cause.Y
4Al
2O
9Crystalline structure is an oblique system, and spacer is P2
1/ C, point group are C
2hWhen doping Eu ion to Y
4Al
2O
9In the time of in the crystal, because Eu ionic radius and Y
3+Radius (R
Y 3+=0.088nm) more approaching, so Eu generally occupies Y in lattice
3+The position, and Eu generally exists with two kinds of ionic speciess: Eu
3+(R
Eu 3+=0.095nm) and Eu
2+(R
Eu 2+=0.109nm), from valence state and ionic radius consider the Eu ion should with the trivalent form be present in nanocrystalline.In conjunction with emmission spectrum, the emission peak in the spectrum all is Eu
3+ 5D
0→
7F
JThe feature emission that produces of transition, even and the reducing atmosphere fluorescent material of preparation down, Eu does not appear in its emmission spectrum yet
2+The emission of ionic feature, Eu is at nanocrystalline Y in this explanation
4Al
2O
9In be form Eu with trivalent ion
3+Exist, the reason that causes this result is just due to the acting in conjunction of ionic radius and charge balance.Analyze emmission spectrum, find in the experiment different emission peaks can occur when with different optical excitation, the emission spectrum that is occurred after the optical excitation of wavelength X=400nm is unimodal λ=597.8nm, is orange light emission (seeing shown in Figure 6).Orange light emission about λ=590nm has not only appearred in the emission peak that is produced behind the ultraviolet excitation of wavelength X=254nm, and the red emission (seeing shown in Figure 7) of λ=610nm occurred.According to Eu in the crystal
3+The general rule of transition of electron is worked as Eu
3+When being in the case that the strict centre of inversion is arranged, will with
5D
0→
7F
1It is main that orange light (about 590nm) is launched in the magnetic dipole transition that allows; Work as Eu
3+When being in the case that departs from the centre of inversion, because at 4f
6Sneaked into the ununiformity of 5d and the 5g configuration and the crystal field of opposite parity in the configuration, the parity selection rule in the crystal is relaxed, the f-f forbidden transition is partly lifted a ban, and will occur
5D
0→
7F
2Deng electric dipole transition; Work as Eu
3+When being in the case of no inversion center of symmetry, often with
5D
0→
7F
2Electric dipole transition red-emitting (about 610nm) is emitted as the master.The brilliant Y of combining nano
4Al
2O
9Constructional feature, its point group are C
2b, because Eu
3+At nanocrystalline Y
4Al
2O
9In occupy Y
3+The position, Eu thus
3+Should be in the case that the strict centre of inversion is arranged, its emission should be
5D
0→
7F
1The magnetic dipole transition orange light (about 590nm) that allows is emitted as the master.Orange light and red emission in preparing the spectrogram of product, have occurred, and the latter's intensity is greater than the former, this explanation part Eu in nanocrystalline
3+Be in the case that departs from the centre of inversion, so occurred
5D
0→
7F
2Electric dipole transition ruddiness (about 610nm) emission.
Claims (6)
1, a kind of method for preparing nano yttrium aluminate as fluorescent powder, it is characterized in that: its method steps is:
(1), with rare earth oxide Eu
2O
3Obtain the mixed polymer colloidal sol of Citrate trianion with sol-gel method;
(2), step (1) gained colloidal sol is put in the microwave oven heating and obtained gelinite;
(3), gelinite is obtained xerogel by drying;
(4), xerogel is heat-treated under differing temps, and carry out the product particle surface and modify, just obtain nano yttrium aluminate as fluorescent powder.
2, the method for claim 1 is characterized in that: sol-gel method is: with rare earth oxide Eu
2O
3Dissolve in 0.1-1N HNO
3In, obtain nitrate solution, then with the mixed mixed solution that gets of other nitrate solution; Add citric acid in above-mentioned solution, obtain the mixed polymer solution of Citrate trianion, regulation and control mixing solutions PH numerical value is 2-8, makes colloidal sol.
3, method as claimed in claim 2 is characterized in that: the steps include: that used citric acid adds the overall control of amount of substance and metal ion such as rare earth doped between 1.5 times～6.5 times.
4, method as claimed in claim 1 or 2 is characterized in that: add entry in the sol-gel method process, what of amount of water are used mole ratio R=[H
2O]: [M (OR)] expression, R is controlled between 2～9.
5, the method for claim 1 is characterized in that: xerogel is heat-treated under 800 ℃～1200 ℃.
6, the method for claim 1 is characterized in that: product particle surface modification process is: with the immersion of 0.01～0.5M gelatin solution, stirring, separation, drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01138218XA CN1142238C (en) | 2001-11-26 | 2001-11-26 | Process for preparing nano yttrium aluminate as fluorescent powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01138218XA CN1142238C (en) | 2001-11-26 | 2001-11-26 | Process for preparing nano yttrium aluminate as fluorescent powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1363643A true CN1363643A (en) | 2002-08-14 |
| CN1142238C CN1142238C (en) | 2004-03-17 |
Family
ID=4674441
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB01138218XA Expired - Fee Related CN1142238C (en) | 2001-11-26 | 2001-11-26 | Process for preparing nano yttrium aluminate as fluorescent powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1142238C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306005C (en) * | 2004-11-15 | 2007-03-21 | 王兵 | Aluminate-base rare earth long afterglow luminous material synthesizing method |
| CN100358076C (en) * | 2004-08-04 | 2007-12-26 | 中国科学院上海光学精密机械研究所 | Method for preparing cerium-doped lutetium pyrosilicate submicron imaging screen |
| CN109096796A (en) * | 2018-08-23 | 2018-12-28 | 华北水利水电大学 | A kind of YAl1-xMxO3The preparation method of (M=Fe, Co, Cu) nano dye |
-
2001
- 2001-11-26 CN CNB01138218XA patent/CN1142238C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358076C (en) * | 2004-08-04 | 2007-12-26 | 中国科学院上海光学精密机械研究所 | Method for preparing cerium-doped lutetium pyrosilicate submicron imaging screen |
| CN1306005C (en) * | 2004-11-15 | 2007-03-21 | 王兵 | Aluminate-base rare earth long afterglow luminous material synthesizing method |
| CN109096796A (en) * | 2018-08-23 | 2018-12-28 | 华北水利水电大学 | A kind of YAl1-xMxO3The preparation method of (M=Fe, Co, Cu) nano dye |
| CN109096796B (en) * | 2018-08-23 | 2020-10-13 | 华北水利水电大学 | Preparation method of YAl1-x Fe xO3 nano pigment |
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| Publication number | Publication date |
|---|---|
| CN1142238C (en) | 2004-03-17 |
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Granted publication date: 20040317 |