CN1347958A - Up converting fluorescent material with nanometer level molybdate substrate and its prepn - Google Patents
Up converting fluorescent material with nanometer level molybdate substrate and its prepn Download PDFInfo
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- CN1347958A CN1347958A CN 01134861 CN01134861A CN1347958A CN 1347958 A CN1347958 A CN 1347958A CN 01134861 CN01134861 CN 01134861 CN 01134861 A CN01134861 A CN 01134861A CN 1347958 A CN1347958 A CN 1347958A
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Abstract
The present invention belongs to the field of nano fluorescent material. Lanthanum oxide (or yttrium or gadolinium oxide), ytterbium oxide and erbiom oxide (or thulium or holmium oxide) are first dissolved in acid to prepare solution; complexone and sodium or potassium molybdenate are added into the solution to produce precipitate, which is centrifugally separated and water washed to prepare aqueous gel, aqueous gel or further prepared alcoholic gel is finally cinerated in a high temperature furnace or heated in a hydrothermal reactor to obtain the nano level up converting fluorescent material. The said material has lanthanum molybdenate as matrix and ytterbium molybdenate and erbium molybdenate as dopant. The material thus prepared has small and homogeneous size, average size 50-60 nm and high light glowing strength and may meet the requirement as biological molecular fluorescent mark material.
Description
Technical field:
The invention belongs to the nano-luminescent material technical field, particularly a kind of is the rare earth ion doped nanometer upconverting fluorescent material and preparation method thereof of matrix with the molybdate.
Background technology:
Upconverting fluorescent material is a kind of at the infrared ray excited luminescent material that can send visible light down.Ytterbium, erbium-codoped molybdate are the higher upconverting fluorescent materials of a kind of efficiency ratio, and such material is normally pressed certain molar ratio with molybdenum oxide (MoO
3), ytterbium oxide (Yb
2O
3), Erbium trioxide (Er
2O
3) wait and mix, under 1200 ℃ high temperature, form by the high temperature solid state reaction calcination.Such material sends red fluorescence (Yu Xianen, practical luminescent material and photoluminescence mechanism, China Light Industry Press, 1997, Beijing) under the 970nm infrared excitation.
Upconverting fluorescent material is because its special nature can be used for preparing (Zarling, et al., US patent 5674698,1997) such as photodiode, solid substrate visible laser, highly sensitive biomolecules fluorescence labeling materials.
As the biomolecules fluorescence labeling material, need the particle of material own little and even, luminous intensity is big, and is stable in the aqueous solution.The preparation of above-mentioned high temperature solid-state method be common material but not nano material, also do not have the bibliographical information of such material preparation method of nano material at present, existing method is difficult to prepare the material that satisfies as the biomolecular labeling purposes.Existing in addition is that the upconverting fluorescent material of matrix has only the ytterbium erbium to mix with the molybdate, and does not prepare the ytterbium thulium, the report of codoped molybdate upconverting fluorescent materials such as ytterbium holmium.
Summary of the invention:
The present invention proposes a kind of nanometer level molybdate substrate upconverting fluorescent material and preparation method thereof, prepared material not only granularity is little and even, can reach nano level, and luminous intensity is big, to satisfy the needs as the biomolecules fluorescence labeling material.This method may further comprise the steps:
(1) with lanthanum trioxide or yttrium oxide or gadolinium sesquioxide, ytterbium oxide, Erbium trioxide or trioxide or Holmium trioxide, be dissolved in wiring solution-forming in hydrochloric acid or the nitric acid, heating for dissolving, making solution middle-weight rare earths ion mol ratio is lanthanum ion (ruthenium ion or gadolinium ion): ytterbium ion: erbium ion (thulium ion or holmium ion)=70-90: 0-29: 0.001-15, volatilization is done, and removes remaining hydrochloric acid or nitric acid;
(2) above-mentioned product is dissolved in water, and adds the doubly ammonia carboxylic class complexing agent of total rare earth (TRE) ionic weight in solution of 0-2;
(3) stir fast down, Sodium orthomolybdate or potassium molybdate solution are added in the above-mentioned solution, generate creaming;
(4) centrifugation precipitates and washes with water, makes hydrogel;
(5) hydrogel is put into High Temperature Furnaces Heating Apparatus as presoma,, promptly get the nano level upconverting fluorescent material 400-1100 ℃ of calcining 1-10 hour.
The solution of configuration can directly be prepared with the soluble salt of rare earth described in this step in above-mentioned steps (1).
The used ammonia carboxylic class complexing agent of step (2) is any in ethylenediamine tetraacetic acid (EDTA), disodium EDTA, diethylenetriamine pentaacetic acid or the hydroxyethylethylene diamine tri-acetic acid.
After making hydrogel in the step (4), also available alcohol soaks or alcogel is made in boiling.
The hydrogel that step (5) also can make step (4) is dispersed in to be poured in the water in the water heating kettle, 150-200 ℃ hydro-thermal reaction 1-10 hour, also can make the nano level upconverting fluorescent material.
Zhi Bei nanometer level molybdate substrate upconverting fluorescent material according to the method described above, with lanthanum molybdate (yttrium molybdate or gadolinium molydbate) is matrix, also be doped with molybdic acid ytterbium, molybdic acid erbium (molybdic acid thulium or molybdic acid holmium), the mol ratio of its rare earth ion is lanthanum ion (ruthenium ion or a gadolinium ion): ytterbium ion: erbium ion (thulium ion or holmium ion)=70-90: 0-29: 0.001-15.
Utilize this method to prepare upconverting fluorescent material, have the following advantages:
(1) prepared material particle size can reach nano level, and is little and even, and median size is 50-60nm;
(2) luminous intensity is big, and light intensity strengthens about 30%;
(3) calcining temperature is low, is reduced to 400-1100 ℃ by common 1200 ℃;
(4) raw material is inexpensive, and technology is simple, and cost is lower.
Description of drawings:
Fig. 1 is the La that utilizes present method preparation
2(MoO
4)
3: Yb, the up-conversion fluorescence spectrographic contrast of Er nanometer upconverting fluorescent material and non-nano upconverting fluorescent material material, solid line 1 is for utilizing the La of present method preparation among the figure
2(MoO
4)
3: Yb, the up-conversion fluorescence spectrum of Er nanometer upconverting fluorescent material, dotted line 2 is the up-conversion fluorescence spectrum of non-nano upconverting fluorescent material material among the figure.
Fig. 2 is the La that utilizes present method preparation
2(MoO
4)
3: Yb, the transmission electron microscope picture of Er nanometer upconverting fluorescent material.
Embodiment:
Embodiment one:
(1) takes by weighing 1.1760g lanthanum trioxide (La
2O
3), 0.3692g ytterbium oxide (Yb
20
3), 0.0537g Erbium trioxide (Er
2O
3), place the 100ml beaker, add 2ml concentrated nitric acid (HNO
3) heating for dissolving, this moment, the mol ratio of rare earth ion was La
3+: Yb
3+: Er
3+=77: 20: 3, volatilization was done, and removes remaining HNO
3
(2) above-mentioned product is added the 30ml deionized water dissolving, change in the 100ml there-necked flask;
(3) stir fast down, sodium molybdate solution is splashed in the above-mentioned there-necked flask, generate creaming;
(4) centrifugation precipitates and washes with water three times, makes hydrogel;
(5) hydrogel is put into High Temperature Furnaces Heating Apparatus as presoma,, promptly get the nano level upconverting fluorescent material, this material median size 50nm 800 ℃ of calcinings 5 hours.
Embodiment two:
(1) takes by weighing 1.1760g lanthanum trioxide (La
2O
3), 0.3692g ytterbium oxide (Yb
2O
3), 0.0537g Erbium trioxide (Er
2O
3), place the 100ml beaker, add 2ml concentrated hydrochloric acid (HCl) heating for dissolving, this moment, the mol ratio of rare earth ion was La
3+: Yb
3+: Er
3+=77: 20: 3, volatilization was done, and removes remaining hydrochloric acid;
(2) above-mentioned product is added the 30ml deionized water dissolving, change in the 100ml there-necked flask;
(3) under stirring fast, potassium molybdate solution is splashed in the above-mentioned there-necked flask, generate creaming;
(4) centrifugation precipitates and washes with water three times, makes hydrogel;
(5) in the hydrogel that makes, add alcohol immersion, make alcogel;
(6) prepared alcogel is put into High Temperature Furnaces Heating Apparatus,, promptly get the nano level upconverting fluorescent material, this material median size 60nm 400 ℃ of calcinings 10 hours.
Embodiment three:
(1) measure Lanthanum trichloride, Ytterbium trichloride, Erbium trichloride and be mixed with 25ml solution, making the rare earth ion mol ratio is La
3+: Yb
3+: Er
3+=70.29: 1, the rare earth ion total concn is 0.04mol/L, places there-necked flask;
(2) ethylenediamine tetraacetic acid (EDTA) (EDTA) solution of adding 5ml 0.2mol/L makes the abundant complexing of EDTA and rare earth ion;
(3) under stirring fast, sodium molybdate solution is injected into rapidly in the above-mentioned there-necked flask, generates creaming;
(4) in the hydrogel that makes, add the ethanol boiling and make alcogel;
(5) alcogel of making is put into High Temperature Furnaces Heating Apparatus as presoma,, promptly get the nano level upconverting fluorescent material 1100 ℃ of calcinings 1 hour.
Embodiment four:
(1) measure Yttrium trichloride, Ytterbium trichloride, thulium chloride and be mixed with 25ml solution, making the rare earth ion mol ratio is Y
3+: Yb
3+: Tm
3+=87: 12.999: 0.001, the rare earth ion total concn was 0.04mol/L, places there-necked flask;
(2) ethylenediamine tetraacetic acid (EDTA) (EDTA) of adding 5ml 0.2mol/L makes the abundant complexing of EDTA and rare earth ion;
(3) under stirring fast, sodium molybdate solution is injected into rapidly in the above-mentioned there-necked flask, generates creaming;
(4) in the hydrogel that makes, add alcohol immersion and make alcogel;
(5) hydrogel is put into High Temperature Furnaces Heating Apparatus as presoma,, promptly get the nano level upconverting fluorescent material 800 ℃ of calcinings 1 hour.
Embodiment five:
(1) measure Yttrium trichloride, Ytterbium trichloride, Holmium trichloride and be mixed with 25ml solution, making the rare earth ion mol ratio is Y
3+: Yb
3+: Ho
3+=90: 9.8: 0.2, the rare earth ion total concn was 0.04mol/L, places there-necked flask;
(2) diethylenetriamine pentaacetic acid (DTPA) solution of adding 10ml 0.2mol/L makes the abundant complexing of DTPA and rare earth ion;
(3) under stirring fast, sodium molybdate solution is injected into rapidly in the above-mentioned there-necked flask, generates creaming;
(4) in the hydrogel that makes, add alcohol immersion and make alcogel;
(5) hydrogel is put into High Temperature Furnaces Heating Apparatus as presoma,, promptly get the nano level upconverting fluorescent material 800 ℃ of calcinings 5 hours.Embodiment six:
(1) measure Yttrium trichloride, Holmium trichloride is mixed with 25ml solution, making the rare earth ion mol ratio is Y
3+: Ho
3+=85: 15, the rare earth ion total concn is 0.04mol/L, places there-necked flask;
(2) disodium ethylene diamine tetraacetate (EDTA) solution of adding 5ml 0.2mol/L makes the abundant complexing of EDTA and rare earth ion;
(3) under stirring fast, sodium molybdate solution is injected into rapidly in the above-mentioned there-necked flask, generates creaming;
(4) centrifugation precipitates and washes with water three times, makes hydrogel;
(5) hydrogel is dispersed in the 40ml water pours in the water heating kettle as presoma, 150 ℃ of hydro-thermal reactions 10 hours make the nano level upconverting fluorescent material.
Embodiment seven:
(1) measure Gadolinium trichloride, Ytterbium trichloride, Holmium trichloride and be mixed with 25ml solution, making rare earth ion muriate mol ratio is Gd
3+: Yb
3+: Ho
3+=80: 19.8: 0.2, the rare earth ion total concn was 0.04mol/L, places there-necked flask;
(2) hydroxyethylethylene diamine tri-acetic acid (HEDTA) solution of adding 5ml 0.2mol/L makes the abundant complexing of HEDTA and rare earth ion;
(3) under stirring fast, sodium molybdate solution is added rapidly in the above-mentioned there-necked flask, generate creaming;
(4) centrifugation precipitates and washes with water three times, makes hydrogel;
(5) hydrogel is dispersed in the 40ml water pours in the water heating kettle as presoma, 200 ℃ of hydro-thermal reactions 1 hour make the nano level upconverting fluorescent material.
Embodiment eight:
(1) measure Gadolinium trichloride, Ytterbium trichloride, Holmium trichloride and be mixed with 25ml solution, making rare earth ion muriate mol ratio is Gd
3+: Yb
3+: Ho
3+=80: 19.8: 0.2, the rare earth ion total concn was 0.04mol/L, places there-necked flask;
(2) hydroxyethylethylene diamine tri-acetic acid (HEDTA) solution of adding 5ml 0.2mol/L makes the abundant complexing of HEDTA and rare earth ion;
(3) under stirring fast, sodium molybdate solution is added rapidly in the above-mentioned there-necked flask, generate creaming;
(4) wash also centrifugation with water, make hydrogel;
(5) hydrogel is dispersed in the 40ml water pours in the water heating kettle as presoma, 180 ℃ of hydro-thermal reactions 5 hours make the nano level upconverting fluorescent material.
Claims (6)
1, a kind of method for preparing the nanometer level molybdate substrate upconverting fluorescent material is characterized in that comprising following steps:
(1) with lanthanum trioxide or yttrium oxide or gadolinium sesquioxide, ytterbium oxide, Erbium trioxide or trioxide or Holmium trioxide, be dissolved in wiring solution-forming in hydrochloric acid or the nitric acid, heating for dissolving, making solution middle-weight rare earths ion mol ratio is lanthanum ion (ruthenium ion or gadolinium ion): ytterbium ion: erbium ion (thulium ion or holmium ion)=70-90: 0-29: 0.001-15, volatilization is done, and removes remaining hydrochloric acid or nitric acid;
(2) above-mentioned product is dissolved in water, and adds the doubly ammonia carboxylic class complexing agent of total rare earth (TRE) ionic weight in solution of 0-2;
(3) stir fast down, Sodium orthomolybdate or potassium molybdate solution are added in the above-mentioned solution, generate creaming;
(4) centrifugation precipitates and washes with water, makes hydrogel;
(5) hydrogel is put into High Temperature Furnaces Heating Apparatus as presoma,, promptly get the nano level upconverting fluorescent material 400-1100 ℃ of calcining 1-10 hour.
2,, it is characterized in that the solution of configuration in the above-mentioned steps (1) can directly be prepared with the soluble salt of rare earth described in this step according to the described preparation method of claim 1.
3,, it is characterized in that the described ammonia carboxylic of above-mentioned steps (2) class complexing agent is any in ethylenediamine tetraacetic acid (EDTA), disodium EDTA, second pentaacetic acid or the hydroxyethylethylene diamine tri-acetic acid according to claim 1 or 2 described preparation methods.
4, according to claim 1 or 2 described preparation methods, after it is characterized in that making hydrogel according to step (4), alcogel is made in also available alcohol immersion or boiling.
5, according to claim 1 or 2 described preparation methods, it is characterized in that hydrogel that described step (5) also can make step (4) is dispersed in pours in the water heating kettle in the water, 150-200 ℃ hydro-thermal reaction 1-10 hour, also can make the nano level upconverting fluorescent material.
6, adopt a kind of nanometer level molybdate substrate upconverting fluorescent material of method preparation according to claim 1, it is characterized in that this material is is matrix with lanthanum molybdate (or yttrium molybdate or gadolinium molydbate), also be doped with molybdic acid ytterbium, molybdic acid erbium (molybdic acid thulium or molybdic acid holmium), the mol ratio of its rare earth ion is lanthanum ion (ruthenium ion or a gadolinium ion): ytterbium ion: erbium ion (thulium ion or holmium ion)=70-90: 0-29: 0.001-15.
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|---|---|---|---|
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|---|---|---|---|
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