CN107720802A - A kind of preparation method for independently filling monodispersed luteium oxide nanosphere - Google Patents
A kind of preparation method for independently filling monodispersed luteium oxide nanosphere Download PDFInfo
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Abstract
The present invention discloses one kind and independently fills monodispersed Lu2O3The preparation method of nanosphere, i.e., the aqueous solution of urea and rare earth lutecium nitrate is well mixed, the total concentration for obtaining controlling lutetium ion in mixed solution is 0.018mol/L, urea concentration is 0.5 1.0mol/L；Gained mixed solution is heated to stop heating when constant temperature after micro-boiling is reacted and rises to 6.0 7.0 to reaction solution pH, naturally cool to room temperature, gained gelatinous precipitate is washed, dried and calcined successively, sphere diameter is produced and independently fills monodispersed Lu for 100 300nm2O3Nanosphere.The preparation method applies also for the Lu with up-conversion luminescence performance2O3The preparation of nanosphere, the monodispersed Lu of self assembly of the simple gained of this method preparation technology2O3Nanosphere regular appearance, size uniformity, it is expected to the luminous host material as transformational marker on a kind of new bioluminescence.
Description
Technical field
The present invention relates to a kind of preparation method of the monodispersed luteium oxide nanosphere of self assembly, belongs to luminescent material technology neck
Domain.
Background technology
Rare earth oxide is a kind of new function material, and they are widely used in high-performance fluorescent material, catalyst, upper conversion material
The field of functional materials such as material.Luteium oxide (Lu2O3) matrix has the absorption coefficient of light of high density high, from crystal structure
See, have band gap is very wide (6.5 eV) between cubic system band and conduction band, a variety of rare earth activators can be accommodated from giving, be advantageous to
The design of difference composition luminescence system.Lutecia based transparent ceramics material is expected to play pass in the digital radial imaging system in future
Key acts on, particularly suitable for the application in terms of static number imaging and fluoroscopy.High-performance luteium oxide fluorescent material is prepared then
Ask luteium oxide powder that there is the characteristics such as regular spherical morphology, narrow Size Distribution, good dispersiveness.
The method master for preparing lutetium base nano-powder at present has synthesis by solid state reaction, sol-gal process, chemical coprecipitation
Deng.
Reaction temperature higher than 1600 DEG C is needed using synthesis by solid state reaction, and needs the longer reaction time, and
And the more difficult single pure phase of acquisition.
The preparation of gel and the more difficult control of drying process in sol-gal process.Using coprecipitation process, precipitating reagent adds
Enter, the control technique such as pH controls and ageing, calcining is more and requires fine, gained nano powder or ball particle diameter distribution not enough uniformly,
Bad dispersibility.
The self assembly lutetium base nanosphere of directly micro-boiling method synthesis proposed by the present invention it is spherical it is regular, size is homogeneous, scattered
Property it is good, coordinate it is rear-earth-doped regulation and control chemical constituent obtained by lutetium base nanosphere be a kind of preferable biological fluorescence material, be expected to use
In biological fluorescent labelling or imaging.
The content of the invention
The invention aims to solve synthesis by solid state reaction, sol-gal process, coprecipitation synthesis oxidation
The synthesis temperature of lutetium nanosphere is high, pattern is irregular, and particle diameter is uneven, the technical problem such as bad dispersibility and a kind of autonomous dress is provided
Single dispersing Lu2O3The preparation method of nanosphere, the preparation method have the autonomous dress single dispersing Lu that synthesis temperature is low, obtains2O3Receive
The advantages that rice ball powder granule pattern spherical in shape, sphere diameter size uniformity are controllable, good dispersion.
Building-up process is very simple, control technological parameter is few.Urea is gradually decomposed alkalescence by this method under the conditions of micro-boiling
Precipitating reagent, be advantageous to uniform mono-dispersed nano ball and prepare.
The technical principle of the present invention
A kind of uniformly monodispersed Lu2O3The preparation method of nanosphere, urea and lutecium nitrate solution are uniformly mixed, in micro-boiling bar
It is alkaline precipitating agent to make the slow uniform decomposition of urea under part, with Lu3+Ion, which reacts, generates lutetium based compound presoma.Reaction
Process urea decomposes slowly to precipitating reagent, makes nucleation process evenly, avoids the too high generation implode of precipitant concentration.Reacted
Journey is a kind of bead self assembling process, is advantageous to obtain pattern rule, size uniform luteium oxide nanosphere, the autonomous dress list of synthesis
Scattered Lu2O3Nanosphere size is between 100-300nm.Compared with ammonium hydrogen carbonate coprecipitation, this method is simple to operate,
Course of reaction is easily controlled, obtained luteium oxide fluorescent material uniform particle sizes, pattern rule, good dispersion.
Technical scheme
One kind independently fills monodispersed Lu2O3The preparation method of nanosphere, specifically comprises the following steps：
（1）, by urea be added in rare earth nitrate aqueous solution and it is well mixed after, obtain mixed solution；
Described rare earth nitrate aqueous solution is the lutecium nitrate aqueous solution；
In the mixed solution of above-mentioned gained, it is 0.5-1.0mol/L, preferably 1.0mol/L to control urea concentration；Control lutetium ion
Concentration be 0.018mol/L；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid pH rises to 6.0-7.0
When or isothermal reaction 30min stop heating, stop heating when preferably pH rises to 6.0, then naturally cool to room temperature, obtain glue
Shape precipitates；
（3）, by step（2）The gelatinous precipitate of gained is washed with deionized water, absolute ethyl alcohol successively；
Repeat to control temperature to be 60 DEG C after above-mentioned washing operation 4-6 time and dried, obtain lutetium based compound presoma, then control
Temperature processed is 800-1000 DEG C and carries out calcining 0.5-4h, preferably controls temperature to carry out calcining 2h for 1000 DEG C, produces sphere diameter
Monodispersed Lu is independently filled for 100-300nm2O3Nanosphere.
Above-mentioned autonomous dress single dispersing Lu2O3The preparation method of nanosphere, works as step（1）In the mixed solution of gained, except nitre
Outside sour lutetium, also contain thulium nitrate；Or in addition to lutecium nitrate, also contain ytterbium nitrate；Or in addition to lutecium nitrate, also simultaneously containing thulium nitrate with
During ytterbium nitrate, available for the Lu for preparing optical property of being turned blue with upper conversion2O3Nanosphere；
Work as above-mentioned steps（1）In the mixed solution of gained, in addition to lutecium nitrate, when also containing thulium nitrate with ytterbium nitrate simultaneously, control
Urea concentration is 1.0 mol/L in mixed solution, while it is 0.018mol/ to control the total concentration of the rare earth ion in mixed solution
L, the amount of each rare earth ion, for calculation in the molar ratio, lutetium ion：Thulium ion, ytterbium ion 99.9-x:0.1:X, wherein x=1-2；
Work as above-mentioned steps（1）In the mixed solution of gained, in addition to lutecium nitrate, also containing thulium nitrate when, control mixed solution in urinate
Plain concentration is 1.0 mol/L, while the total concentration of the rare earth ion in mixed solution is 0.018mol/L, each rare earth ion
Amount, for calculation in the molar ratio, preferred lutetium ion：Thulium ion is 99.9:0.1；
Work as above-mentioned steps（1）In the mixed solution of gained, in addition to lutecium nitrate, also containing ytterbium nitrate when, control mixed solution in urinate
Plain concentration is 1.0 mol/L, while it is 0.018mol/L to control the total concentration of the rare earth ion in mixed solution, each rare earth ion
Amount, for calculation in the molar ratio, lutetium ion：Ytterbium ion is 100-y：Y, wherein y=1-2.
Only with above-mentioned steps in the present invention（1）In the mixed solution of gained, in addition to lutecium nitrate, also also contain thulium nitrate simultaneously
With during ytterbium nitrate obtained by the Lu for independently filling monodispersed thulium ion, ytterbium ion codope2O3It is illustrated exemplified by nanosphere,
But it is not intended to limit step（1）The mixed solution of gained, in addition to lutecium nitrate, also contain thulium nitrate, or in addition to lutecium nitrate, contain nitric acid
The application of ytterbium.
The uniform monodispersed Lu of above-mentioned gained2O3Nanosphere, it can be seen that the chi of luteium oxide nanosphere from surface sweeping electron microscope
It is very little between 100-300, between preferably 150-200nm, microscopic appearance is regular, and monodispersity is fine.It is coprecipitated with ammonium hydrogen carbonate
Shallow lake method is compared, and Powder by Homogenous Precipitation is more suitable for uniform monodispersed lutetium base nanosphere because of the self-assembling reaction of course of reaction
Prepare.
Beneficial effects of the present invention
A kind of uniformly monodispersed Lu of the present invention2O3The preparation method of nanosphere, urea and lutecium nitrate solution are uniformly mixed,
Reaction is self-assembled into uniform monodispersed Lu under the conditions of micro-boiling2O3Nanosphere.This method has evaded ammonium hydrogen carbonate coprecipitation powder
The technical problems such as body particle size is uneven, bad dispersibility.
Further, a kind of uniformly monodispersed Lu of the invention2O3The preparation method of nano-phosphor, urinate in course of reaction
Element decomposes slowly to precipitating reagent, avoids the implode caused by precipitant concentration is too high of ammonium hydrogen carbonate coprecipitation, can obtain shape
Looks are regular, size uniform, monodispersed particle diameter are 100-300nm, preferably 150-200nm Lu2O3Nanosphere.
Brief description of the drawings
The concentration of urea is independently to fill monodispersed Lu obtained by 0.5mol/L in Fig. 1, embodiment 12O3The SEM of nanosphere
Pattern；
The concentration of urea is independently to fill monodispersed Lu obtained by 1.0mol/L in Fig. 2, embodiment 22O3The SEM shapes of nanosphere
Looks；
The pH value of reaction end is controlled independently to fill monodispersed Lu for 6.0 gained in Fig. 3, embodiment 32O3The SEM of nanosphere
Figure；
The pH value of reaction end is controlled independently to fill monodispersed Lu for 7.0 gained in Fig. 4, embodiment 42O3The SEM of nanosphere
Figure；
Monodispersed thulium ion, the Lu of ytterbium ion codope are independently filled obtained by Fig. 5, embodiment 5,62O3The TEM figures of nanosphere；
Monodispersed thulium ion, the Lu of ytterbium ion codope are independently filled obtained by Fig. 6, embodiment 5,62O3The upper conversion of nanosphere
Fluorescent emission spectrogram.
Embodiment
The present invention is expanded on further by way of example and in conjunction with the accompanying drawings, but is not intended to limit the present invention.
In various embodiments of the present invention, monodispersed Lu is independently filled2O3Nanosphere and independently fill monodispersed thulium ion, ytterbium
Ion co-doped Lu2O3The morphology observation of nanosphere is using field emission scanning electron microscope（FESEM Japan JEOL is public
Take charge of JSM-6700F）.What is be analysed to before observation independently fills monodispersed Lu2O3Nanosphere and independently fill monodispersed thulium ion,
The Lu of ytterbium ion codope2O3Nanosphere powder is uniformly sprayed on conducting resinl, through steaming gold（Au）It is placed in after processing on sample stage,
Carry out SEM signs；
Embodiment 1
One kind independently fills monodispersed Lu2O3The preparation method of nanosphere, specifically comprises the following steps：
（1）, urea is added in the rare earth lutecium nitrate aqueous solution and it is well mixed after, obtain mixed solution；
In above-mentioned gained mixed solution, the concentration that controls lutetium ion is 0.018mol/L, urea concentration 0.5mol/L；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid isothermal reaction 30min stops
Only heat, then naturally cool to room temperature, obtain gelatinous precipitate；
（3）, by step（2）The gelatinous precipitate of gained is washed with deionized water, absolute ethyl alcohol successively；
Repeat to control temperature to be 60 DEG C after above-mentioned washing operation 4-6 time and dried to obtain lutetium based compound presoma, then controlled
Temperature processed is 1000 DEG C and carries out calcining 2h, produces and independently fills monodispersed Lu2O3Nanosphere.
Embodiment 2
One kind independently fills monodispersed Lu2O3The preparation method of nanosphere, specifically comprises the following steps：
（1）, urea is added in the rare earth lutecium nitrate aqueous solution and it is well mixed after, obtain mixed solution；
In above-mentioned gained mixed solution, the concentration that controls lutetium ion is 0.018mol/L, urea concentration 1.0mol/L；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid isothermal reaction 30min stops
Only heat, then naturally cool to room temperature, obtain gelatinous precipitate；
（3）, by step（2）The gelatinous precipitate of gained is washed with deionized water, absolute ethyl alcohol successively；
Repeat to control temperature to be 60 DEG C after above-mentioned washing operation 4-6 time and dried to obtain lutetium based compound presoma, then controlled
Temperature processed is 1000 DEG C and carries out calcining 2h, produces and independently fills monodispersed Lu2O3Nanosphere.
Monodispersed Lu will be independently filled obtained by embodiment 1 and embodiment 22O3Nanosphere, electricity is scanned by Flied emission respectively
Its microstructure of sem observation, gained SEM schemes as shown in Figure 1 and Figure 2, it can be seen that embodiment 1 and the institute of embodiment 2 from Fig. 1, Fig. 2
What is obtained independently fills monodispersed Lu2O3Nanometer ball particle is regular spherical, and size distribution is good, in single dispersing trend.Embodiment 1
Gained independently fills monodispersed Lu2O3Nanosphere particle size difference is larger, and wherein bead size is and big about in 100nm or so
Ball size is about 300nm, and bead proportion is larger, and spheroid uniformity is slightly poor；
The gained of embodiment 2 independently fills monodispersed Lu2O3The particle size of nanosphere nanosphere is relatively uniform, and particle diameter is tieed up substantially
Hold between 150-250nm, bead proportion is relatively fewer, and distribution of particles is narrower.
In summary, it is believed that urea concentration be 1.0 mol/L be more suitable for self assembly it is monodispersed independently fill it is monodispersed
Lu2O3The preparation of nanosphere.
Embodiment 3
One kind independently fills monodispersed Lu2O3The preparation method of nanosphere, specifically comprises the following steps：
（1）, urea is added in the rare earth lutecium nitrate aqueous solution and it is well mixed after, obtain mixed solution；
In above-mentioned gained mixed solution, the concentration that controls lutetium ion is 0.018mol/L, urea concentration 1.0mol/L；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid pH stops when rising to 6.0
Only heat, then naturally cool to room temperature, obtain gelatinous precipitate；
（3）, by step（2）The gelatinous precipitate of gained is washed with deionized water, absolute ethyl alcohol successively；
Repeat to control temperature to be 60 DEG C after above-mentioned washing operation 4-6 time and dried to obtain lutetium based compound presoma, then controlled
Temperature processed is 1000 DEG C and carries out calcining 2h, produces and independently fills monodispersed Lu2O3Nanosphere.
Embodiment 4
One kind independently fills monodispersed Lu2O3The preparation method of nanosphere, specifically comprises the following steps：
（1）, urea is added in the rare earth lutecium nitrate aqueous solution and it is well mixed after, obtain mixed solution；
In above-mentioned gained mixed solution, the concentration that controls lutetium ion is 0.018mol/L, urea concentration 1.0mol/L；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid pH stops when rising to 7.0
Only heat, then naturally cool to room temperature, obtain gelatinous precipitate；
（3）, by step（2）The gelatinous precipitate of gained carries out 4-6 rear control temperature of diafiltration with deionized water, absolute ethyl alcohol successively
Dried to obtain lutetium based compound presoma for 60 DEG C, then control temperature to carry out calcining 2h for 1000 DEG C, produce autonomous dress
Monodispersed Lu2O3Nanosphere.
Monodispersed Lu will be independently filled obtained by embodiment 3 and embodiment 42O3Nanosphere carries out pattern table by SEM respectively
Sign, gained SEM scheme as shown in Figure 3, Figure 4, as can be seen from Figure 3 independently fill monodispersed Lu obtained by embodiment 32O3Nanometer
Ball is uniformly dispersed, disperseed in single, and particle size is about 150nm or so, is not reunited significantly.
The gained of embodiment 4 independently fills monodispersed Lu2O3The size of nanosphere is larger and particle diameter distribution is uneven, size
About between 100-300nm, and there is a small amount of cotton-shaped agglomeration, bead size is about 100nm, and big ball size is about 300nm, is deposited
It is slightly poor in certain sphere diameter size mismatch, dispersiveness.
Embodiment 5
A kind of Lu with up-conversion luminescence performance2O3Nanosphere, i.e., independently fill monodispersed thulium ion, ytterbium ion codope
Lu2O3The preparation method of nanosphere, specifically comprises the following steps：
（1）, urea is added in the rare earth nitrate aqueous solution being made up of rare earth lutecium nitrate, thulium nitrate with ytterbium nitrate and mixed
After uniformly, mixed solution is obtained；
The total concentration that rare earth lutetium ion, thulium ion and ytterbium ion are controlled in the mixed solution of above-mentioned gained is 0.018 mol/L, urine
Plain concentration is 1.0 mol/L;
The amount of each rare earth ion in mixed solution, for calculation in the molar ratio, lutetium ion：Thulium ion：Ytterbium ion is 98.9：0.1：1；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid pH rises to 6.0 stoppings
Heating, then naturally cools to room temperature, obtains gelatinous precipitate；
（3）, by step（2）The gelatinous precipitate of gained is washed with deionized water, absolute ethyl alcohol successively；
Control temperature to obtain lutetium based compound presoma for 60 DEG C after repeating above-mentioned washing operation 4-6 time, then control the temperature to be
1000 DEG C carry out calcining 2h, produce and independently fill monodispersed thulium ion, the Lu of ytterbium ion codope2O3Nanosphere.
Embodiment 6
A kind of Lu with up-conversion luminescence performance2O3Nanosphere, i.e., independently fill monodispersed thulium ion, ytterbium ion codope
Lu2O3The preparation method of nanosphere, specifically comprises the following steps：
（1）, urea is added in the rare earth nitrate aqueous solution being made up of rare earth lutecium nitrate, thulium nitrate with ytterbium nitrate and mixed
After uniformly, mixed solution is obtained；
The total concentration that rare earth lutetium ion, thulium ion and ytterbium ion are controlled in the mixed solution of above-mentioned gained is 0.018 mol/L, urine
Plain concentration is 1.0 mol/L;
The amount of each rare earth ion in mixed solution, for calculation in the molar ratio, lutetium ion：Thulium ion：Ytterbium ion is 97.9：0.1：2；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid pH rises to 6.0 stoppings
Heating, then naturally cools to room temperature, obtains gelatinous precipitate；
（3）, by step（2）The gelatinous precipitate of gained is washed with deionized water, absolute ethyl alcohol successively；
Repeat to control temperature to be 60 DEG C after above-mentioned washing operation 4-6 time and dried, obtain lutetium based compound presoma, then control
Temperature processed is 1000 DEG C and carries out calcining 2h, produces and independently fills monodispersed thulium ion, the Lu of ytterbium ion codope2O3Nanosphere.
By the thulium ion of the gained of embodiment 5,6, the Lu of ytterbium ion codope2O3Nanosphere carries out morphology characterization by TEM,
Gained SEM schemes as shown in figure 5, the lutetium base nanometer that as can be seen from Figure 5 thulium ion, the ytterbium ion of the gained of embodiment 5,6 are co-doped with
Ball is uniformly dispersed, disperseed in single, and particle size is about 150nm or so, is not reunited significantly.
Using Edinburgh, Britain FLSP-920 XRFs to the thulium ion of above-described embodiment 5 and the gained of embodiment 6,
The Lu of ytterbium ion codope2O3Nanosphere sample carries out up-conversion luminescence performance measurement, and the up-conversion fluorescence transmitting spectrogram of gained is such as
Shown in Fig. 6, from fig. 6 it can be seen that in the case where 980nm near infrared lights excite, thulium ion, the ytterbium of embodiment 5 and the gained of embodiment 6
Ion co-doped Lu2O3The equal blue light-emitting of nanosphere sample, thulium ion, the Lu of ytterbium ion codope of the gained of embodiment 62O3Receive
Rice ball sample is than the thulium ion of the gained of embodiment 5, the Lu of ytterbium ion codope2O3The blue light that nanosphere sample is sent is stronger；From glimmering
Light spectrogram can also see that in 477nm and 490nm, all fall within blue spectral range.And the thulium ion of the gained of embodiment 6, ytterbium from
The Lu of sub- codope2O3Nanosphere sample is than the thulium ion of the gained of embodiment 5, the Lu of ytterbium ion codope2O3Nanosphere sample is special
The more of peak intensity are levied, illustrate that ytterbium ion plays critical effect to up-conversion luminescence efficiency as activator, its doping concentration, because
This preparation method of the invention, can be by preparation process（1）The chemical constituent of rare-earth cation in middle mixed solution is adjusted
Convenience on section is luminous with very big advantage with high efficiency blue up-conversion for synthesis.
In summary, a kind of uniformly monodispersed Lu of the invention2O3The preparation method of nanosphere, method operation, equipment letter
Singly, it is irregular to overcome the luteium oxide powder granule pattern of ammonium hydrogen carbonate coprecipitation preparation, reunites the shortcomings that serious, can obtain
Uniform particle sizes, its particle diameter are about 100-300nm, preferably 150-200nm, and pattern rule, uniform monodispersed Lu2O3Nanometer
Ball.
Above said content is only the basic explanation under present inventive concept, and is appointed according to what technical scheme was made
What equivalent transformation, all should belong to protection scope of the present invention.
Claims (9)
1. one kind independently fills monodispersed Lu2O3The preparation method of nanosphere, it is characterised in that specifically comprise the following steps：
（1）, by urea be added in rare earth nitrate aqueous solution and it is well mixed after, obtain mixed solution；
Described rare earth nitrate aqueous solution is the lutecium nitrate aqueous solution；
In the mixed solution of above-mentioned gained, it is 0.5-1.0mol/L to control urea concentration, and the concentration for controlling lutetium ion is
0.018mol/L；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid pH rises to 6.0-7.0
When or isothermal reaction 30min stop heating, then naturally cool to room temperature, obtain gelatinous precipitate；
（3）, by step（2）The gelatinous precipitate of gained is washed with deionized water, absolute ethyl alcohol successively；
Repeat to control temperature to be 60 DEG C after above-mentioned washing operation 4-6 time and dried, the lutetium based compound forerunner that then will be obtained
Body controls temperature to carry out calcining 0.5-4h for 800-1000 DEG C, that is, obtains the autonomous dress single dispersing that sphere diameter is 100-300nm
Lu2O3Nanosphere.
2. autonomous dress single dispersing Lu as claimed in claim 12O3The preparation method of nanosphere, it is characterised in that step（1）In mix
Close in solution, it is 1.0mol/L to control urea concentration.
3. autonomous dress single dispersing Lu as claimed in claim 22O3The preparation method of nanosphere, it is characterised in that step（2）In treat
Reaction solution pH stops heating when rising to 6.0.
4. autonomous dress single dispersing Lu as claimed in claim 32O3The preparation method of nanosphere, it is characterised in that step（3）It is middle to incite somebody to action
Obtained lutetium based compound precursor controlling temperature is 1000 DEG C and carries out calcining 2h.
5. autonomous dress single dispersing Lu as claimed in claim 42O3The preparation method of nanosphere, it is characterised in that step（3）In
To sphere diameter monodispersed Lu is independently filled for 150-200nm2O3Nanosphere.
6. autonomous dress single dispersing Lu as claimed in claim 12O3The preparation method of nanosphere is applied to have up-conversion luminescence
The Lu of energy2O3The preparation of nanosphere, it is characterised in that comprise the following steps that：
（1）, by urea be added in rare earth nitrate aqueous solution and it is well mixed after, obtain mixed solution；
Described rare earth nitrate aqueous solution is the rare earth nitrate aqueous solution containing lutecium nitrate and thulium nitrate, or to contain nitric acid
The rare earth nitrate aqueous solution of lutetium and ytterbium nitrate, or be the rare earth nitrate aqueous solution containing lutecium nitrate, thulium nitrate and ytterbium nitrate；
In the mixed solution of above-mentioned gained, it is 1.0 mol/L to control urea concentration, while controls the total concentration of rare earth ion to be
0.018 mol/L；
When in the mixed solution of above-mentioned gained, in addition to lutecium nitrate, also simultaneously containing thulium nitrate with ytterbium nitrate when, it is each in mixed solution
The amount of rare earth ion, for calculation in the molar ratio, lutetium ion：Thulium ion, ytterbium ion 99.9-x:0.1:X, wherein x=1-2；
When in the mixed solution of above-mentioned gained, in addition to lutecium nitrate, also containing thulium nitrate when, each rare earth ion in mixed solution
Amount, for calculation in the molar ratio, lutetium ion：Thulium ion is 99.9:0.1；
When in the mixed solution of above-mentioned gained, in addition to lutecium nitrate, also containing ytterbium nitrate when, each rare earth ion in mixed solution
Amount, for calculation in the molar ratio, lutetium ion：Ytterbium ion is 100-y：Y, wherein y=1-2；
（2）, by step（1）Constant temperature is reacted after gained mixed solution is heated to micro-boiling, and question response liquid pH rises to 6.0-7.0
When or isothermal reaction 30min stop heating, then naturally cool to room temperature, obtain gelatinous precipitate；
（3）, by step（2）The gelatinous precipitate of gained is washed with deionized water, absolute ethyl alcohol successively；
Repeat to control temperature to be 60 DEG C after above-mentioned washing operation 4-6 time and dried, the lutetium based compound forerunner that then will be obtained
Body controls temperature to carry out calcining 0.5-4h for 800-1000 DEG C, i.e. sphere diameter is that independently filling for 100-300nm is monodispersed
Lu2O3Nanosphere.
7. there is the Lu of up-conversion luminescence performance as claimed in claim 62O3The preparation method of nanosphere, it is characterised in that step
Suddenly（1）Described in rare earth nitrate aqueous solution be the rare earth nitrate aqueous solution containing lutecium nitrate, thulium nitrate and ytterbium nitrate；
Step（2）Middle question response liquid pH stops heating when rising to 6.0；
Step（3）It is middle that obtained lutetium based compound precursor controlling temperature is subjected to calcining 2h for 1000 DEG C.
8. there is the Lu of up-conversion luminescence performance as claimed in claim 72O3The preparation method of nanosphere, it is characterised in that step
Suddenly（1）In：The amount of each rare earth ion in mixed solution, for calculation in the molar ratio, lutetium ion：Thulium ion, ytterbium ion 99.9-x:
0.1:X, wherein x=1.
9. there is the Lu of up-conversion luminescence performance as claimed in claim 72O3The preparation method of nanosphere, it is characterised in that step
Suddenly（1）In：The amount of each rare earth ion in mixed solution, for calculation in the molar ratio, lutetium ion：Thulium ion, ytterbium ion 99.9-x:
0.1:X, wherein x=2.
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| Title |
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| RUMIN LI等: "Facile synthesis and multicolor luminescent properties of uniform Lu2O3:Ln (Ln = Eu3+, Tb3+, Yb3+/Er3+, Yb3+/Tm3+, and Yb3+/Ho3+) nanospheres", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
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