CN107674672A - A kind of rear-earth-doped fluorination ferrisodium and preparation method thereof - Google Patents
A kind of rear-earth-doped fluorination ferrisodium and preparation method thereof Download PDFInfo
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- CN107674672A CN107674672A CN201710744663.8A CN201710744663A CN107674672A CN 107674672 A CN107674672 A CN 107674672A CN 201710744663 A CN201710744663 A CN 201710744663A CN 107674672 A CN107674672 A CN 107674672A
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Abstract
The present invention relates to ferroelectric optical field of detecting, and in particular to a kind of rear-earth-doped fluorination ferrisodium and preparation method thereof.A kind of rear-earth-doped fluorination ferrisodium, the rear-earth-doped fluorination ferrisodium is the Eu synthesized using hydro-thermal method3+Adulterate Na3FeF6.This method specifically comprises the following steps：1) Fe (NO are prepared respectively3)3Solution, NaF solution NH4HF2Solution, then three kinds of solution are mixed, be eventually adding HF, stirring obtains Fe (NO3)3Solution；2) Eu (NO are prepared3)3Solution, with Fe (NO3)3Solution is well mixed；3) 1~5ml acetone will be added in mixed solution, reacts 8~24h in temperature is 185~210 DEG C of baking ovens；4) solution is cooled to room temperature, Eu is obtained after eccentric cleaning3+Adulterate Na3FeF6.Na prepared by this method3FeF6With good crystallinity.
Description
Technical field
The present invention relates to ferroelectric optical field of detecting, and in particular to a kind of rear-earth-doped fluorination ferrisodium and its preparation side
Method.
Background technology
Rare earth element has by the 4f5d electron structures not being fully filled with of external world's shielding, the jump between a variety of energy levels
Move and provide strong condition, produce abundant transmitting and absorption spectrum.Rare earth luminescent material has lot of advantages：For example light turns
It is good etc. to change efficiency high, high color purity, high temperature resistant and stability, be widely used in illuminating, show, military affairs, in the field such as medical science.
A3BF6There is the compound of ice crystal stone-type interesting magnetic property, light emitting ionic matrix to cause the concern of many researchers.
At present, He Lijie et al. has synthesized compound N a with hydro-thermal method3FeF6And its magnetic property is studied.Hair
Existing Na3FeF6Under hydrothermal conditions, product has fairly regular geometric shape, and it is ice crystal stone-type compound, has double calcium titaniums
Calcium structure, monoclinic system.Product heats are still stable to 400 DEG C.Magnetic result of study shows, Na3FeF6With special
Anti-ferromagnetism structure.At present, to Na3FeF6Research it is seldom, its unique structure and anti-ferromagnetism are also the spy of new material tool
Point.
Fluorescent powder using fluoride as matrix, chemically stable is good, and raw material are comparatively relatively cheap, phonon energy phase
Than relatively low for, there is maximum electronegativity in institute's periodic table of elements, and fluoride can with it is big absolutely in the periodic table of elements
Most members can be as the matrix of various fluorescent materials using fluoride；Fluoride has special physics and chemical property.At present, state
The interior report on fluoride is seldom, but the research and report on fluoride red fluorescence powder are few.Ferric flouride
Sodium powder end is that unique white powder material, the light emitting ionic characteristics of luminescence are had a great influence by local fields, had in ferrimagnet
Hope and luminescent properties are regulated and controled by outfield, but rare earth ion doped whether can light does not have correlation to report for work.
The content of the invention
The invention aims to solve above-mentioned fluorination ferrisodium rear-earth-doped at present to lack asking for related manufacturing processes
A kind of topic, there is provided rear-earth-doped fluorination ferrisodium and preparation method thereof.
Therefore the applicant by long-term exploration propose it is a kind of prepared in closed reactor using hydro-thermal method it is dilute
The method of the fluorination ferrisodium of soil doping.
In order to reach foregoing invention purpose, the present invention uses following technical scheme：
A kind of rear-earth-doped fluorination ferrisodium, the rear-earth-doped fluorination ferrisodium is the Eu synthesized using hydro-thermal method3+Mix
Miscellaneous Na3FeF6。
Scheme as a further improvement, Eu3+Addition be Na3FeF61-20%.
Scheme as a further improvement, Eu3+Addition be Na3FeF61-8%.
A kind of preparation method of rear-earth-doped fluorination ferrisodium, specifically comprises the following steps：
1) Fe (NO are prepared respectively3)3Solution, NaF solution NH4HF2Solution, then three kinds of solution are mixed, are eventually adding
HF, stirring obtain Fe (NO3)3Solution；
2) Eu (NO are prepared3)3Solution, with Fe (NO3)3Solution is well mixed；
3) 1~5ml acetone will be added in mixed solution, reacts 8~24h in temperature is 185~210 DEG C of baking ovens；
4) solution is cooled to room temperature, Eu is obtained after eccentric cleaning3+Adulterate Na3FeF6。
This method is to use Na3FeF6As matrix, Eu3+Ion prepares different proportion as activator using hydro-thermal method
Doping concentration, it is intended to find the doping ratio of best luminous intensity, be desirably to obtain luminescent properties good chemical stable performance
Red fluorescence powder.
Scheme as a further improvement, specifically comprise the following steps：
1) matrix Na3FeF6The preparation of solution：
0.05~0.2mol/L Fe (NO are prepared respectively3)3Solution, 0.25~1mol/L NaF solution, 0.25~1mol/
L NH4HF2Each 100ml of solution, measure 15ml NaF solution, 15ml Fe (NO respectively with pipette3)3Solution, 45ml's
NH4HF2Solution is placed in same beaker, is eventually adding 3ml HF solution, stirs 10min, obtains depositing Na3FeF6Solution；
2) 0.1mol/L Eu (NO are prepared3)3Solution, by Eu3+:With Fe3+Volume ratio for 1%~20% with deposition
Na3FeF6Solution is well mixed；
3) mixed solution is transferred in reactor, adds 1~5ml acetone, it is anti-in temperature is 185~210 DEG C of baking ovens
Answer 8~24h；
4) solution is cooled to room temperature, then solution is transferred in centrifuge tube；Centrifuge tube is put into centrifuge and centrifuged
20 minutes, rotating speed 8000r/min；After centrifugation once terminates, supernatant is removed, ethanol is added in centrifuge tube or acetone enters
Row secondary centrifuging；Repeat the above steps after secondary centrifuging and centrifuged three times, obtain Na3FeF6:Eu3+Sample, i.e. Eu3+Doping
Na3FeF6。。
This method is to utilize hydro-thermal method synthesis Eu3+Adulterate Na3FeF6Red characteristic fluorescent powder.
A small amount of Eu3+Addition can increase the luminous intensity of fluorescent powder, after the ratio of fluorescent powder is more than 5%, fluorescence
The luminous intensity of powder is with Eu3+Addition, intensity gradually reduces.
Hydro-thermal method：Hydro-thermal method refers to solution being placed in the closed reactor of high pressure, Jie using water as reaction
The reaction under high pressure that matter is carried out.Using some materials under conditions of HTHP, it is changed into solvable special nature from insoluble, makes anti-
It should be able to be carried out under conditions of liquid phase.The advantages of hydro-thermal method is that the temperature of reaction is relatively low, and the particle for reacting the material of gained is equal
One property is relatively good, and reaction is more stable.Experimental method is as follows：Transfer the solution into the reactor that capacity is 100ml, loading
No more than 80%, it is put into electric drying oven with forced convection.
Eu3+The addition of doping is advantageous to show the diffraction maximum of fluorescent powder, it was demonstrated that the material has good crystallization
Property.
Compared with prior art, beneficial effect is the present invention：There is provided a kind of new preparation method, the material of preparation has good
Good crystallinity.
Brief description of the drawings
Fig. 1 is the obtained rear-earth-doped Na in the closed reactor of high pressure of embodiments of the invention 13FeF6Fluorescent material
SEM figure；
Fig. 2 is the XRD spectra of the products therefrom of embodiments of the invention 1；
Fig. 3 is the various concentrations Na of the products therefrom of embodiments of the invention 13FeF6:The ultraviolet absorpting spectrum of Eu3+ fluorescent material
Stereoscan photograph；
Fig. 4 is the products therefrom Na of embodiments of the invention 13FeF6:The PLE of 5%Eu3+ fluorescent material；
Fig. 5 is the products therefrom various concentrations Na of embodiments of the invention 13FeF6:Eu3+ emission spectrum.
Embodiment
Explanation is further described to technical scheme below by specific embodiment.
If without specified otherwise, the raw material employed in embodiments of the invention is raw material commonly used in the art, is implemented
Method employed in example, it is the conventional method of this area.
Embodiment 1：
A kind of rear-earth-doped fluorination ferrisodium preparation method, step are as follows：
1) matrix Na3FeF6The preparation of solution
Prepare 0.05mol/L Fe (NO3)3Solution, 0.25mlo/L NaF solution, 0.25mol/L NH4HF2Solution is each
100ml.Measure 15ml NaF solution, 15ml Fe (NO respectively with pipette3)3Solution, 45ml NH4HF2Solution put with together
In one beaker, 3ml HF solution is eventually adding, stirs 10min.
2) activator is added
Prepare 0.1mol/L Eu (NO3)3Solution, by Eu3+:Fe3+Volume ratio be 3%, 5%, 7%, 10%, 15%,
18%th, 20%, 25% matches somebody with somebody 8 solution examples respectively, is well mixed.
3) hydro-thermal method synthesis Na3FeF6:Eu3+
Hydro-thermal method：Hydro-thermal method refers to solution being placed in the closed reactor of high pressure, Jie using water as reaction
The reaction under high pressure that matter is carried out.Using some materials under conditions of HTHP, it is changed into solvable special nature from insoluble, makes anti-
It should be able to be carried out under conditions of liquid phase.The advantages of hydro-thermal method is that the temperature of reaction is relatively low, and the particle for reacting the material of gained is equal
One property is relatively good, and reaction is more stable.Experimental method is as follows：
In the reactor transferred the solution into, loading is no more than 80%, is put into electric drying oven with forced convection, temperature setting
For 190 degrees Celsius, react 16 hours.
4) centrifuge
When solution is cooled to room temperature, solution is transferred in centrifuge tube, loading does not exceed 80%.Centrifuge tube is put
Enter in centrifuge and centrifuge 20 minutes, rotating speed 8000r/min.After centrifugation once terminates, supernatant is removed, is added in centrifuge tube
Deionized water carries out secondary centrifuging.Repeat the above steps after secondary centrifuging and centrifuged three times.
5) dry
After centrifugation terminates, by centrifuge tube, settled solution is gone at the middle and upper levels, and precipitation is put into electric drying oven with forced convection and dried,
Until the moisture in precipitation all evaporates.Precipitation after drying is crushed into powder and is fitted into test tube, carries out label.
Embodiment 2：
A kind of rear-earth-doped fluorination ferrisodium preparation method, step are as follows：
1) matrix Na3FeF6The preparation of solution
Prepare 0.1mol/L Fe (NO3)3Solution, 0.5mlo/L NaF solution, 0.5mol/L NH4HF2Solution is each
100ml.Measure 15ml NaF solution, 15ml Fe (NO respectively with pipette3)3Solution, 45ml NH4HF2Solution put with together
In one beaker, 3ml HF solution is eventually adding, stirs 10min.
2) activator is added
Prepare 0.1mol/L Eu (NO3)3Solution, by Eu3+:Fe3+Volume ratio be 3%, 5%, 7%, 10%, 15%,
18%th, 20%, 25% matches somebody with somebody 8 solution examples respectively, is well mixed.
3) hydro-thermal method synthesis Na3FeF6:Eu3+
Hydro-thermal method：Hydro-thermal method refers to solution being placed in the closed reactor of high pressure, Jie using water as reaction
The reaction under high pressure that matter is carried out.Using some materials under conditions of HTHP, it is changed into solvable special nature from insoluble, makes anti-
It should be able to be carried out under conditions of liquid phase.The advantages of hydro-thermal method is that the temperature of reaction is relatively low, and the particle for reacting the material of gained is equal
One property is relatively good, and reaction is more stable.Experimental method is as follows：
Transfer the solution into the reactor that capacity is 80ml, loading is no more than 80%, is put into electric drying oven with forced convection
In, temperature setting is 190 degrees Celsius, is reacted 16 hours.
4) centrifuge
When solution is cooled to room temperature, solution is transferred in centrifuge tube, loading does not exceed 80%.Centrifuge tube is put
Enter in centrifuge and centrifuge 20 minutes, rotating speed 8000r/min.After centrifugation once terminates, supernatant is removed, is added in centrifuge tube
Deionized water carries out secondary centrifuging.Repeat the above steps after secondary centrifuging and centrifuged three times.
5) dry
After centrifugation terminates, by centrifuge tube, settled solution is gone at the middle and upper levels, and precipitation is put into electric drying oven with forced convection and dried,
Until the moisture in precipitation all evaporates.Precipitation after drying is crushed into powder and is fitted into test tube, carries out label.
Embodiment 3：
A kind of rear-earth-doped fluorination ferrisodium preparation method, step are as follows：
1) matrix Na3FeF6The preparation of solution
Prepare 0.2mol/L Fe (NO3)3Solution, 1mlo/L NaF solution, 1mol/L NH4HF2Each 100ml of solution.
Measure 15ml NaF solution, 15ml Fe (NO respectively with pipette3)3Solution, 45ml NH4HF2Solution is put and same beaker
In, 3ml HF solution is eventually adding, stirs 10min.
2) activator is added
Prepare 0.1mol/L Eu (NO3)3Solution, by Eu3+:Fe3+Volume ratio be 3%, 5%, 7%, 10%, 15%,
18%th, 20%, 25% matches somebody with somebody 8 solution examples respectively, is well mixed.
3) hydro-thermal method synthesis Na3FeF6:Eu3+
Hydro-thermal method：Hydro-thermal method refers to solution being placed in the closed reactor of high pressure, Jie using water as reaction
The reaction under high pressure that matter is carried out.Using some materials under conditions of HTHP, it is changed into solvable special nature from insoluble, makes anti-
It should be able to be carried out under conditions of liquid phase.The advantages of hydro-thermal method is that the temperature of reaction is relatively low, and the particle for reacting the material of gained is equal
One property is relatively good, and reaction is more stable.Experimental method is as follows：
Transfer the solution into the reactor that capacity is 80ml, loading is no more than 80%, is put into electric drying oven with forced convection
In, temperature setting is 190 degrees Celsius, is reacted 16 hours.
4) centrifuge
When solution is cooled to room temperature, solution is transferred in centrifuge tube, loading does not exceed 80%.Centrifuge tube is put
Enter in centrifuge and centrifuge 20 minutes, rotating speed 8000r/min.After centrifugation once terminates, supernatant is removed, is added in centrifuge tube
Deionized water carries out secondary centrifuging.Repeat the above steps after secondary centrifuging and centrifuged three times.
5) dry
After centrifugation terminates, by centrifuge tube, settled solution is gone at the middle and upper levels, and precipitation is put into electric drying oven with forced convection and dried,
Until the moisture in precipitation all evaporates.Precipitation after drying is crushed into powder and is fitted into test tube, carries out label.
The material that it can be seen from performance characterizations of Fig. 1-Fig. 5 to product prepared by the application has good crystallinity,
Suitable for current various demands.
This method significantly improves the supply of rear-earth-doped fluorination ferrisodium, expands rear-earth-doped fluorination ferrisodium
Application, meet the needs of production.
Claims (5)
1. a kind of rear-earth-doped fluorination ferrisodium, it is characterised in that the rear-earth-doped fluorination ferrisodium is to be closed using hydro-thermal method
Into Eu3+Adulterate Na3FeF6。
A kind of 2. rear-earth-doped fluorination ferrisodium according to claim 1, it is characterised in that Eu3+Addition be
Na3FeF61-20%.
A kind of 3. rear-earth-doped fluorination ferrisodium according to claim 1 or 2, it is characterised in that Eu3+Addition be
Na3FeF61-8%.
A kind of 4. preparation method of rear-earth-doped fluorination ferrisodium as claimed in claim 1 or 2, it is characterised in that specific bag
Include following steps：
1) Fe (NO are prepared respectively3)3Solution, NaF solution NH4HF2Solution, then three kinds of solution are mixed, are eventually adding HF, stirred
Obtain Fe (NO3)3Solution；
2) Eu (NO are prepared3)3Solution, with Fe (NO3)3Solution is well mixed；
3) 1~5ml acetone will be added in mixed solution, reacts 8~24h in temperature is 185~210 DEG C of baking ovens；
4) solution is cooled to room temperature, Eu is obtained after eccentric cleaning3+Adulterate Na3FeF6。
A kind of 5. preparation method of rear-earth-doped fluorination ferrisodium as claimed in claim 4, it is characterised in that specifically include as
Lower step：
1) matrix Na3FeF6The preparation of solution：0.05~0.2mol/L Fe (NO are prepared respectively3)3Solution, 0.25~1mol/L's
NaF solution, 0.25~1mol/L NH4HF2Each 100ml of solution, measure 15ml NaF solution, 15ml Fe respectively with pipette
(NO3)3Solution, 45ml NH4HF2Solution is placed in same beaker, is eventually adding 3ml HF solution, is stirred 10min, is sunk
Product Na3FeF6Solution；
2) 0.1mol/L Eu (NO are prepared3)3Solution, by Eu3+:With Fe3+Volume ratio for 1%~20% with deposition Na3FeF6It is molten
Liquid is well mixed；
3) mixed solution is transferred in the reactor that capacity is 100ml, adds 1~5ml acetone, be 185~210 DEG C in temperature
8~24h is reacted in baking oven；
4) solution is cooled to room temperature, then solution is transferred in centrifuge tube；Centrifuge tube is put into centrifuge and centrifuges 20 points
Clock, rotating speed 8000r/min；After centrifugation once terminates, supernatant is removed, ethanol is added in centrifuge tube or acetone carries out two
Secondary centrifugation；Repeat the above steps after secondary centrifuging and centrifuged three times, obtain Na3FeF6:Eu3+Sample, i.e. Eu3+Doping
Na3FeF6。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104357057A (en) * | 2014-11-27 | 2015-02-18 | 长春工业大学 | Rare earth doped micro/nano-scale luminescent matrix material K2NaScF6 and preparation method thereof |
| JP2015111107A (en) * | 2013-10-28 | 2015-06-18 | 国立大学法人東北大学 | Scintillator and radiation detector |
| CN106853997A (en) * | 2016-12-14 | 2017-06-16 | 北京理工大学 | A kind of positive electrode and preparation method thereof and positive pole coating material and lithium ion battery |
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2017
- 2017-08-25 CN CN201710744663.8A patent/CN107674672B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015111107A (en) * | 2013-10-28 | 2015-06-18 | 国立大学法人東北大学 | Scintillator and radiation detector |
| CN104357057A (en) * | 2014-11-27 | 2015-02-18 | 长春工业大学 | Rare earth doped micro/nano-scale luminescent matrix material K2NaScF6 and preparation method thereof |
| CN106853997A (en) * | 2016-12-14 | 2017-06-16 | 北京理工大学 | A kind of positive electrode and preparation method thereof and positive pole coating material and lithium ion battery |
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| POOJA RAWAT ET AL.,: ""Wet-chemical synthesis, structural characterization and optical properties of rare-earth doped halo perovskite K3GaF6"", 《JOURNAL OF FLUORINE CHEMISTRY》 * |
| 北京师范大学 等: "《无机化学 下册》", 30 June 1982, 人民教育出版社 * |
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