CN106316386A - Preparation method of rare earth-doped bismuth system layered perovskite oxide ferroelectric up-conversion material - Google Patents
Preparation method of rare earth-doped bismuth system layered perovskite oxide ferroelectric up-conversion material Download PDFInfo
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Abstract
The invention discloses a preparation method of a rare earth-doped bismuth system layered perovskite oxide ferroelectric up-conversion material. The chemical formula of the rare earth-doped bismuth system layered perovskite oxide ferroelectric up-conversion material is Bi4-xRExTi3O12, wherein RE is one or more of Er, Tm and Yb, and x is not less than 0 and not more than 0.14. The Bi4-xRExTi3O12 nano-material is prepared through a co-precipitation reaction technology, and the method comprises proportioning, dissolving, mixing, precipitating, cleaning and calcining steps. The method has the advantages of convenience in operation, simple process, stable process, low cost, and easiness in large-scale industrial promotion. The Bi4-xRExTi3O12 nanomaterial synthesized in the invention has a good up-conversion luminescence performance, and ceramic produced by using the nanomaterial has excellent ferroelectric performances. The produced bismuth system layered perovskite oxide ferroelectric up-conversion material with excellent ferroelectric and up-conversion performances has wide application prospect in the technical fields of future photoelectric sensing and photoelectric integration.
Description
Technical field
The present invention relates to field of functional materials, be specifically related to a kind of rear-earth-doped bismuth system layered perovskite ferrum
Electricity up-conversion and preparation method thereof.
Background technology
Up-conversion luminescence, also referred to as anti-Stokes (Anti-stokes) are luminous, are to be swashed by low-energy photon
Sending out material makes it launch the process of high-energy photons.Rare earth upper conversion function material is at solid-state laser, three-dimensional
Stereo display, temperature sensing, photovoltaic cell, the aspect such as bio-imaging has broad prospect of application.Due to tool
Having relatively low phonon energy, fluoride and chloride is to change host material in research most widely at present.Lose
Regret, the physical and chemical performance stability of fluoride and chloride upper conversion function material is very poor and it is to ring
There is pollution in border, and these problems seriously limit the actual application of such upper conversion function material.In addition, it is necessary to
Pointing out, functional material has also been researched and proposed requirements at the higher level by the fast development of modern microelectronic industry.Single material
In material, several physical and intrinsic interactive realization thereof are the directions of future feature device material development.
But, the most widely studied up-conversion the most only has up-conversion luminescence simple function.Recently, hold concurrently
Tool ferroelectricity function is interior at the international level with the bismuth system layered perovskite ferroelectricity up-conversion of light emitting properties
Cause giving more sustained attention of researcher.Compared with the most traditional fluoride and chloride up-conversion,
Bismuth system layered perovskite ferroelectricity up-conversion has relatively low phonon energy, stable physics
Chemical characteristic, environmentally safe and can simultaneously the most to external world electricity respond with light stimulus.Therefore, bismuth system stratiform calcium
Titanium ore oxide ferroelectric up-conversion is one the most promising multifunctional light electrical part class material.
The preparation method of the bismuth system layered perovskite ferroelectricity up-conversion of research mainly has tradition at present
Solid reaction process and sol-gal process.For solid reaction process, in preparation process, chemical raw material is difficult to uniformly
Mixing, product needs high-temperature calcination that element evaporation can be caused to form various defect, and obtained sample crystallite dimension
Relatively big and particle diameter uneven, these all have a strong impact on material physical property.For sol-gal process, prepared
Journey is it is generally required to various metal alkoxide, relatively costly, is difficult to large-scale production.In contrast, coprecipitation
Cost is relatively low and can realize each element in preparation process in the contact of molecule rank and reaction, product calcining heat
Low, the high-purity that is easy to get and the nano material of size uniform.
Summary of the invention
It is an object of the invention to overcome the deficiency of prior art, it is provided that a kind of new rear-earth-doped bismuth system stratiform calcium
Titanium ore oxide ferroelectric up-conversion preparation method.
For achieving the above object and other purpose, the present invention is achieved by following technical solution:
The invention provides the preparation of a kind of rear-earth-doped bismuth system layered perovskite ferroelectricity up-conversion
Method, the chemical formula of this rear-earth-doped bismuth system layered perovskite ferroelectricity up-conversion is
Bi4-xRExTi3O12, wherein, RE is one or more in Er, Tm and Yb；Span 0≤the x of x
≤0.14。
Described rear-earth-doped bismuth system layered perovskite ferroelectricity up-conversion is for using co-precipitation legal system
Standby, described method comprises the steps:
Step 1: with the Bi (NO of analytical pure level3)3·5H2O, C16H36O4Ti, the Er (NO of high-purity grade3)3·5H2O,
Tm(NO3)3·6H2O, Yb (NO3)3·6H2O is raw material, according to chemical formula Bi4-xRExTi3O12, wherein, RE is
One or more in Er, Tm and Yb；Span 0≤x≤0.14 of x, is carried out in accordance with mol ratio
Proportioning；
Step 2: analytical pure concentrated nitric acid (65～68%) is dissolved in deionized water, concentrated nitric acid and deionized water
Volume ratio be 1: 5, prepare 60 milliliters of concentrated nitric acid-deionized water solutions；
Step 3: by appropriate Bi (NO3)3·5H2O adds in the concentrated nitric acid-deionized water solution of step 2 gained,
Stir 1 hour, obtain settled solution A；
Step 4: by appropriate Er (NO3)3·5H2O、Tm(NO3)3·6H2O、Yb(NO3)3·6H2O adds 15 millis
Rising in deionized water, stirring and dissolving obtains settled solution B；
Step 5: by the addition of C16H36O1Ti adds in 50 milliliters of analytical pure dehydrated alcohol, and stirring and dissolving must be clarified
Solution C；
Step 6: step 4 gained B solution is slowly added in step 3 gained solution A, uses deionized water
It is settled to 150 milliliters, and stirring and dissolving obtains settled solution D；
Step 7: step 5 gained C solution is slowly added in step 6 gained solution D, and add 8 millis
Rise concentrated nitric acid, continuously stirred 2 hours, obtain settled solution E；
Step 8: be slowly added dropwise by ammonia in step 7 gained E solution, stir, regulates PH～10,
Carry out coprecipitation reaction 2 hours, obtain Bi4-xRExTi3O12Precursor solution；
Step 9: by step 8 gained Bi4-xRExTi3O12Precursor solution utilizes deionized water to be centrifuged repeatedly washing,
Regulation PH～7, obtains product Bi4-xRExTi3O12；
Step 10: step 9 products therefrom is placed in electric drying oven with forced convection and dries 12 hours at 90 DEG C,
To Bi4-xRExTi3O12Precursor powder；
Step 11: step 10 gained precursor powder is placed in high temperature box furnace through 500～800 DEG C of heat treatments
Within 90 minutes, obtain Bi4-xRExTi3O12Nano material；
Step 12: by step 11 gained Bi1-xRExTi3O12Nano powder adds the PVA that concentration is 5% make
Grain, prepares the ceramic green blank of diameter 10mm under 8MPa pressure；
Step 13: by step 12 gained Bi4-xRExTi3O12Ceramic green blank is inserted in high temperature furnace, continuous warming,
It is incubated 60 minutes plastic removals, then continuous warmings at 700 DEG C, sinters 90 minutes at 1000 DEG C, obtain Bi4-xRExTi3O12
Ceramic material.
Compared with prior art, the method have the advantages that
(1) co-precipitation preparation method of the present invention has that technique is simple, process stabilizing, cost are relatively low, be prone to big
The advantages such as technical scale popularization.
(2) present invention just can synthesize different-grain diameter size by simple regulation and control preparation temperature, and size is equal
Even, that upper conversion performance is good fluorescent nano material.
(3) utilizing the nano material that the present invention obtains, under relatively lower temp, the ceramics sample of synthesis represents
Go out the ferroelectric properties of excellence.
(4) the bismuth system layered perovskite material that prepared by the present invention has the ferroelectricity of excellence and upper transformational
Can, in technical fields such as following photoelectric sensing and light are electrically integrated, there is broad prospect of application.
Accompanying drawing illustrates:
That Fig. 1 is given is the Bi of preparation under different temperatures4Ti3O12The X ray diffracting spectrum of nano material.
That Fig. 2 is given is the Bi of preparation under different temperatures4Ti3O12The electron scanning micrograph of nano material.
What Fig. 3 was given is to utilize Bi of the present invention4Ti3O12Ceramics sample room temperature ferroelectric hysteresis loop prepared by nano material.
That Fig. 4 is given is the Bi utilizing conventional solid reaction method to prepare4Ti3O12Ceramics sample room temperature ferroelectric hysteresis loop.
That Fig. 5 is given is Bi3.92Er0.08Ti3O12The electron scanning micrograph of nano material.
That Fig. 6 is given is the Bi of synthesis at 700 DEG C3.92Er0.08Ti3O12The Up-conversion emission spectrum of nano material.
That Fig. 7 is given is synthesis Bi at 700 DEG C3.86Er0.04Yb0.1Ti3O12The scanning electron microscope of nano material
Photo.
That Fig. 8 is given is synthesis Bi at 700 DEG C3.86Er0.04Yb0.1Ti3O12The Up-conversion emission spectrum of nano material.
That Fig. 9 is given is synthesis Bi at 700 DEG C3.89Tm0.01Yb0.1Ti3O12The scanning electron microscope of nano material
Photo.
That Figure 10 is given is synthesis Bi at 700 DEG C3.89Tm0.01Yb0.1Ti3O12The Up-conversion emission light of nano material
Spectrum.
Detailed description of the invention:
In conjunction with specific embodiment, the present invention is further described through:
Embodiment 1
Preparation Bi4Ti3O12Nano material, preparation method is as follows:
By 50 ml deionized water, 10 milliliters of analytical pure concentrated nitric acids (content 65～68%) add 250 milliliters
In beaker, it is placed on magnetic stirring apparatus and stirs, obtain 60 milliliters of concentrated nitric acid-deionized water solutions.By 3.9198
Gram Bi (NO3)3·5H2O adds in concentrated nitric acid-deionized water solution, stirs 1 hour, then utilizes deionization
Water is settled to 150 milliliters, obtains settled solution A.By 2.0625 grams of C16H36O4Ti adds 50 milliliters of analytical pure
In dehydrated alcohol, stirring and dissolving obtains settled solution B.B solution is slowly added in solution A, and adds 8
Milliliter concentrated nitric acid, continuously stirred 2 hours, obtains settled solution C.Ammonia is slowly added dropwise in C solution,
Stir, regulate PH～10, obtain Bi4Ti3O12Precursor solution D.Precursor solution D is carried out altogether
Precipitation 2 hours, is then centrifuged repeatedly washing through deionized water, is placed in electric drying oven with forced convection at 90 DEG C
Dry 12 hours, obtain Bi4Ti3O12Precursor powder.Precursor powder is placed in high temperature box furnace through 500～
800 DEG C of heat treatments obtain Bi in 90 minutes4Ti3O12Nano material.By Bi4Ti3O12Adding concentration in nano powder is
The PVA of 5% carries out pelletize, prepares the ceramic green blank of diameter 10mm, then at high temperature under 8MPa pressure
In stove, 1000 DEG C sinter 90 minutes, obtain Bi4Ti3O12Ceramic material.
Comparative example
Conventional solid reaction method prepares Bi1Ti3O12Ceramic material, preparation method is as follows:
Use the Bi of analytical pure level2O3And TiO (99%)2(99%) it is raw material, joins according to mol ratio
Compare, weigh various raw material.With analytical pure dehydrated alcohol as medium, the raw material prepared is placed in Achates tank,
Carrying out ball milling on planetary ball mill, Ball-milling Time is 24 hours.Slurry after ball milling is placed in beaker,
Dry in an oven, drying time 12 hours, dry temperature 95 degree, it is thus achieved that dry powder body.By ovendry power
Body agate mortar grinds, and is subsequently placed in corundum crucible, puts in batch-type furnace, and continuous warming to 850 DEG C is pre-
Burn 5 hours, program determination after being cooled to 500 degree, furnace cooling.Product utilization agate mortar is ground,
Add the PVA that concentration is 5% and carry out pelletize, under 10MPa pressure, prepare the ceramic green blank of diameter 13mm,
Then in high temperature furnace 1150 DEG C be calcined 2 hours, obtain Bi4Ti3O12Ceramic material.
That Fig. 1 is given is the Bi of preparation under different temperatures4Ti3O12The X ray diffracting spectrum of nano material.
That Fig. 2 is given is the Bi of preparation under different temperatures4Ti3O12The electron scanning micrograph of nano material.
What Fig. 3 was given is to utilize Bi of the present invention1Ti3O12Ceramics sample room temperature ferroelectric hysteresis loop prepared by nano material.
That Fig. 4 is given is the Bi utilizing conventional solid reaction method to prepare4Ti3O12Ceramics sample room temperature ferroelectric hysteresis loop.
Embodiment 2
Preparation Bi3.92Er0.08Ti3O12, preparation method is as follows:
By 50 ml deionized water, 10 milliliters of analytical pure concentrated nitric acids (content 65～68%) add 250 milliliters
In beaker, it is placed on magnetic stirring apparatus and stirs, obtain 60 milliliters of concentrated nitric acid-deionized water solutions.By 3.8414
Gram Bi (NO3)3·5H2O adds in concentrated nitric acid-deionized water solution, stirs 1 hour, obtains settled solution A.
By 0.0709 gram of Er (NO3)3·5H2O joins in 15 ml deionized water, and stirring and dissolving obtains settled solution B.Will
Solution B is slowly added in solution A, is settled to 150 milliliters with deionized water, continuously stirred settled solution C.
By 2.0625 grams of C16H36O4Ti adds in 50 milliliters of analytical pure dehydrated alcohol, and stirring and dissolving obtains settled solution D.By D
Solution is slowly added in C solution, and adds 8 milliliters of concentrated nitric acids, continuously stirred 2 hours, obtains settled solution E.
Ammonia is slowly added dropwise in E solution, stirs, regulate PH=10, obtain Bi3.92Er0.08Ti3O12Forerunner
Liquid solution F.Precursor solution F is carried out coprecipitation reaction 2 hours, is then centrifuged repeatedly washing through deionized water,
It is placed in electric drying oven with forced convection to dry 12 hours at 90 DEG C, obtains Bi3.92Er0.08Ti3O12Precursor powder.By forerunner
Powder body is placed in high temperature box furnace and within 90 minutes, obtains Bi through 500～800 DEG C of heat treatments3.92Er0.08Ti3O12Nanometer material
Material.
That Fig. 5 is given is Bi3.92Er0.08Ti3O12The electron scanning micrograph of nano material.
That Fig. 6 is given is the Bi of synthesis at 700 DEG C3.92Er0.08Ti3O12The Up-conversion emission spectrum of nano material.
Embodiment 3
Preparation Bi3.86Er0.01Yb0.1Ti3O12, preparation method is as follows:
By 50 ml deionized water, 10 milliliters of analytical pure concentrated nitric acids (content 65～68%) add 250 milliliters
In beaker, it is placed on magnetic stirring apparatus and stirs, obtain 60 milliliters of concentrated nitric acid-deionized water solutions.By 3.7826
Gram Bi (NO3)3·5H2O adds in concentrated nitric acid-deionized water solution, stirs 1 hour, obtains settled solution A.
By 0.0305 gram of Er (NO3)3·5H2O and 0.0934 gram of Yb (NO3)3·5H2O joins in 15 ml deionized water,
Stirring and dissolving obtains settled solution B.Solution B is slowly added in solution A, is settled to 150 millis with deionized water
Rise, continuously stirred settled solution C.By 2.0625 grams of C16H36O4Ti adds in 50 milliliters of analytical pure dehydrated alcohol,
Stirring and dissolving obtains settled solution D.Solution D is slowly added in C solution, and adds 8 milliliters of concentrated nitric acids, hold
Continuous stirring 2 hours, obtains settled solution E.Ammonia is slowly added dropwise in E solution, stirs, regulation
PH=10, obtains Bi3.86Er0.04Yb0.1Ti3O12Precursor solution F.Precursor solution F is carried out coprecipitation reaction 2
Hour, then it is centrifuged repeatedly washing through deionized water, is placed in electric drying oven with forced convection and dries 12 hours at 90 DEG C,
Obtain Bi3.86Er0.04Yb0.1Ti3O12Precursor powder.Precursor powder is placed in high temperature box furnace through 500～800 DEG C
Heat treatment obtains Bi in 90 minutes3.86Er0.04Yb0.1Ti3O12Nano material.
That Fig. 7 is given is synthesis Bi at 700 DEG C3.86Er0.04Yb0.1Ti3O12The scanning electron microscope of nano material
Photo.
That Fig. 8 is given is synthesis Bi at 700 DEG C3.86Er0.04Yb0.1Ti3O12The Up-conversion emission spectrum of nano material.
Embodiment 4
Preparation Bi3.89Tm0.01Yb0.1Ti3O12, preparation method is as follows:
By 50 ml deionized water, 10 milliliters of analytical pure concentrated nitric acids (content 65～68%) add 250 milliliters
In beaker, it is placed on magnetic stirring apparatus and stirs, obtain 60 milliliters of concentrated nitric acid-deionized water solutions.By 3.8120
Gram Bi (NO3)3·5H2O adds in concentrated nitric acid-deionized water solution, stirs 1 hour, obtains settled solution A.
By 0.0093 gram of Tm (NO3)3·5H2O and 0.0934 gram of Yb (NO3)3·5H2O joins in 15 ml deionized water,
Stirring and dissolving obtains settled solution B.Solution B is slowly added in solution A, is settled to 150 millis with deionized water
Rise, continuously stirred settled solution C.By 2.0625 grams of C16H36O4Ti adds in 50 milliliters of analytical pure dehydrated alcohol,
Stirring and dissolving obtains settled solution D.Solution D is slowly added in C solution, and adds 8 milliliters of concentrated nitric acids, hold
Continuous stirring 2 hours, obtains settled solution E.Ammonia is slowly added dropwise in E solution, stirs, regulation
PH=10, obtains Bi3.89Tm0.01Yb0.1Ti3O12Precursor solution F.Precursor solution F is carried out coprecipitation reaction 2
Hour, then it is centrifuged repeatedly washing through deionized water, is placed in electric drying oven with forced convection and dries 12 hours at 90 DEG C,
Obtain Bi3.89Tm0.01Yb0.1Ti3O12Precursor powder.Precursor powder is placed in high temperature box furnace through 500～800 DEG C
Heat treatment obtains Bi in 90 minutes3.89Tm0.01Yb0.1Ti3O12Nano material.
That Fig. 9 is given is synthesis Bi at 700 DEG C3.89Tm0.01Yb0.1Ti3O12The scanning electron microscope of nano material
Photo.
That Figure 10 is given is synthesis Bi at 700 DEG C3.89Tm0.01Yb0.1Ti3O12The Up-conversion emission light of nano material
Spectrum.
Claims (2)
1. a preparation method for rear-earth-doped bismuth system layered perovskite ferroelectricity up-conversion, this is dilute
The chemical formula of native doping bismuth system layered perovskite ferroelectricity up-conversion is Bi4-xRExTi3O12, wherein,
RE is one or more in Er, Tm and Yb；Span 0≤x≤0.14 of x.
The system of rear-earth-doped bismuth system the most as claimed in claim 1 layered perovskite ferroelectricity up-conversion
Preparation Method, it is characterised in that described ferroelectricity up-conversion is for using coprecipitation reaction method to prepare, described
Method comprise the steps:
(1) dispensing: with the Bi (NO of analytical pure level3)3·5H2O, C16H36O4Ti, high-purity grade
Er(NO3)3·5H2O, Tm (NO3)3·6H2O, Yb (NO3)3·6H2O is raw material, according to chemical formula Bi4-xRExTi3O12,
Wherein, one or more during RE is Er, Tm and Yb；Span 0≤x≤0.14 of x, abides by
Proportioning is carried out according to mol ratio；
(2) dissolve: analytical pure concentrated nitric acid (65～68%) is dissolved in deionized water, concentrated nitric acid and go from
The volume ratio of sub-water is 1: 5, prepares 60 milliliters of concentrated nitric acid-deionized water solutions；
(3) dissolve: by appropriate Bi (NO3)3·5H2O adds the concentrated nitric acid-deionized water solution of step 2 gained
In, stir 1 hour, obtain settled solution A；
(4) dissolve: by appropriate Er (NO3)3·5H2O、Tm(NO3)3·6H2O、Yb(NO3)3·6H2O adds
In 15 ml deionized water, stirring and dissolving obtains settled solution B；
(5) dissolve: by the addition of C16H36O4Ti adds in 50 milliliters of analytical pure dehydrated alcohol, and stirring and dissolving obtains
Settled solution C；
(6) mixing: step 4 gained B solution is slowly added in step 3 gained solution A, spend from
Sub-water is settled to 150 milliliters, and stirring and dissolving obtains settled solution D；
(7) mixing: step 5 gained C solution is slowly added in step 6 gained solution D, and adds
8 milliliters of concentrated nitric acids, continuously stirred 2 hours, obtain settled solution E；
(8) precipitation: be slowly added dropwise by ammonia in step 7 gained E solution, stir, regulates PH
～10, carry out coprecipitation reaction 2 hours, obtain Bi4-xRExTi3O12Precursor solution；
(9) clean: by step 8 gained Bi4-xRExTi3O12Precursor solution utilizes deionized water to be centrifuged repeatedly
Washing, regulates PH～7, obtains product Bi4-xRExTi3O12；
(10) dry: step 9 products therefrom is placed in electric drying oven with forced convection and dries 12 hours at 90 DEG C,
Obtain Bi4-xRExTi3O12Precursor powder；
(11) calcining: step 10 gained precursor powder is placed in high temperature box furnace through 500～800 DEG C of heat
Process and obtain Bi in 90 minutes4-xRExTi3O12Nano material；
(12) base: by step 11 gained Bi4-xRExTi3O12Nano powder adds the PVA that concentration is 5% enter
Row pelletize, prepares the ceramic green blank of diameter 10mm under 8MPa pressure；
(13) sintering: by step 12 gained Bi4-xRExTi3O12Ceramic green blank is inserted in high temperature furnace, continuously
Heat up, be incubated 60 minutes plastic removals, then continuous warmings at 700 DEG C, sinter 90 minutes at 1000 DEG C,
Bi4-xRExTi3O12Ceramic material.
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| CN106809875A (en) * | 2017-03-07 | 2017-06-09 | 南京工业大学 | Preparation method of perovskite-based multi-wavelength infrared photoelectric response nano material |
| CN106978175A (en) * | 2017-03-30 | 2017-07-25 | 同济大学 | Bismuth laminated multifunctional material of the rare earth doped element of one class and preparation method thereof |
| CN111410531A (en) * | 2020-04-25 | 2020-07-14 | 中国民航大学 | Up-conversion luminescence reversible regulation material based on photochromic effect and preparation method thereof |
| CN112745841A (en) * | 2020-12-25 | 2021-05-04 | 广西大学 | Alkali metal reinforced bismuth titanate-based up-conversion fluorescent material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106809875A (en) * | 2017-03-07 | 2017-06-09 | 南京工业大学 | Preparation method of perovskite-based multi-wavelength infrared photoelectric response nano material |
| CN106978175A (en) * | 2017-03-30 | 2017-07-25 | 同济大学 | Bismuth laminated multifunctional material of the rare earth doped element of one class and preparation method thereof |
| CN106978175B (en) * | 2017-03-30 | 2020-10-30 | 同济大学 | Rare earth element doped bismuth layer structure multifunctional material and preparation method thereof |
| CN111410531A (en) * | 2020-04-25 | 2020-07-14 | 中国民航大学 | Up-conversion luminescence reversible regulation material based on photochromic effect and preparation method thereof |
| CN112745841A (en) * | 2020-12-25 | 2021-05-04 | 广西大学 | Alkali metal reinforced bismuth titanate-based up-conversion fluorescent material and preparation method thereof |
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Application publication date: 20170111 |