CN104746176A - Method for preparing CaTiO3:Eu<3+>/TiO2 composite fibers - Google Patents

Method for preparing CaTiO3:Eu<3+>/TiO2 composite fibers Download PDF

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CN104746176A
CN104746176A CN201510187945.3A CN201510187945A CN104746176A CN 104746176 A CN104746176 A CN 104746176A CN 201510187945 A CN201510187945 A CN 201510187945A CN 104746176 A CN104746176 A CN 104746176A
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composite fibre
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nanocrystalline
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CN104746176B (en
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王国凤
孟玲
魏廷库
潘清江
潘凯
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Heilongjiang University
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Heilongjiang University
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Abstract

The invention discloses a method for preparing CaTiO3:Eu<3+>/TiO2 composite fibers and relates to a method for synthesizing the CaTiO3:Eu<3+>/TiO2 composite fibers, which is used for solving the problem of the conventional CaTiO3:Eu<3+> nanocrystalline surface fluorescence quenching. The method for preparing the composite fibers comprises the following steps: 1. uniformly mixing CaTiO3:Eu<3+> nanocrystalline, PVP, tetrabutyl titanate and absolute ethyl alcohol, thereby obtaining a spinning solution; 2. performing electrostatic spinning on the spinning solution in an electrostatic spinning solution, thereby obtaining a precursor material; and 3. roasting the precursor material, thereby obtaining the CaTiO3:Eu<3+>/TiO2 composite fibers. The CaTiO3:Eu<3+>/TiO2 composite fibers prepared by the invention are of a one-dimensional structure, the CaTiO3:Eu<3+> surface is coated by virtue of TiO2, and the CaTiO3:Eu<3+> nanocrystalline surface fluorescence quenching is avoided.

Description

CaTiO 3: Eu 3+/ TiO 2the preparation method of composite fibre
Technical field
The present invention relates to a kind of CaTiO 3: Eu 3+/ TiO 2the synthetic method of composite fibre.
Background technology
Composite, to the development of modern science and technology, has very important effect.The depth of investigation and speed and the scale of applying range and production development thereof of composite, become one of important symbol of a measurement national science advanced technology level.Composite is a kind of mixture.All play very large effect in a lot of field, instead of much traditional material.Composite is divided into metal and metallic composite, nonmetal with metallic composite, nonmetal and nonmetallic composite by its composition.Composite is due to its excellent combination property, particularly the designability of its performance is widely used in the fields such as Aero-Space, national defence, traffic, physical culture, nano composite material is then the part of wherein most attraction, development is very fast, and the strategy of World Developed Countries new material development is all put into important position the development of nano composite material.The composite of pluralistic function body can have several functions.Meanwhile, also likely new function is produced due to complex effect.Multifunctional composite is the developing direction of functional composite material.At present, the method preparing composite has a lot.Wherein method of electrostatic spinning is subject to extensive concern because it is simple to operate, the scope of application is wide, cost is low and do not change solution self-characteristic.
Rare earth is the indispensable component of the various functions materials such as luminescence, magnetics, superconduction, and rare earth optical function material is widely used in the fields such as terminal demonstration, opto-electronic device, laser technology and biology.After ZnS:Mn nano-crystalline granule has the quantum luminous efficiency higher than body material since people's reported first such as R.N.Bhargava in 1994, micro-nano luminous material receives the extensive concern of Chinese scholars.Rare earth micro-nano luminous material can show many unusual characteristics, as small-size effect, high-ratio surface effect, quantum effect, extremely strong optical, electrical, magnetic property, superconductivity, high chemism etc., greatly can improve performance and the function of material.The design and functions research of novel rare-earth composite is the focus that scholars pay close attention to always.
Summary of the invention
The object of the invention is to solve existing CaTiO 3: Eu 3+the problem of nanocrystal surface fluorescent quenching, and CaTiO is provided 3: Eu 3+/ TiO 2the preparation method of composite fibre.
CaTiO of the present invention 3: Eu 3+/ TiO 2the preparation method of composite fibre realizes according to the following steps:
One, by CaTiO 3: Eu 3+nanocrystalline, PVP (polyvinylpyrrolidone), butyl titanate and absolute ethyl alcohol mix, and obtain spinning solution;
Two, the spinning solution that step one obtains is placed in electrostatic spinning apparatus and carries out electrostatic spinning, obtain CaTiO 3: Eu 3+/ TiO 2composite fibre persursor material;
Three, CaTiO step 2 obtained 3: Eu 3+/ TiO 2composite fibre persursor material puts into Muffle furnace, carries out calcination process, obtain CaTiO at the temperature of 400 ~ 500 DEG C 3: Eu 3+/ TiO 2composite fibre.
The CaTiO that the present invention prepares 3: Eu 3+/ TiO 2composite fibre is one-dimentional structure, passes through TiO 2to CaTiO 3: Eu 3+surface is carried out coated, decreases CaTiO 3: Eu 3+nanocrystalline surface state, avoids CaTiO 3: Eu 3+nanocrystal surface fluorescent quenching, has special luminescent properties.
Accompanying drawing explanation
Fig. 1 is the CaTiO that embodiment one prepares 3: Eu 3+/ TiO 2the electron scanning micrograph of composite fibre;
Fig. 2 is the CaTiO that embodiment one prepares 3: Eu 3+/ TiO 2the XRD collection of illustrative plates of composite fibre;
Fig. 3 is the CaTiO that embodiment one prepares 3: Eu 3+/ TiO 2the fluorescence spectrum of composite fibre.
Detailed description of the invention
Detailed description of the invention one: present embodiment CaTiO 3: Eu 3+/ TiO 2the preparation method of composite fibre follows these steps to implement:
One, by CaTiO 3: Eu 3+nanocrystalline, PVP (polyvinylpyrrolidone), butyl titanate and absolute ethyl alcohol mix, and obtain spinning solution;
Two, the spinning solution that step one obtains is placed in electrostatic spinning apparatus and carries out electrostatic spinning, obtain CaTiO 3: Eu 3+/ TiO 2composite fibre persursor material;
Three, CaTiO step 2 obtained 3: Eu 3+/ TiO 2composite fibre persursor material puts into Muffle furnace, carries out calcination process, obtain CaTiO at the temperature of 400 ~ 500 DEG C 3: Eu 3+/ TiO 2composite fibre.
Present embodiment CaTiO 3: Eu 3+/ TiO 2technique prepared by composite fibre is simple, cost is low, equipment needed thereby is simple, is easy to realize suitability for industrialized production.
Detailed description of the invention two: present embodiment and detailed description of the invention one are unlike the CaTiO described in step one 3: Eu 3+nanocrystalline preparation method is as follows: join in ethylene glycol solution by calcium acetate, europium nitrate and butyl titanate, and reaction terminates rear collection solid formation, dries solid formation, then at the temperature lower calcination of 600 DEG C, obtains CaTiO 3: Eu 3+nanocrystalline.Other step and parameter identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention two are unlike the CaTiO described in step one 3: Eu 3+nanocrystalline preparation method is as follows: join in 60mL ethylene glycol solution by 0.009mol calcium acetate, 0.001mol europium nitrate and 3.4mL butyl titanate, reaction terminates rear collection solid formation, dry solid formation at 130 DEG C, then at the temperature lower calcination of 600 DEG C, obtain CaTiO 3: Eu 3+nanocrystalline.Other step and parameter identical with detailed description of the invention two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three are 0.05 ~ 2mol/L unlike the concentration of PVP in step one spinning solution.Other step and parameter identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four unlike step one by 0.5 gram of CaTiO 3: Eu 3+nanocrystalline, 2 grams of PVP (polyvinylpyrrolidone), 4 grams of butyl titanates and 10 milliliters of absolute ethyl alcohols mix, and obtain spinning solution.Other step and parameter identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five are placed in electrostatic spinning apparatus unlike the spinning solution that step one obtains by step 2, adjustment spinning voltage is 12kV, relative humidity is 35%, indoor temperature is 15 DEG C, receiving range is 20cm, carries out electrostatic spinning.Other step and parameter identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: the CaTiO that step 2 obtains unlike step 3 by one of present embodiment and detailed description of the invention one to six 3: Eu 3+/ TiO 2composite fibre persursor material puts into Muffle furnace, is warming up to 400 ~ 500 DEG C with the speed of 1 DEG C/min.Other step and parameter identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven carry out calcination process 2h unlike step 3 at the temperature of 450 DEG C.Other step and parameter identical with one of detailed description of the invention one to seven.
Embodiment one: the present embodiment CaTiO 3: Eu 3+/ TiO 2the preparation method of composite fibre follows these steps to implement:
One, be 40 DEG C in temperature, mixing speed is by 0.5 gram of CaTiO under 150 revs/min of conditions 3: Eu 3+nanocrystalline, 2 grams of PVP (polyvinylpyrrolidone), 4 grams of butyl titanates and 10 milliliters of absolute ethyl alcohols mix, and obtain spinning solution;
Two, the spinning solution that step one obtains is placed in electrostatic spinning apparatus, regulate spinning voltage to be 12kV, relative humidity is 35%, and indoor temperature is 15 DEG C, and receiving range is that 20cm carries out electrostatic spinning, obtains CaTiO 3: Eu 3+/ TiO 2composite fibre persursor material;
Three, CaTiO step 2 obtained 3: Eu 3+/ TiO 2composite fibre persursor material puts into Muffle furnace, is warming up to 450 DEG C with the speed of 1 DEG C/min, the roasting temperature process 2 hours of 450 DEG C, obtains CaTiO 3: Eu 3+/ TiO 2composite fibre.
Gained CaTiO in the present embodiment 3: Eu 3+/ TiO 2the electron scanning micrograph of composite fibre as shown in Figure 1; Gained CaTiO in the present embodiment 3: Eu 3+/ TiO 2the XRD collection of illustrative plates of composite fibre as shown in Figure 2; Gained CaTiO in the present embodiment 3: Eu 3+/ TiO 2the fluorescence spectrum of composite fibre as shown in Figure 3.The CaTiO that the present embodiment obtains 3: Eu 3+/ TiO 2composite fibre avoids nanocrystal surface fluorescent quenching, and fluorometric investigation result shows CaTiO 3: Eu 3+/ TiO 2composite fibre is good luminescent material.

Claims (8)

1.CaTiO 3: Eu 3+/ TiO 2the preparation method of composite fibre, it is characterized in that realizing according to the following steps:
One, by CaTiO 3: Eu 3+nanocrystalline, PVP, butyl titanate and absolute ethyl alcohol mix, and obtain spinning solution;
Two, the spinning solution that step one obtains is placed in electrostatic spinning apparatus and carries out electrostatic spinning, obtain CaTiO 3: Eu 3+/ TiO 2composite fibre persursor material;
Three, CaTiO step 2 obtained 3: Eu 3+/ TiO 2composite fibre persursor material puts into Muffle furnace, carries out calcination process, obtain CaTiO at the temperature of 400 ~ 500 DEG C 3: Eu 3+/ TiO 2composite fibre.
2. CaTiO according to claim 1 3: Eu 3+/ TiO 2the preparation method of composite fibre, is characterized in that the CaTiO described in step one 3: Eu 3+nanocrystalline preparation method is as follows: join in ethylene glycol solution by calcium acetate, europium nitrate and butyl titanate, and reaction terminates rear collection solid formation, dries solid formation, then at the temperature lower calcination of 600 DEG C, obtains CaTiO 3: Eu 3+nanocrystalline.
3. CaTiO according to claim 2 3: Eu 3+/ TiO 2the preparation method of composite fibre, is characterized in that the CaTiO described in step one 3: Eu 3+nanocrystalline preparation method is as follows: join in 60mL ethylene glycol solution by 0.009mol calcium acetate, 0.001mol europium nitrate and 3.4mL butyl titanate, reaction terminates rear collection solid formation, dry solid formation at 130 DEG C, then at the temperature lower calcination of 600 DEG C, obtain CaTiO 3: Eu 3+nanocrystalline.
4. CaTiO according to claim 1 3: Eu 3+/ TiO 2the preparation method of composite fibre, is characterized in that the concentration of PVP in step one spinning solution is 0.05 ~ 2mol/L.
5. CaTiO according to claim 1 3: Eu 3+/ TiO 2the preparation method of composite fibre, is characterized in that step one is by 0.5 gram of CaTiO 3: Eu 3+nanocrystalline, 2 grams of PVP, 4 grams of butyl titanates and 10 milliliters of absolute ethyl alcohols mix, and obtain spinning solution.
6. CaTiO according to claim 1 3: Eu 3+/ TiO 2the preparation method of composite fibre, is characterized in that the spinning solution that step one obtains by step 2 is placed in electrostatic spinning apparatus, and adjustment spinning voltage is 12kV, and relative humidity is 35%, and indoor temperature is 15 DEG C, and receiving range is 20cm, carries out electrostatic spinning.
7. CaTiO according to claim 1 3: Eu 3+/ TiO 2the preparation method of composite fibre, is characterized in that the CaTiO that step 2 obtains by step 3 3: Eu 3+/ TiO 2composite fibre persursor material puts into Muffle furnace, is warming up to 400 ~ 500 DEG C with the speed of 1 DEG C/min.
8. CaTiO according to claim 1 3: Eu 3+/ TiO 2the preparation method of composite fibre, is characterized in that step 3 carries out calcination process 2h at the temperature of 450 DEG C.
CN201510187945.3A 2015-04-20 2015-04-20 CaTiO3: Eu3+/ TiO2the preparation method of composite fibre Expired - Fee Related CN104746176B (en)

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