CN104746176B - CaTiO3: Eu3+/ TiO2the preparation method of composite fibre - Google Patents
CaTiO3: Eu3+/ TiO2the preparation method of composite fibre Download PDFInfo
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Abstract
CaTiO3:Eu3+/TiO2The preparation method of composite fibre, the present invention relates to a kind of CaTiO3:Eu3+/TiO2The synthetic method of composite fibre, it is in order to solve existing CaTiO3:Eu3+The problem of nanocrystal surface fluorescent quenching.The preparation method of composite fibre: one, by CaTiO3:Eu3+Nanocrystalline, PVP, butyl titanate and dehydrated alcohol mix homogeneously, obtain spinning liquid；Two, carry out electrostatic spinning during spinning liquid is placed in electrostatic spinning apparatus, obtain persursor material；Three, persursor material is carried out calcination process, obtain CaTiO3:Eu3+/TiO2Composite fibre.The CaTiO that the present invention prepares3:Eu3+/TiO2Composite fibre is one-dimentional structure, passes through TiO2To CaTiO3:Eu3+Surface is coated with, it is to avoid CaTiO3:Eu3+Nanocrystal surface fluorescent quenching.
Description
Technical field
The present invention relates to a kind of CaTiO3:Eu3+/TiO2The synthetic method of composite fibre.
Background technology
The composite development to modern science and technology, has highly important effect.The depth of investigation of composite and application range and the speed of production development and scale, it has also become weigh one of important symbol of a national science advanced technology level.Composite is a kind of mixture.All play the biggest effect in a lot of fields, instead of the most traditional material.Composite is divided into metal and metallic composite, nonmetal and metallic composite, nonmetal and nonmetallic composite by its composition.Composite is due to its excellent combination property, the particularly 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 the most most captivation, quickly, the strategy of World Developed Countries new material development is all put into important position the development of nano composite material in development.The composite of pluralistic function body can have several functions.At the same time it also is possible to produce new function 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 owing to it is simple to operate, range is wide, low cost and do not change solution self-characteristic and receive significant attention.
Rare earth is the component that the various functions materials such as luminescence, magnetics, superconduction are indispensable, 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 higher than the quantum luminous efficiency of body material since R.N.Bhargava in 1994 et al. reported first, micro-nano luminous material receives the extensive concern of Chinese scholars.Rare earth micro-nano luminous material can show many unusual characteristics, such as small-size effect, high-ratio surface effect, quantum effect, extremely strong optical, electrical, magnetic property, superconductivity, high chemism etc., can be greatly improved performance and the function of material.The design of novel rare-earth composite and performance study are always scholars institute focus of attention.
Summary of the invention
The invention aims to solve existing CaTiO3:Eu3+The problem of nanocrystal surface fluorescent quenching, and CaTiO is provided3:Eu3+/TiO2The preparation method of composite fibre.
CaTiO of the present invention3:Eu3+/TiO2The preparation method of composite fibre realizes according to the following steps:
One, by CaTiO3:Eu3+Nanocrystalline, PVP (polyvinylpyrrolidone), butyl titanate and dehydrated alcohol mix homogeneously, obtain spinning liquid；
Two, the spinning liquid that step one obtains is placed in electrostatic spinning apparatus carries out electrostatic spinning, obtain CaTiO3:Eu3+/TiO2Composite fibre persursor material；
Three, the CaTiO that step 2 is obtained3:Eu3+/TiO2Composite fibre persursor material is put in Muffle furnace, carries out calcination process, obtain CaTiO at a temperature of 400～500 DEG C3:Eu3+/TiO2Composite fibre.
The CaTiO that the present invention prepares3:Eu3+/TiO2Composite fibre is one-dimentional structure, passes through TiO2To CaTiO3:Eu3+Surface is coated with, and decreases CaTiO3:Eu3+Nanocrystalline surface state, it is to avoid CaTiO3:Eu3+Nanocrystal surface fluorescent quenching, has special luminescent properties.
Accompanying drawing explanation
Fig. 1 is the CaTiO that embodiment one prepares3:Eu3+/TiO2The electron scanning micrograph of composite fibre；
Fig. 2 is the CaTiO that embodiment one prepares3:Eu3+/TiO2The XRD figure spectrum of composite fibre；
Fig. 3 is the CaTiO that embodiment one prepares3:Eu3+/TiO2The fluorescence spectrum of composite fibre.
Detailed description of the invention
Detailed description of the invention one: present embodiment CaTiO3:Eu3+/TiO2The preparation method of composite fibre follows these steps to implement:
One, by CaTiO3:Eu3+Nanocrystalline, PVP (polyvinylpyrrolidone), butyl titanate and dehydrated alcohol mix homogeneously, obtain spinning liquid；
Two, the spinning liquid that step one obtains is placed in electrostatic spinning apparatus carries out electrostatic spinning, obtain CaTiO3:Eu3+/TiO2Composite fibre persursor material；
Three, the CaTiO that step 2 is obtained3:Eu3+/TiO2Composite fibre persursor material is put in Muffle furnace, carries out calcination process, obtain CaTiO at a temperature of 400～500 DEG C3:Eu3+/TiO2Composite fibre.
Present embodiment CaTiO3:Eu3+/TiO2Technique prepared by composite fibre is simple, low cost, equipment needed thereby are simple, it is easy to accomplish industrialized production.
Detailed description of the invention two: present embodiment CaTiO described in step one unlike detailed description of the invention one3:Eu3+Nanocrystalline preparation method is as follows: join in ethylene glycol solution by calcium acetate, europium nitrate and butyl titanate, and reaction collects solid formation after terminating, and dries solid formation, then calcines at a temperature of 600 DEG C, obtain CaTiO3:Eu3+Nanocrystalline.Other step and parameter are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment CaTiO described in step one unlike detailed description of the invention two3:Eu3+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 collects solid formation after terminating, dry solid formation at 130 DEG C, then calcine at a temperature of 600 DEG C, obtain CaTiO3:Eu3+Nanocrystalline.Other step and parameter are identical with detailed description of the invention two.
Detailed description of the invention four: in present embodiment step one spinning liquid unlike one of detailed description of the invention one to three, the concentration of PVP is 0.05～2mol/L.Other step and parameter are identical with one of detailed description of the invention one to three.
Detailed description of the invention five: present embodiment unlike one of detailed description of the invention one to four step one by 0.5 gram of CaTiO3:Eu3+Nanocrystalline, 2 grams of PVP (polyvinylpyrrolidone), 4 grams of butyl titanates and 10 milliliters of dehydrated alcohol mix homogeneously, obtain spinning liquid.Other step and parameter are identical with one of detailed description of the invention one to four.
Detailed description of the invention six: the spinning liquid that step one is obtained by present embodiment step 2 unlike one of detailed description of the invention one to five is placed in electrostatic spinning apparatus, regulation spinning voltage is 12kV, and relative humidity is 35%, and indoor temperature is 15 DEG C, receiving range is 20cm, carries out electrostatic spinning.Other step and parameter are identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: the CaTiO that step 2 is obtained by present embodiment step 3 unlike one of detailed description of the invention one to six3:Eu3+/TiO2Composite fibre persursor material is put in Muffle furnace, is warming up to 400～500 DEG C with the speed of 1 DEG C/min.Other step and parameter are identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: present embodiment step 3 unlike one of detailed description of the invention one to seven carries out calcination process 2h at a temperature of 450 DEG C.Other step and parameter are identical with one of detailed description of the invention one to seven.
Embodiment one: the present embodiment CaTiO3:Eu3+/TiO2The preparation method of composite fibre follows these steps to implement:
One, be 40 DEG C in temperature, mixing speed be 150 revs/min under the conditions of by 0.5 gram of CaTiO3:Eu3+Nanocrystalline, 2 grams of PVP (polyvinylpyrrolidone), 4 grams of butyl titanates and 10 milliliters of dehydrated alcohol mix homogeneously, obtain spinning liquid；
Two, being placed in electrostatic spinning apparatus by the spinning liquid that step one obtains, regulation spinning voltage is 12kV, and relative humidity is 35%, and indoor temperature is 15 DEG C, and receiving range is that 20cm carries out electrostatic spinning, obtains CaTiO3:Eu3+/TiO2Composite fibre persursor material；
Three, the CaTiO that step 2 is obtained3:Eu3+/TiO2Composite fibre persursor material is put in Muffle furnace, is warming up to 450 DEG C with the speed of 1 DEG C/min, and at a temperature of 450 DEG C, calcination process 2 hours, obtain CaTiO3:Eu3+/TiO2Composite fibre.
Gained CaTiO in the present embodiment3:Eu3+/TiO2The electron scanning micrograph of composite fibre is as shown in Figure 1；Gained CaTiO in the present embodiment3:Eu3+/TiO2The XRD figure of composite fibre is composed as shown in Figure 2；Gained CaTiO in the present embodiment3:Eu3+/TiO2The fluorescence spectrum of composite fibre is as shown in Figure 3.The CaTiO that the present embodiment obtains3:Eu3+/TiO2Composite fibre avoids nanocrystal surface fluorescent quenching, and fluorometric investigation result shows CaTiO3:Eu3+/TiO2Composite fibre is good luminescent material.
Claims (7)
1.CaTiO3:Eu3+/TiO2The preparation method of composite fibre, it is characterised in that be to realize according to the following steps:
One, by CaTiO3:Eu3+Nanocrystalline, PVP, butyl titanate and dehydrated alcohol mix homogeneously, obtain spinning liquid；
Two, the spinning liquid that step one obtains is placed in electrostatic spinning apparatus carries out electrostatic spinning, obtain CaTiO3:Eu3+/TiO2
Composite fibre persursor material；
Three, the CaTiO that step 2 is obtained3:Eu3+/TiO2Composite fibre persursor material is put in Muffle furnace, 400～
Carry out calcination process at a temperature of 500 DEG C, obtain CaTiO3:Eu3+/TiO2Composite fibre；
Wherein step 2 regulation 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.
CaTiO the most according to claim 13:Eu3+/TiO2The preparation method of composite fibre, it is characterised in that step one
Described CaTiO3:Eu3+Nanocrystalline preparation method is as follows: calcium acetate, europium nitrate and butyl titanate are joined ethylene glycol
In solution, reaction collects solid formation after terminating, and dries solid formation, then calcines at a temperature of 600 DEG C, obtain CaTiO3:Eu3+
Nanocrystalline.
CaTiO the most according to claim 23:Eu3+/TiO2The preparation method of composite fibre, it is characterised in that step one
Described CaTiO3:Eu3+Nanocrystalline preparation method is as follows: by 0.009mol calcium acetate, 0.001mol europium nitrate and 3.4mL
Butyl titanate joins in 60mL ethylene glycol solution, and reaction collects solid formation after terminating, and dries solid formation, so at 130 DEG C
After at a temperature of 600 DEG C calcine, obtain CaTiO3:Eu3+Nanocrystalline.
CaTiO the most according to claim 13:Eu3+/TiO2The preparation method of composite fibre, it is characterised in that step one
In spinning liquid, the concentration of PVP is 0.05～2mol/L.
CaTiO the most according to claim 13:Eu3+/TiO2The preparation method of composite fibre, it is characterised in that step one
By 0.5 gram of CaTiO3:Eu3+Nanocrystalline, 2 grams of PVP, 4 grams of butyl titanates and 10 milliliters of dehydrated alcohol mix homogeneously,
To spinning liquid.
CaTiO the most according to claim 13:Eu3+/TiO2The preparation method of composite fibre, it is characterised in that step 3
The CaTiO that step 2 is obtained3:Eu3+/TiO2Composite fibre persursor material is put in Muffle furnace, with the speed liter of 1 DEG C/min
Temperature is to 400～500 DEG C.
CaTiO the most according to claim 13:Eu3+/TiO2The preparation method of composite fibre, it is characterised in that step 3
Calcination process 2h is carried out at a temperature of 450 DEG C.
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