CN105271380A - Preparation method of gadolinium-doped bismuth titanate with nano-sheet cluster structure - Google Patents
Preparation method of gadolinium-doped bismuth titanate with nano-sheet cluster structure Download PDFInfo
- Publication number
- CN105271380A CN105271380A CN201510726065.9A CN201510726065A CN105271380A CN 105271380 A CN105271380 A CN 105271380A CN 201510726065 A CN201510726065 A CN 201510726065A CN 105271380 A CN105271380 A CN 105271380A
- Authority
- CN
- China
- Prior art keywords
- mixed solution
- mixed
- solution
- preparation
- mineralizer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of gadolinium-doped bismuth titanate with a nano-sheet cluster structure. The preparation method comprises the following steps of: 1, dropwise adding triethanolamine into isopropanol solution of tetra-isopropyl titanate to obtain a mixed solution A; 2, uniformly mixing the mixed solution of bismuth nitrate and gadolinium nitrate and ethylene glycol monomethyl ether to obtain a mixed solution B, and then dropwise adding the mixed solution A into the mixed solution B to obtain mixed solution C; 3, adding sodium dodecylbenzene sulfonate into the mixed solution C, obtaining xerogel after carrying out ultrasonic oscillation, vacuum standing and ultrasonic water bath processing, and then adding the xerogel into mineralizer solution to carry out stirring so as to obtain a mixed solution D; performing the microwave hydrothermal reaction to obtain suspension E; 5, sequentially carrying out centrifugation, washing and vacuum freeze drying processing to obtain the gadolinium-doped bismuth titanate with the nano-sheet cluster structure. The gadolinium-doped bismuth titanate powder prepared by the preparation method is high in purity, is narrow particle size distribution, is excellent in reaction activity and can be applicable to the field of photocatalysis degradation.
Description
Technical field
The invention belongs to inorganic functional material fabricating technology field, be specifically related to a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture.
Background technology
Ferroelectric material is a kind of important functional materials, has a series of excellent properties such as significant electrical polarization characteristics, dielectricity, piezoelectricity, pyroelectric, electrooptic effect, thus obtains the widespread use of people.In recent years, along with bismuth oxide-based layered perovskite ferroelectric material is in the important application in the piezoelectric device field of non-volatility ferroelectric random access memory (NVFRAM) and high-temperature high-frequency, and the extensive concern of scientific circles is subject to.Wherein, bismuth titanates Bi
4ti
3o (BIT) is a kind of typical three layers of bismuth layer perovskite structure Lead-free ferroelectric ceramics material, by (Bi
2ti
3o
10)
2-with (Bi
2o
2)
2+a kind of natural superlattice structure alternately stacking along c-axis direction, has higher Curie temperature, less relative permittivity, excellent mechanical quality.Further, it also has excellent photocatalysis performance, in novel energy and environment protection, also have extremely wide application prospect.
But bismuth titanates coercive field is at room temperature higher; Be difficult to fully be polarized and preparation temperature is higher, this is difficult to fully show with regard to making the ferroelectricity of this material, can not be widely used in daily life and produce.In recent years, investigator improves its performance by ion doping, the dopant ion of widespread use has strontium, samarium, lanthanum etc., and the correlative study adopting gadolinium (Gd) to carry out adulterating rarely has report, and the report especially adopting sol-gel microwave-hydrothermal method to be prepared is more rare.Applicant thinks, because ultrasonic wave added sol-gel microwave-hydrothermal method is temperature required lower, and the size distribution degree of material and sheet bunch property can effectively improve powder surface amass, increase reactive behavior obtain more dominance energy.And sheet clustering architecture can provide convenient for nanometer micro-processing technology etc., for the practical application of nano material lays the foundation, therefore has larger researching value.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture.The method adopts ultrasonic wave added sol-gel microwave hydrothermal preparation technology, can at a lower temperature, obtain the Bismuth Titanate Nanopowder of Gd2 O3 with single bismuth oxide-based layered perovskite orthorhombic phase, morphology controllable in the short period, made powder purity is high, narrow particle size distribution, reunion mild degree, grain component and form is controlled, reactive behavior is good.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture, and it is characterized in that, the method comprises the following steps:
Step one, tetra isopropyl titanate is dissolved in Virahol, obtains the aqueous isopropanol of tetra isopropyl titanate, then trolamine is added drop-wise in the aqueous isopropanol of described tetra isopropyl titanate, after ultrasonic wave mixes, obtains mixed liquor A; In described mixed liquor A, the volumn concentration of tetra isopropyl titanate is 5% ~ 10%;
Step 2, by Bismuth trinitrate and Gadolinium trinitrate in molar ratio 1: the mixed solution that (0.06 ~ 0.14) mixes mixes with Glacial acetic acid and ethylene glycol monomethyl ether ultrasonic wave, obtain mixed liquid B, then mixed liquor A described in step one is added drop-wise in described mixed liquid B, after ultrasonic wave mixes, obtains mixed solution C; In described mixed liquid B, the total concn of Bismuth trinitrate and Gadolinium trinitrate is 0.04mol/L ~ 0.08mol/L, and the volume ratio of described Glacial acetic acid and ethylene glycol monomethyl ether is (10 ~ 15): 1, and the volume ratio of described mixed liquor A and mixed liquid B is 1: 8;
Step 3, Sodium dodecylbenzene sulfonate is joined in the C of mixed solution described in step 2, ultra-sonic oscillation 0.5h ~ 1h final vacuum leaves standstill 3h ~ 5h, obtain colloidal sol, then described colloidal sol is joined in ultrasound bath pot, be that under the condition of 60 DEG C ~ 80 DEG C, ultra-sonic oscillation 30h ~ 40h carries out ultrasonic water bath process in temperature, obtain xerogel, described xerogel is joined in mineralizer solution stir 2h ~ 4h afterwards, obtain mixed solution D; The add-on of described xerogel adds 80g ~ 120g xerogel in often liter of mineralizer solution, described mineralizer solution to be mixed with deionized water by mineralizer and forms, described mineralizer be sodium hydroxide and potassium hydroxide in molar ratio (1 ~ 2): 1 mixed solution mixed;
Step 4, the D of mixed solution described in step 3 is added in warm-pressing double-control microwave hydrothermal reaction, be microwave hydrothermal reaction 20min ~ 60min under the condition of 140 DEG C ~ 200 DEG C in temperature, after naturally cooling, obtain suspension E;
Step 5, to the E of suspension described in step 4 carry out successively centrifugal, washing and vacuum lyophilization process, obtain the Gd2 O3 bismuth titanates with nanometer sheet clustering architecture.
Above-mentioned a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture, it is characterized in that, in the aqueous isopropanol of tetra isopropyl titanate described in step one, the concentration of tetra isopropyl titanate is 0.1mol/L ~ 0.2mol/L.
Above-mentioned a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture, is characterized in that, the speed dripped described in step one and step 2 is all not more than 6mL/min.
Above-mentioned a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture, is characterized in that, the add-on of Sodium dodecylbenzene sulfonate described in step 3 adds 0.05mol ~ 0.1mol dodecylbenzene naphthenic acid sodium in often liter of mixed solution C.
Above-mentioned a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture, it is characterized in that, in the solution of mineralizer described in step 3, concentration hydroxy is 2.5mol/L ~ 3.5mol/L.
The present invention compared with prior art has the following advantages:
1, the present invention adopts ultrasonic wave added sol-gel microwave hydrothermal preparation technology to prepare the bismuth titanates of Gd2 O3, can at a lower temperature (140 DEG C ~ 200 DEG C), obtain the Bismuth Titanate Nanopowder of Gd2 O3 with single bismuth oxide-based layered perovskite orthorhombic phase, morphology controllable in the short period (20min ~ 60min).The present invention is found by lot of experiments, and by controlling the mol ratio of bismuth and gadolinium, tetra isopropyl titanate is selected in titanium source, solvent selection Virahol, and adds the hydrolysis that a certain amount of triethanol amine can suppress tetra isopropyl titanate well.
2, the present invention selects tetra isopropyl titanate to be titanium source, Virahol is solvent, Bismuth trinitrate is bismuth source, sodium hydroxide and potassium hydroxide are mineralizer, pass through ultrasonic reaction, vacuum leaves standstill, the processes such as ultrasonic water bath, in the aqueous isopropanol of tetra isopropyl titanate and the acetic acid ethylene glycol monomethyl ether mixing solutions in bismuth source, there is ultrasonic hydrolysis complex reaction form vitreosol, colloidal sol dehydrating condensation under ultrasonic water bath forms xerogel, xerogel is dissolved in the mineralizer solution that sodium hydroxide and potassium hydroxide mixes, obtain reaction precursor liquid solution, be placed in warm-pressing double-control microwave hydrothermal reaction occur low temperature fast sol-gel microwave hydrothermal reaction, by regulating the concentration of mineralizer, thus obtain even-grained doped bismuth titanate nano-sheet powder, its length, width all controls at 20nm ~ 40nm, gauge control is at 3nm ~ 5nm, nano-powder pattern can manual control.
3, compared with traditional method, the present invention does not need high-temperature calcination, and product is directly crystalline state, and required equipment is simple, and preparation temperature is low, repeatable strong.Can pass through nucleation, growth and the adjustment in reaction times, realize the control that powder granule pattern, size are reunited, thus make that purity is high, narrow particle size distribution, reunion mild degree, grain component and form is controlled, reactive behavior is good nano-powder, the nano-powder preparation field of pattern, size tunable can be widely used in.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the SEM photo with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture prepared by the embodiment of the present invention 1.
Fig. 2 is the XRD figure with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture prepared by the embodiment of the present invention 1.
Embodiment
Embodiment 1
The preparation method that the present embodiment has the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture comprises the following steps:
Step one, be dissolved in Virahol by tetra isopropyl titanate, obtain the aqueous isopropanol of tetra isopropyl titanate, in the aqueous isopropanol of described tetra isopropyl titanate, the concentration of tetra isopropyl titanate is 0.15mol/L; Then trolamine is added drop-wise to the speed being not more than 6mL/min in the aqueous isopropanol of described tetra isopropyl titanate, after ultrasonic wave mixes, obtains mixed liquor A; In described mixed liquor A, the volumn concentration of tetra isopropyl titanate is 7.5%;
Step 2, by Bismuth trinitrate and Gadolinium trinitrate in molar ratio 1: 0.12 mixed solution mixed mix with Glacial acetic acid and ethylene glycol monomethyl ether ultrasonic wave, obtain mixed liquid B, then mixed liquor A described in step one is added drop-wise in described mixed liquid B with the speed being not more than 6mL/min, after ultrasonic wave mixes, obtains mixed solution C; In described mixed liquid B, the concentration of Bismuth trinitrate and the concentration sum of Gadolinium trinitrate are 0.05mol/L, and the volume ratio of described Glacial acetic acid and ethylene glycol monomethyl ether is 12: 1; The volume ratio of described mixed liquor A and mixed liquid B is 1: 8;
Step 3, according to the proportion scale adding 0.08mol dodecylbenzene naphthenic acid sodium in often liter of mixed solution C, Sodium dodecylbenzene sulfonate is added in the C of mixed solution described in step 2, ultra-sonic oscillation 0.5h final vacuum leaves standstill 4h, obtain colloidal sol, then the SL-24 ultrasound bath pot of Jintan Sheng Lan instrument manufacturing company limited is adopted to carry out ultrasonic water bath process to described colloidal sol, the temperature of ultrasonic water bath process is 70 DEG C, the time of ultrasonic water bath process is 35h, obtain xerogel, afterwards described xerogel is joined in mineralizer solution and stir 3h, obtain mixed solution D; The add-on of described xerogel adds 100g xerogel in often liter of mineralizer solution, described mineralizer solution to be mixed with deionized water by mineralizer and forms, described mineralizer is sodium hydroxide and the potassium hydroxide mixed solution that mixes of 1.5:1 in molar ratio, and in described mineralizer solution, concentration hydroxy is 3mol/L;
Step 4, the D of mixed solution described in step 3 is added in warm-pressing double-control microwave hydrothermal reaction, be microwave hydrothermal reaction 40min under the condition of 160 DEG C in temperature, after naturally cooling, obtain suspension E;
Step 5, to the E of suspension described in step 4 carry out successively centrifugal, washing and vacuum lyophilization process, obtain the Gd2 O3 bismuth titanates with nanometer sheet clustering architecture.
Fig. 1 is the SEM photo of Gd2 O3 bismuth titanates prepared by the present embodiment.As shown in Figure 1, Gd2 O3 bismuth titanate powder particle closely to be arranged cluster with nano-sheet, and even particle size distribution, wherein the length and width of nanometer sheet all control at 20nm ~ 40nm, and thickness is 3nm ~ 5nm.
Fig. 2 is the XRD figure of Gd2 O3 bismuth titanates prepared by the present embodiment.As shown in Figure 2, when the reaction times is between 40min ~ 90min, the peak shape of the XRD characteristic peak of reaction product there is no obvious increase, all with Bi
4ti
3o
12standard diffraction peak is consistent, and this illustrates that the crystallization when reaction times 40min of Gd2 O3 bismuth titanate powder is complete, and the position that Gd element instead of part Bi atom has completely entered among the lattice of metatitanic acid, synthesizes target product completely.Compare the method that Gd bismuth titanate nano-material is mixed in other preparation, the preparation time of the present embodiment obviously shortens, and has the advantage of energy-saving and emission-reduction.
Embodiment 2
The preparation method that the present embodiment has the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture comprises the following steps:
Step one, be dissolved in Virahol by tetra isopropyl titanate, obtain the aqueous isopropanol of tetra isopropyl titanate, in the aqueous isopropanol of described tetra isopropyl titanate, the concentration of tetra isopropyl titanate is 0.2mol/L; Then trolamine is added drop-wise to the speed being not more than 6mL/min in the aqueous isopropanol of described tetra isopropyl titanate, after ultrasonic wave mixes, obtains mixed liquor A; In described mixed liquor A, the volumn concentration of tetra isopropyl titanate is 5%;
Step 2, by Bismuth trinitrate and Gadolinium trinitrate in molar ratio 1: 0.14 mixed solution mixed mix with Glacial acetic acid and ethylene glycol monomethyl ether ultrasonic wave, obtain mixed liquid B, then mixed liquor A described in step one is added drop-wise in described mixed liquid B with the speed being not more than 6mL/min, after ultrasonic wave mixes, obtains mixed solution C; In described mixed liquid B, the concentration of Bismuth trinitrate and the concentration sum of Gadolinium trinitrate are 0.08mol/L, and the volume ratio of described Glacial acetic acid and ethylene glycol monomethyl ether is 15: 1; The volume ratio of described mixed liquor A and mixed liquid B is 1: 8;
Step 3, according to the proportion scale adding 0.1mol dodecylbenzene naphthenic acid sodium in often liter of mixed solution C, Sodium dodecylbenzene sulfonate is added in the C of mixed solution described in step 2, ultra-sonic oscillation 0.5h final vacuum leaves standstill 3h, obtain colloidal sol, then the SL-24 ultrasound bath pot of Jintan Sheng Lan instrument manufacturing company limited is adopted to carry out ultrasonic water bath process to described colloidal sol, the temperature of ultrasonic water bath process is 70 DEG C, the time of ultrasonic water bath process is 40h, obtain xerogel, afterwards described xerogel is joined in mineralizer solution and stir 2h, obtain mixed solution D; The add-on of described xerogel adds 120g xerogel in often liter of mineralizer solution, described mineralizer solution to be mixed with deionized water by mineralizer and forms, described mineralizer is sodium hydroxide and the potassium hydroxide mixed solution that mixes of 1:1 in molar ratio, and in described mineralizer solution, concentration hydroxy is 2.5mol/L;
Step 4, the D of mixed solution described in step 3 is added in warm-pressing double-control microwave hydrothermal reaction, be microwave hydrothermal reaction 60min under the condition of 140 DEG C in temperature, after naturally cooling, obtain suspension E;
Step 5, to the E of suspension described in step 4 carry out successively centrifugal, washing and vacuum lyophilization process, obtain the Gd2 O3 bismuth titanates with nanometer sheet clustering architecture.
The present embodiment adopts ultrasonic wave added sol-gel microwave hydrothermal preparation technology, can at a lower temperature, obtain the Bismuth Titanate Nanopowder of Gd2 O3 with single bismuth oxide-based layered perovskite orthorhombic phase, morphology controllable in the short period, made powder purity is high, narrow particle size distribution, reunion mild degree, grain component and form is controlled, reactive behavior is good.
Embodiment 3
The preparation method that the present embodiment has the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture comprises the following steps:
Step one, be dissolved in Virahol by tetra isopropyl titanate, obtain the aqueous isopropanol of tetra isopropyl titanate, in the aqueous isopropanol of described tetra isopropyl titanate, the concentration of tetra isopropyl titanate is 0.2mol/L; Then trolamine is added drop-wise to the speed being not more than 6mL/min in the aqueous isopropanol of described tetra isopropyl titanate, after ultrasonic wave mixes, obtains mixed liquor A; In described mixed liquor A, the volumn concentration of tetra isopropyl titanate is 10%;
Step 2, by Bismuth trinitrate and Gadolinium trinitrate in molar ratio 1: 0.13 mixed solution mixed mix with Glacial acetic acid and ethylene glycol monomethyl ether ultrasonic wave, obtain mixed liquid B, then mixed liquor A described in step one is added drop-wise in described mixed liquid B with the speed being not more than 6mL/min, after ultrasonic wave mixes, obtains mixed solution C; In described mixed liquid B, the concentration of Bismuth trinitrate and the concentration sum of Gadolinium trinitrate are 0.08mol/L, and the volume ratio of described Glacial acetic acid and ethylene glycol monomethyl ether is 12: 1; The volume ratio of described mixed liquor A and mixed liquid B is 1: 8;
Step 3, according to the proportion scale adding 0.05mol dodecylbenzene naphthenic acid sodium in often liter of mixed solution C, Sodium dodecylbenzene sulfonate is added in the C of mixed solution described in step 2, ultra-sonic oscillation 0.5h final vacuum leaves standstill 5h, obtain colloidal sol, then the SL-24 ultrasound bath pot of Jintan Sheng Lan instrument manufacturing company limited is adopted to carry out ultrasonic water bath process to described colloidal sol, the temperature of ultrasonic water bath process is 60 DEG C, the time of ultrasonic water bath process is 30h, obtain xerogel, afterwards described xerogel is joined in mineralizer solution and stir 2h, obtain mixed solution D; The add-on of described xerogel adds 80g xerogel in often liter of mineralizer solution, described mineralizer solution to be mixed with deionized water by mineralizer and forms, described mineralizer is sodium hydroxide and the potassium hydroxide mixed solution that mixes of 2:1 in molar ratio, and in described mineralizer solution, concentration hydroxy is 3.5mol/L;
Step 4, the D of mixed solution described in step 3 is added in warm-pressing double-control microwave hydrothermal reaction, be microwave hydrothermal reaction 60min under the condition of 140 DEG C in temperature, after naturally cooling, obtain suspension E;
Step 5, to the E of suspension described in step 4 carry out successively centrifugal, washing and vacuum lyophilization process, obtain the Gd2 O3 bismuth titanates with nanometer sheet clustering architecture.
The present embodiment adopts ultrasonic wave added sol-gel microwave hydrothermal preparation technology, can at a lower temperature, obtain the Bismuth Titanate Nanopowder of Gd2 O3 with single bismuth oxide-based layered perovskite orthorhombic phase, morphology controllable in the short period, made powder purity is high, narrow particle size distribution, reunion mild degree, grain component and form is controlled, reactive behavior is good.
Embodiment 4
The preparation method that the present embodiment has the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture comprises the following steps:
Step one, be dissolved in Virahol by tetra isopropyl titanate, obtain the aqueous isopropanol of tetra isopropyl titanate, in the aqueous isopropanol of described tetra isopropyl titanate, the concentration of tetra isopropyl titanate is 0.2mol/L; Then trolamine is added drop-wise to the speed being not more than 6mL/min in the aqueous isopropanol of described tetra isopropyl titanate, after ultrasonic wave mixes, obtains mixed liquor A; In described mixed liquor A, the volumn concentration of tetra isopropyl titanate is 10%;
Step 2, by Bismuth trinitrate and Gadolinium trinitrate in molar ratio 1: 0.06 mixed solution mixed mix with Glacial acetic acid and ethylene glycol monomethyl ether ultrasonic wave, obtain mixed liquid B, then mixed liquor A described in step one is added drop-wise in described mixed liquid B with the speed being not more than 6mL/min, after ultrasonic wave mixes, obtains mixed solution C; In described mixed liquid B, the concentration of Bismuth trinitrate and the concentration sum of Gadolinium trinitrate are 0.04mol/L, and the volume ratio of described Glacial acetic acid and ethylene glycol monomethyl ether is 12.5: 1; The volume ratio of described mixed liquor A and mixed liquid B is 1: 8;
Step 3, according to the proportion scale adding 0.05mol dodecylbenzene naphthenic acid sodium in often liter of mixed solution C, Sodium dodecylbenzene sulfonate is added in the C of mixed solution described in step 2, ultra-sonic oscillation 0.5h final vacuum leaves standstill 5h, obtain colloidal sol, then the SL-24 ultrasound bath pot of Jintan Sheng Lan instrument manufacturing company limited is adopted to carry out ultrasonic water bath process to described colloidal sol, the temperature of ultrasonic water bath process is 70 DEG C, the time of ultrasonic water bath process is 40h, obtain xerogel, afterwards described xerogel is joined in mineralizer solution and stir 4h, obtain mixed solution D; The add-on of described xerogel adds 120g xerogel in often liter of mineralizer solution, described mineralizer solution to be mixed with deionized water by mineralizer and forms, described mineralizer is sodium hydroxide and the potassium hydroxide mixed solution that mixes of 2:1 in molar ratio, and in described mineralizer solution, concentration hydroxy is 2.5mol/L;
Step 4, the D of mixed solution described in step 3 is added in warm-pressing double-control microwave hydrothermal reaction, be microwave hydrothermal reaction 20min under the condition of 140 DEG C in temperature, after naturally cooling, obtain suspension E;
Step 5, to the E of suspension described in step 4 carry out successively centrifugal, washing and vacuum lyophilization process, obtain the Gd2 O3 bismuth titanates with nanometer sheet clustering architecture.
The present embodiment adopts ultrasonic wave added sol-gel microwave hydrothermal preparation technology, can at a lower temperature, obtain the Bismuth Titanate Nanopowder of Gd2 O3 with single bismuth oxide-based layered perovskite orthorhombic phase, morphology controllable in the short period, made powder purity is high, narrow particle size distribution, reunion mild degree, grain component and form is controlled, reactive behavior is good.
Embodiment 5
The preparation method that the present embodiment has the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture comprises the following steps:
Step one, be dissolved in Virahol by tetra isopropyl titanate, obtain the aqueous isopropanol of tetra isopropyl titanate, in the aqueous isopropanol of described tetra isopropyl titanate, the concentration of tetra isopropyl titanate is 0.2mol/L; Then trolamine is added drop-wise to the speed being not more than 6mL/min in the aqueous isopropanol of described tetra isopropyl titanate, after ultrasonic wave mixes, obtains mixed liquor A; In described mixed liquor A, the volumn concentration of tetra isopropyl titanate is 5%;
Step 2, by Bismuth trinitrate and Gadolinium trinitrate in molar ratio 1: 0.05 mixed solution mixed mix with Glacial acetic acid and ethylene glycol monomethyl ether ultrasonic wave, obtain mixed liquid B, then mixed liquor A described in step one is added drop-wise in described mixed liquid B with the speed being not more than 6mL/min, after ultrasonic wave mixes, obtains mixed solution C; In described mixed liquid B, the concentration of Bismuth trinitrate and the concentration sum of Gadolinium trinitrate are 0.08mol/L, and the volume ratio of described Glacial acetic acid and ethylene glycol monomethyl ether is 10: 1; The volume ratio of described mixed liquor A and mixed liquid B is 1: 8;
Step 3, according to the proportion scale adding 0.1mol dodecylbenzene naphthenic acid sodium in often liter of mixed solution C, Sodium dodecylbenzene sulfonate is added in the C of mixed solution described in step 2, ultra-sonic oscillation 1h final vacuum leaves standstill 5h, obtain colloidal sol, then the SL-24 ultrasound bath pot of Jintan Sheng Lan instrument manufacturing company limited is adopted to carry out ultrasonic water bath process to described colloidal sol, the temperature of ultrasonic water bath process is 80 DEG C, the time of ultrasonic water bath process is 40h, obtain xerogel, afterwards described xerogel is joined in mineralizer solution and stir 4h, obtain mixed solution D; The add-on of described xerogel adds 120g xerogel in often liter of mineralizer solution, described mineralizer solution to be mixed with deionized water by mineralizer and forms, described mineralizer is sodium hydroxide and the potassium hydroxide mixed solution that mixes of 1.8:1 in molar ratio, and in described mineralizer solution, concentration hydroxy is 3.5mol/L;
Step 4, the D of mixed solution described in step 3 is added in warm-pressing double-control microwave hydrothermal reaction, be microwave hydrothermal reaction 20min under the condition of 200 DEG C in temperature, after naturally cooling, obtain suspension E;
Step 5, to the E of suspension described in step 4 carry out successively centrifugal, washing and vacuum lyophilization process, obtain the Gd2 O3 bismuth titanates with nanometer sheet clustering architecture.
The present embodiment adopts ultrasonic wave added sol-gel microwave hydrothermal preparation technology, can at a lower temperature, obtain the Bismuth Titanate Nanopowder of Gd2 O3 with single bismuth oxide-based layered perovskite orthorhombic phase, morphology controllable in the short period, made powder purity is high, narrow particle size distribution, reunion mild degree, grain component and form is controlled, reactive behavior is good.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (5)
1. have a preparation method for the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture, it is characterized in that, the method comprises the following steps:
Step one, tetra isopropyl titanate is dissolved in Virahol, obtains the aqueous isopropanol of tetra isopropyl titanate, then trolamine is added drop-wise in the aqueous isopropanol of described tetra isopropyl titanate, after ultrasonic wave mixes, obtains mixed liquor A; In described mixed liquor A, the volumn concentration of tetra isopropyl titanate is 5% ~ 10%;
Step 2, by Bismuth trinitrate and Gadolinium trinitrate in molar ratio 1: the mixed solution that (0.06 ~ 0.14) mixes mixes with Glacial acetic acid and ethylene glycol monomethyl ether ultrasonic wave, obtain mixed liquid B, then mixed liquor A described in step one is added drop-wise in described mixed liquid B, after ultrasonic wave mixes, obtains mixed solution C; In described mixed liquid B, the total concn of Bismuth trinitrate and Gadolinium trinitrate is 0.04mol/L ~ 0.08mol/L, and the volume ratio of described Glacial acetic acid and ethylene glycol monomethyl ether is (10 ~ 15): 1, and the volume ratio of described mixed liquor A and mixed liquid B is 1: 8;
Step 3, Sodium dodecylbenzene sulfonate is joined in the C of mixed solution described in step 2, ultra-sonic oscillation 0.5h ~ 1h final vacuum leaves standstill 3h ~ 5h, obtain colloidal sol, then described colloidal sol is joined in ultrasound bath pot, be that under the condition of 60 DEG C ~ 80 DEG C, ultra-sonic oscillation 30h ~ 40h carries out ultrasonic water bath process in temperature, obtain xerogel, described xerogel is joined in mineralizer solution stir 2h ~ 4h afterwards, obtain mixed solution D; The add-on of described xerogel adds 80g ~ 120g xerogel in often liter of mineralizer solution, described mineralizer solution to be mixed with deionized water by mineralizer and forms, described mineralizer be sodium hydroxide and potassium hydroxide in molar ratio (1 ~ 2): 1 mixed solution mixed;
Step 4, the D of mixed solution described in step 3 is added in warm-pressing double-control microwave hydrothermal reaction, be microwave hydrothermal reaction 20min ~ 60min under the condition of 140 DEG C ~ 200 DEG C in temperature, after naturally cooling, obtain suspension E;
Step 5, to the E of suspension described in step 4 carry out successively centrifugal, washing and vacuum lyophilization process, obtain the Gd2 O3 bismuth titanates with nanometer sheet clustering architecture.
2. a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture according to claim 1, it is characterized in that, in the aqueous isopropanol of tetra isopropyl titanate described in step one, the concentration of tetra isopropyl titanate is 0.1mol/L ~ 0.2mol/L.
3. a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture according to claim 1, is characterized in that, the speed dripped described in step one and step 2 is all not more than 6mL/min.
4. a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture according to claim 1, it is characterized in that, the add-on of Sodium dodecylbenzene sulfonate described in step 3 adds 0.05mol ~ 0.1mol dodecylbenzene naphthenic acid sodium in often liter of mixed solution C.
5. a kind of preparation method with the Gd2 O3 bismuth titanates of nanometer sheet clustering architecture according to claim 1, it is characterized in that, in the solution of mineralizer described in step 3, concentration hydroxy is 2.5mol/L ~ 3.5mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510726065.9A CN105271380A (en) | 2015-10-31 | 2015-10-31 | Preparation method of gadolinium-doped bismuth titanate with nano-sheet cluster structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510726065.9A CN105271380A (en) | 2015-10-31 | 2015-10-31 | Preparation method of gadolinium-doped bismuth titanate with nano-sheet cluster structure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105271380A true CN105271380A (en) | 2016-01-27 |
Family
ID=55141319
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510726065.9A Pending CN105271380A (en) | 2015-10-31 | 2015-10-31 | Preparation method of gadolinium-doped bismuth titanate with nano-sheet cluster structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105271380A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111569913A (en) * | 2020-05-13 | 2020-08-25 | 南昌航空大学 | Gd (Gd)3+Preparation method of doped BiOBr photocatalytic material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821087A (en) * | 2006-03-06 | 2006-08-23 | 湖北大学 | Neodymium doped bismuth titanate nano line array ferro-electric storage material and its synthetic method |
| CN101219813A (en) * | 2008-01-24 | 2008-07-16 | 浙江大学 | Iron doped sodium-bismuth titanate multiferroics and method for producing the same |
| CN101229930A (en) * | 2008-01-24 | 2008-07-30 | 浙江大学 | Nickel doped bismuth sodium titanate multiferroics and preparation method thereof |
| CN101767818A (en) * | 2010-01-21 | 2010-07-07 | 上海大学 | Ion-doped potassium bismuth titanate nano powder and preparation method thereof |
| CN102963929A (en) * | 2012-11-16 | 2013-03-13 | 华南理工大学 | Method for preparing lanthanum-doped bismuth titanate nano powder by sol-gel hydrothermal method |
-
2015
- 2015-10-31 CN CN201510726065.9A patent/CN105271380A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821087A (en) * | 2006-03-06 | 2006-08-23 | 湖北大学 | Neodymium doped bismuth titanate nano line array ferro-electric storage material and its synthetic method |
| CN101219813A (en) * | 2008-01-24 | 2008-07-16 | 浙江大学 | Iron doped sodium-bismuth titanate multiferroics and method for producing the same |
| CN101229930A (en) * | 2008-01-24 | 2008-07-30 | 浙江大学 | Nickel doped bismuth sodium titanate multiferroics and preparation method thereof |
| CN101767818A (en) * | 2010-01-21 | 2010-07-07 | 上海大学 | Ion-doped potassium bismuth titanate nano powder and preparation method thereof |
| CN102963929A (en) * | 2012-11-16 | 2013-03-13 | 华南理工大学 | Method for preparing lanthanum-doped bismuth titanate nano powder by sol-gel hydrothermal method |
Non-Patent Citations (1)
| Title |
|---|
| 康雄兵: "稀土掺杂钛酸铋纳米粉体的湿化学法合成及表征", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111569913A (en) * | 2020-05-13 | 2020-08-25 | 南昌航空大学 | Gd (Gd)3+Preparation method of doped BiOBr photocatalytic material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106946566B (en) | Preparation method of flaky barium strontium titanate powder material | |
| CN102534794B (en) | Preparation method for perovskite lead titanate single-crystal nanometer sheet | |
| CN102963929B (en) | Method for preparing lanthanum-doped bismuth titanate nano powder by sol-gel hydrothermal method | |
| CN103276448B (en) | A kind of preparation method of perovskite structure lead titanate monocrystal nano sheet | |
| CN102925979B (en) | Method for preparing perovskite lead titanate crystal nanosheet | |
| CN102583517B (en) | Preparation method of strontium titanate nanometer piece | |
| CN101619494A (en) | Method for preparing perovskite structure lead titanate monocrystal nano rod | |
| CN102691105A (en) | Method for preparing barium titanate monocrystal nano particles of six-pin structural perovskite | |
| CN103553589B (en) | Method for preparing CaCu3Ti4O12 ceramic material | |
| CN102531582B (en) | Method for preparing sodium bismuth titanate nanometer sheet | |
| CN105040090A (en) | Preparation method of lead titanate-strontium titanate monocrystal nanometer material with core-shell structure | |
| CN102923766B (en) | Preparation method of lead-titanate ceramic single-crystal nanosheet | |
| CN101831710B (en) | Method for preparing lead titanate monocrystal nanometer branch crystal with perovskite structure | |
| CN103739008A (en) | Flaky bismuth lanthanum titanate nano-crystal and preparation method thereof | |
| CN102060325B (en) | Tetragonal-phase barium titanate nanorod array and preparation method thereof | |
| CN106187163A (en) | A kind of high tetragonal-phase barium titanate of rare earth neodymium doping and preparation method thereof | |
| CN102677145B (en) | Preparation method of perovskite structure lead titanate single crystal nanoparticles | |
| CN102515263B (en) | Preparation method of barium strontium titanate stellar crystal | |
| CN102877131B (en) | Preparation method of octahedral structural perovskite lead titanate single crystal nano particles | |
| CN101100310A (en) | Preparation method for nanometer barium titanate | |
| CN102674442A (en) | Method for preparing strontium titanate nano powder through microwave hydrothermal method | |
| CN105271380A (en) | Preparation method of gadolinium-doped bismuth titanate with nano-sheet cluster structure | |
| CN102925980B (en) | Preparation method of tetragonal perovskite structure lead zirconate ceramic single crystal nanosheet | |
| CN104402433A (en) | Preparation method for low-loss and high-resistivity Bi4Ti3O12-based lead-free piezoelectric ceramics | |
| CN104891559B (en) | With titanium dioxide for titanium source synthesis Li doping PbTiO3the method of nano-particle and product and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160127 |