CN107673403A - A kind of preparation method of layered titanic acid strontium - Google Patents
A kind of preparation method of layered titanic acid strontium Download PDFInfo
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- CN107673403A CN107673403A CN201711014501.5A CN201711014501A CN107673403A CN 107673403 A CN107673403 A CN 107673403A CN 201711014501 A CN201711014501 A CN 201711014501A CN 107673403 A CN107673403 A CN 107673403A
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- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
A kind of preparation method of layered titanic acid strontium, according to SrO (SrTiO3)2Stoichiometric proportion, weigh butyl titanate and strontium nitrate；Complexing agent is added into the ethanol solution of butyl titanate, stirs to complexing agent and dissolves, obtain mixed solution；Strontium nitrate solution is added in mixed solution, is well mixed, then heating obtains the sol of homogeneous transparent, is dried to obtain xerogel after standing, is sintered after xerogel is ground, obtains layered titanic acid strontium.The present invention is due to using sol-gal process so the layered titanic acid strontium of pure phase can be obtained, particle diameter distribution is uniform, preferred orientation is obvious, diameter is high with thickness ratio, and two dimensional character is obvious, effectively reduces its sintering temperature, and impurity is not easily introduced in preparation process and technical process simple operations are convenient, by the layered titanic acid strontium powder application of the present invention in thermoelectric material, its superior thermoelectricity capability in addition its natural preferred orientation growth the characteristics of, can effectively improve horizontal thermoelectricity capability parameter.
Description
Technical field
The present invention relates to materials science field, and in particular to a kind of preparation method of layered titanic acid strontium.
Background technology
In recent years, the research of lamellar compound is increasingly subject to the attention of more and more people, is turned to by traditional three-dimensional material
The research of low-dimensional materials, due to the layer structure of uniqueness, its interlayer turns into chemical reactivity center, layer structure and interlayer
Learning reactivity makes it be had broad application prospects in numerous areas such as ion exchange, absorption, conduction, separation and catalysis, this
Its application has been widened significantly.And layered titanic acid strontium does not only belong to the high temperature conventional thermoelectric materials of excellent performance, but also have
There is natural layer structure so that its research is paid much attention to by scientific research personnel.
Strontium titanates sintering temperature height is prepared in the prior art, and impurity is easily introduced in preparation process, the product grain of preparation
Spend uneven.
The content of the invention
To overcome the problems of the prior art, it is an object of the invention to provide a kind of method for preparing layered titanic acid strontium.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of layered titanic acid strontium, according to SrO (SrTiO3)2Stoichiometric proportion, weigh butyl titanate and
Strontium nitrate；Complexing agent is added into the ethanol solution of butyl titanate, stirs to complexing agent and dissolves, obtain mixed solution；By nitre
Sour strontium solution is added in mixed solution, is well mixed, and then heating obtains the sol of homogeneous transparent, is dried to obtain after standing
Xerogel, sintered after xerogel is ground, obtain layered titanic acid strontium.
Further improve of the invention is that the ethanol solution of butyl titanate is made by procedure below：By metatitanic acid four
Butyl ester is dissolved in absolute ethyl alcohol, obtains the ethanol solution of butyl titanate, and the ratio of butyl titanate and ethanol is 0.1mol：
500mL。
Further improve of the invention is that the addition of complexing agent is the 1.0~2.2 of titanium and the amount of the total material of strontium
Times.
Further improve of the invention is that complexing agent is citric acid.
Further improve of the invention is that strontium nitrate solution is that strontium titanates is added in deionized water to be made, and
Strontium titanates and the ratio of deionized water are 0.1mol：500mL.
Further improve of the invention is that the temperature of heating is 60 DEG C, and the time of heating is 1~4h.
Further improve of the invention is that drying is specifically carried out in two stages, and first stage temperature is 60~120,
Time is 1~10h, and second stage temperature is 121~130 DEG C, and the time is 1~10h.
Further improve of the invention is that the time of standing is 24~48h.
Further improve of the invention is that sintering temperature is 800~1100 DEG C, and the time is 2~8h.
Compared with prior art, the device have the advantages that：The present invention utilizes strontium nitrate, butyl titanate, complexing agent
The presoma of layered titanic acid strontium is prepared using sol-gal process Deng raw material, then layered titanic acid strontium powder is made through calcining.The present invention
It is average because using sol-gal process, so the layered titanic acid strontium of pure phase can be obtained, particle diameter distribution is uniform, and preferred orientation is obvious
Particle size is 400nm, and diameter is high with thickness ratio, and two dimensional character is obvious, relatively conventional preparation method, effectively reduces it
Sintering temperature, and impurity and technical process simple operations convenience are not easily introduced in preparation process, overcome traditional high temperature and consolidate
Phase method easily generates the strontium titanates of Emission in Cubic this shortcoming.By the layered titanic acid strontium powder application of the present invention in thermoelectric material, its
Superior thermoelectricity capability in addition its natural preferred orientation growth the characteristics of, can effectively improve horizontal thermoelectricity capability parameter,
Prospect is considerable.
Brief description of the drawings
Fig. 1 is the heat flow curve of the DSC tests of precursor powder prepared by the embodiment of the present invention 1；
Fig. 2 is the thermogravimetric curve of the DSC tests of precursor powder prepared by the embodiment of the present invention 1；
Fig. 3 is X-ray diffractogram of the layered titanic acid strontium powder under 1000 DEG C of heat treatment prepared by the embodiment of the present invention 1
Spectrum；
Fig. 4 is surface sweeping Electronic Speculum of the layered titanic acid strontium powder under 1000 DEG C of heat treatment prepared by the embodiment of the present invention 1
(SEM) photo.
Embodiment
Below in conjunction with the present invention is described in further detail with the drawings and specific embodiments：
Embodiment 1
(1), raw material uses butyl titanate, citric acid, strontium nitrate, absolute ethyl alcohol and deionized water.According to SrO
(SrTiO3)2Stoichiometric weighs butyl titanate 3.4032g, citric acid 15g, strontium nitrate 4.2326g, absolute ethyl alcohol
60mL, deionized water 60mL；
(2), 3.4032g butyl titanate is dissolved in the beaker A for filling 60mL absolute ethyl alcohols under room temperature state, is placed on
Being stirred two hours with 50~200r/min rotating speeds on magnetic stirring apparatus makes it fully dissolve；
(3) the complexing agent citric acid that 15g, is weighed under room temperature state is added in A beakers, is continued on magnetic stirring apparatus with 50
~200r/min rotating speeds stir one hour, make its dissolving, obtain clear solution A；
(4) strontium nitrate that 4.2326g, is weighed under room temperature state is dissolved in the beaker B for the deionized water for filling 60mL, is placed on
Being stirred two hours with 50~200r/min rotating speeds on magnetic stirring apparatus makes it fully dissolve；
(5), the solution in beaker B is slowly added drop-wise in beaker A, is added dropwise 150 minutes altogether, makes it well mixed, obtains
To solution C；When just starting to be added dropwise, color can gradually change to micro- white by clarifying, then have and micro- be back in vain with the change that continues back of dropwise addition
Pellucidity；
(6), solution C is placed on magnetic stirring apparatus, 60 DEG C of heating water baths are stirred 2 hours with 50~200r/min rotating speeds,
It is fully reacted, obtain the colloidal sol of homogeneous transparent, during which color does not have any change；
(7), obtained colloidal sol is placed in ventilating kitchen and stands 24 hours, its internal structure is tended towards stability state；
(8), colloidal sol is put into 120 DEG C of baking oven and dried 2 hours, will not be precipitated in drying process, but in drying
At 40 minutes, solution colour can turn white, and subsequent color can change to jaundice state from state of turning white, and occur without precipitation.Heat up afterwards
Dried 5 hours to 140 DEG C, obtain the cellular xerogel of yellow；
(9), xerogel is placed in agate mortar and is fully ground, presoma is made；
(10), presoma is put into sintering furnace at 1000 DEG C, 4h is sintered under atmospheric atmosphere, then using agate
Mortar grinder obtains layered titanic acid strontium.
Figure it is seen that it is observed that the weight of sample significantly reduces, but the weight of different samples reduces hair
Life is within the scope of different temperature.It is due to when temperature raises, caused by organic matter is decomposed that weight, which is reduced,.Arrived in room temperature
The reduction of weight is mainly the dehydration of gel in the range of 200 DEG C；Weight is remarkably decreased after 200 DEG C, is because machine function
Group proceeds by thermal decomposition, changes after 600 DEG C and little, now target product initially forms.Accordingly in Fig. 1,100~
The exothermic peak occurred in the range of 400 DEG C is mainly the decomposition of large amount of organic, and mainly organo-functional group proceeds by thermal decomposition,
These functional groups mainly include citric acid and butyl ester group etc.；Exothermic peak in the range of 400~600 DEG C be residual organic substances and
NO3- decomposition；The endothermic peak occurred in the range of 600~1000 DEG C makes weight lose seldom, and this is Sr2TiO4Particle amorphous arrives
Polycrystalline changes and Sr2TiO4The formation of phase；Curvilinear motion is very small after 1000 DEG C, it is possible thereby to estimate its firing temperature.
From figure 3, it can be seen that when sintering 4 hours, only SrO (SrTiO on XRD3) diffraction maximum, illustrate at this temperature
Obtained target product is pure phase.
From fig. 4, it can be seen that when heat treatment temperature is 1000 DEG C, electromicroscopic photograph can be seen that compound with layered form
In the presence of this is consistent with XRD anticipations.
Embodiment 2
(1), raw material uses butyl titanate, citric acid, strontium nitrate, absolute ethyl alcohol and deionized water.According to SrO
(SrTiO3)2Stoichiometric weighs butyl titanate 3.4042g, citric acid 10g, strontium nitrate 4.2359g, absolute ethyl alcohol
35mL, deionized water 35mL；
(2), 3.4032g butyl titanate is dissolved in the beaker A for filling 35mL absolute ethyl alcohols under room temperature state, is placed on
Being stirred one hour with 50~200r/min rotating speeds on magnetic stirring apparatus makes it fully dissolve；
(3) the complexing agent citric acid that 10g, is weighed under room temperature state is added in A beakers, on magnetic stirring apparatus with 50~
200r/min rotating speeds continue to stir half an hour, make its dissolving, obtain clear solution A；
(4) strontium nitrate that 4.2359g, is weighed under room temperature state is dissolved in the beaker B for the deionized water for filling 35mL, is placed on
Being stirred three hours with 50~200r/min rotating speeds on magnetic stirring apparatus makes it fully dissolve；
(5), the solution in beaker B is slowly added drop-wise in beaker A, is added dropwise 180 minutes altogether, makes it well mixed, obtains
To solution C；When just starting to be added dropwise, color can gradually change to micro- white by clarifying, then have and micro- be back in vain with the change that continues back of dropwise addition
Pellucidity；
(6), solution C is placed on magnetic stirring apparatus, 60 DEG C of heating water baths stir 3 hours under 50~200r/min, make
It fully reacts, and obtains the colloidal sol of homogeneous transparent, and during which color does not have any change；
(7), obtained colloidal sol is placed in ventilating kitchen and stands 36 hours, its internal structure is tended towards stability state；
(8), colloidal sol is put into 130 DEG C of baking oven and dried two hours, will not be precipitated in drying process, but in drying
At 20 minutes, solution colour can turn white, and subsequent color can change to jaundice state from state of turning white, and occur without precipitation.Heat up afterwards
Dried 4 hours to 150 DEG C, obtain the cellular xerogel of yellow；
(9), xerogel is placed in agate mortar and is fully ground, presoma is made；
(10), presoma is put into sintering furnace at 950 DEG C, 4h is sintered under atmospheric atmosphere, then using agate
Mortar grinder obtains layered titanic acid strontium.
Embodiment 3
(1), raw material uses butyl titanate, citric acid, strontium nitrate, absolute ethyl alcohol and deionized water.According to SrO
(SrTiO3)2Stoichiometric weighs butyl titanate 3.4017g, citric acid 8g, strontium nitrate 4.2331g, absolute ethyl alcohol
40mL, deionized water 40mL；
(2), 3.4017g butyl titanate is dissolved in the beaker A for filling 40mL absolute ethyl alcohols under room temperature state, is placed on
Being stirred 80 minutes with 50~200r/min rotating speeds on magnetic stirring apparatus makes it fully dissolve；
(3) the complexing agent citric acid that 8g, is weighed under room temperature state is added in A beakers, on magnetic stirring apparatus with 50~
200r/min rotating speeds continue to stir half an hour, make its dissolving, obtain clear solution A；
(4) strontium nitrate that 4.2331g, is weighed under room temperature state is dissolved in the beaker B for the deionized water for filling 40mL, is placed on
Being stirred two hours with 50~200r/min rotating speeds on magnetic stirring apparatus makes it fully dissolve；
(5), the solution in beaker B is slowly added drop-wise in beaker A, is added dropwise 135 minutes altogether, makes it well mixed, obtains
To solution C；When just starting to be added dropwise, color can gradually change to micro- white by clarifying, then have and micro- be back in vain with the change that continues back of dropwise addition
Pellucidity；
(6), solution C is placed on magnetic stirring apparatus, 60 DEG C of heating water baths are stirred 1 hour with 50~200r/min rotating speeds,
It is fully reacted, obtain the colloidal sol of homogeneous transparent, during which color does not have any change；
(7), obtained colloidal sol is placed in ventilating kitchen and stands 12 hours, its internal structure is tended towards stability state；
(8), colloidal sol is put into 60 DEG C of baking oven and dried two hours, is then placed in 140 DEG C of baking oven and dries two hours,
It will not be precipitated in drying process, but when drying 15 minutes, solution colour can turn white, and subsequent color can become from state of turning white
To jaundice state, precipitation is occurred without.Obtain the cellular xerogel of yellow；
(9), xerogel is placed in agate mortar and is fully ground, presoma is made；
(10), presoma is put into sintering furnace at 1050 DEG C, is sintered under atmospheric atmosphere 3 hours, then uses
Agate mortar grinds to obtain layered titanic acid strontium.
Embodiment 4
According to SrO (SrTiO3)2Stoichiometric proportion, weigh butyl titanate and strontium nitrate；Butyl titanate is dissolved in nothing
In water-ethanol, the ethanol solution of butyl titanate is obtained, and the ratio of butyl titanate and ethanol is 0.1mol：500mL.By titanium
Sour strontium is added in deionized water and is made, and strontium titanates and the ratio of deionized water are 0.1mol：500mL.
Citric acid is added into the ethanol solution of butyl titanate, stirs to citric acid and dissolves, obtain mixed solution；By nitre
Sour strontium solution is added in mixed solution, is well mixed, and is then heated 1h at 60 DEG C, is obtained the sol of homogeneous transparent, is stood
10h is first dried after 24h at 60 DEG C, 10h is dried at 121 DEG C, obtains xerogel, 8h at 800 DEG C after xerogel is ground
Sintering, obtains layered titanic acid strontium.Wherein the addition of citric acid is 1.0 times of the amount of titanium and the total material of strontium.
Embodiment 5
According to SrO (SrTiO3)2Stoichiometric proportion, weigh butyl titanate and strontium nitrate；Butyl titanate is dissolved in nothing
In water-ethanol, the ethanol solution of butyl titanate is obtained, and the ratio of butyl titanate and ethanol is 0.1mol：500mL.By titanium
Sour strontium is added in deionized water and is made, and strontium titanates and the ratio of deionized water are 0.1mol：500mL.
Citric acid is added into the ethanol solution of butyl titanate, stirs to citric acid and dissolves, obtain mixed solution；By nitre
Sour strontium solution is added in mixed solution, is well mixed, and is then heated 2h at 60 DEG C, is obtained the sol of homogeneous transparent, is stood
1h is first dried after 48h at 120 DEG C, 1h is dried at 200 DEG C, obtains xerogel, 2h at 1100 DEG C after xerogel is ground
Sintering, obtains layered titanic acid strontium.Wherein the addition of citric acid is 2.2 times of the amount of titanium and the total material of strontium.
Embodiment 6
According to SrO (SrTiO3)2Stoichiometric proportion, weigh butyl titanate and strontium nitrate；Butyl titanate is dissolved in nothing
In water-ethanol, the ethanol solution of butyl titanate is obtained, and the ratio of butyl titanate and ethanol is 0.1mol：500mL.By titanium
Sour strontium is added in deionized water and is made, and strontium titanates and the ratio of deionized water are 0.1mol：500mL.
Citric acid is added into the ethanol solution of butyl titanate, stirs to citric acid and dissolves, obtain mixed solution；By nitre
Sour strontium solution is added in mixed solution, is well mixed, and is then heated 4h at 60 DEG C, is obtained the sol of homogeneous transparent, is stood
5h is first dried after 35h at 80 DEG C, 4h is dried at 150 DEG C, obtains xerogel, 5h burns at 1000 DEG C after xerogel is ground
Knot, obtains layered titanic acid strontium.Wherein the addition of citric acid is 1.5 times of the amount of titanium and the total material of strontium.
The specific steps of the inventive method mainly include：(1) preparation of layered titanic acid strontium presoma；(2) layered titanic acid strontium
The preparation of powder.Layered titanic acid strontium powder grain prepared by the present invention is evenly distributed, and average grain size is 400nm or so.
Diameter is high with thickness ratio, and two dimensional character is obvious, relatively conventional preparation method, effectively reduces its sintering temperature, technique letter
Single operation is convenient, there is huge application prospect.
Claims (9)
1. a kind of preparation method of layered titanic acid strontium, it is characterised in that according to SrO (SrTiO3)2Stoichiometric proportion, weigh titanium
Sour four butyl esters and strontium nitrate；Complexing agent is added into the ethanol solution of butyl titanate, stirs to complexing agent and dissolves, mixed
Solution；Strontium nitrate solution is added in mixed solution, is well mixed, then heating obtains the sol of homogeneous transparent, stands
After be dried to obtain xerogel, sintered after xerogel is ground, obtain layered titanic acid strontium.
A kind of 2. preparation method of layered titanic acid strontium according to claim 1, it is characterised in that the ethanol of butyl titanate
Solution is made by procedure below：Butyl titanate is dissolved in absolute ethyl alcohol, obtains the ethanol solution of butyl titanate, and
The ratio of butyl titanate and ethanol is 0.1mol：500mL.
3. the preparation method of a kind of layered titanic acid strontium according to claim 1, it is characterised in that the addition of complexing agent is
1.0~2.2 times of the amount of titanium and the total material of strontium.
4. the preparation method of a kind of layered titanic acid strontium according to claim 1 or 3, it is characterised in that complexing agent is lemon
Acid.
5. the preparation method of a kind of layered titanic acid strontium according to claim 1, it is characterised in that strontium nitrate solution is by titanium
Sour strontium is added in deionized water and is made, and strontium titanates and the ratio of deionized water are 0.1mol：500mL.
6. the preparation method of a kind of layered titanic acid strontium according to claim 1, it is characterised in that the temperature of heating is 60
DEG C, the time of heating is 1~4h.
7. the preparation method of a kind of layered titanic acid strontium according to claim 1, it is characterised in that drying is specifically divided to two ranks
Duan Jinhang, first stage temperature are 60~120, and the time be 1~10h, and second stage temperature is 121~130 DEG C, the time for 1~
10h。
A kind of 8. preparation method of layered titanic acid strontium according to claim 1, it is characterised in that the time of standing be 24~
48h。
A kind of 9. preparation method of layered titanic acid strontium according to claim 1, it is characterised in that sintering temperature be 800~
1100 DEG C, the time is 2~8h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589879A (en) * | 2019-10-11 | 2019-12-20 | 浙江大学 | Preparation of Sr by alkaline sol-gel method2TiO4Method for preparing nano powder |
| CN115504503A (en) * | 2022-09-26 | 2022-12-23 | 陕西科技大学 | Niobium-doped cubic-phase two-dimensional sheet strontium titanate material and preparation method thereof |
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| CN101423243A (en) * | 2008-11-25 | 2009-05-06 | 北京科技大学 | La doped SrTiO3 base oxide pyroelectric material and preparation method |
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- 2017-10-26 CN CN201711014501.5A patent/CN107673403A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101423243A (en) * | 2008-11-25 | 2009-05-06 | 北京科技大学 | La doped SrTiO3 base oxide pyroelectric material and preparation method |
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| N. ZHOU ET AL.: "Synthesis of SrO(SrTiO3)n (n = 1, 2, 1) compounds and electronic structure analysis", 《MATERIALS RESEARCH BULLETIN》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589879A (en) * | 2019-10-11 | 2019-12-20 | 浙江大学 | Preparation of Sr by alkaline sol-gel method2TiO4Method for preparing nano powder |
| CN115504503A (en) * | 2022-09-26 | 2022-12-23 | 陕西科技大学 | Niobium-doped cubic-phase two-dimensional sheet strontium titanate material and preparation method thereof |
| CN115504503B (en) * | 2022-09-26 | 2023-09-05 | 陕西科技大学 | Niobium-doped cubic phase two-dimensional flaky strontium titanate material and preparation method thereof |
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