CN106554035A - The method that Sr titanate powder is prepared using molten-salt growth method - Google Patents
The method that Sr titanate powder is prepared using molten-salt growth method Download PDFInfo
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- CN106554035A CN106554035A CN201510616759.7A CN201510616759A CN106554035A CN 106554035 A CN106554035 A CN 106554035A CN 201510616759 A CN201510616759 A CN 201510616759A CN 106554035 A CN106554035 A CN 106554035A
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Abstract
The present invention relates to the method for preparing Sr titanate powder using molten-salt growth method, the preparation method includes：Step 1）It is 1 by molal weight ratio：1SrCO3And TiO2Mixture be well mixed with fused-salt medium and nonionic surfactant, in 700～800 DEG C react 4～12 hours, be cooled to room temperature, wherein, the SrCO3And TiO2Mixture gross mass and the fused salt mass ratio be 1：5～1：10, the SrCO3And TiO2Mixture gross mass and the nonionic surfactant mass ratio be 1：3～1：6；Step 2）By step 1）The product of gained is at least washed once, and 100 DEG C are dried 4～8 hours in an oven.Compared with prior art, the preparation method reaction temperature is low, process is simple, environmental protection, obtained Sr titanate powder complete crystallization, even particle size distribution.
Description
Technical field
The invention belongs to technical field of material chemistry, and in particular to a kind of preparation method of Sr titanate powder.
Background technology
In metal material, organic and inorganic nonmetallic materials, add appropriate strontium and its compound can change some performances very
To making it have specific function, the title of intrinsic " metal monosodium glutamate ".In strontium resource, strontium titanates (SrTiO3) it is exactly wherein one
Plant important compound.Strontium titanates has superconductivity, Semiconductor gas sensors, thermal sensitivity and light sensitivity, and dielectric loss is low, color
Scattered frequency is high, in addition also high-k, low-dielectric loss the advantages of.Compared with calcium material, with more preferable temperature stabilization
Property and high withstand voltage intensity, be, using a kind of wider ceramic material, to can be used to manufacture grain-boundary layer capacitor, PTC in electronics industry
Thermistor, high-voltage capacitor, oxygen sensitive element, capacitor varistor multifunction original paper；Replace SiO with it in holder2Can
Storage is made to improve more than 30 times；Oxygen sensitive element is made in addition for controlling the lambda sensor of automobile lean burn；Other strontium titanates
The fields such as photocatalytic hydrogen production by water decomposition, photocatalytic degradation organic contamination are widely used in photocatalysis performance.
At present, Sr titanate powder preparation method has many kinds, mainly has sol-gel, chemical precipitation method, high temperature solid-state
Method, microwave method, plasma method and hydro-thermal method.Solid phase method is a kind of method that tradition prepares strontium titanates powder, with cost
The advantage of low, preparation process is simple.Although solid reaction process can be prepared on a large scale, wherein still exist many inevitable
Shortcoming as prepare powder grain size it is big, chemical uniformity is poor, it is easy reunion and powder purity it is not high, especially need height
Temperature.Other several methods can obtain high-purity, single phase structure, nanometer grade powder, have the disadvantage that reaction is complicated, long flow path,
Combined coefficient is low, and building-up process can produce environmentally harmful waste water.As Chinese patent CN102674442A is reported
Add titanate esters, ethanol and acetic acid, then strontium ion is added dropwise in " method for strontium titanate nano powder being prepared using microwave-hydrothermal method "
The aqueous solution, forms colloidal sol, afterwards plus alkali, adjusts pH to 8～14, obtains precursor pulp, and precursor pulp is placed in reactor
In, carry out microwave hydrothermal reaction, product is separated, be dried after obtain strontium titanate nano powder.The method step is more, need
Strictly to control pH and produce waste liquid.Also useful molten-salt growth method synthesis Sr titanate powder such as Chinese patent CN103449511A
" a kind of Strontium titanate submicron crystal and preparation method thereof " is first by SrO2With TiO2Mol ratio 1：0.65～1：0.85
9～10.5h is reacted at 650～750 DEG C, thermal response product is then washed with acid solution, the removal of impurity is gone.The patent needs to use acid solution
Process, produce waste liquid, not environmentally.With patent of the present invention comparatively, raw material first is different, this patent is
SrCO3And TiO2, secondly patent of the present invention need not be processed with acid solution, it is to avoid waste liquor contamination environment.
The content of the invention
For the disadvantages described above of prior art, it is an object of the present invention to provide a kind of environmentally friendly, combined coefficient
What high, energy consumption was low efficiently prepares Sr titanate powder method.
Here, the present invention provides a kind of preparation method of Sr titanate powder, the preparation method includes：Step 1) general mole
Mass ratio is 1：1SrCO3And TiO2Mixture be well mixed with fused-salt medium and nonionic surfactant, in 700～
800 DEG C of reaction 4h～12h, are cooled to room temperature, wherein, the SrCO3And TiO2Mixture gross mass and the fused salt
Mass ratio be 1：5～1：10, the SrCO3And TiO2Mixture gross mass and the nonionic surfactant
Mass ratio be 1：3～1：6；Step 2) by step 1) obtained by product at least wash once, 100 DEG C of bakings in an oven
4～8 hours.
In the present invention, adopt SrCO3And TiO2Mixture mix with fused-salt medium and nonionic surfactant
The presoma is reacted titanium at high temperature that can obtain complete crystallization, even particle size distribution as presoma for the even mixture for obtaining
Sour strontium powder.Compared with conventional solid-state method, present example is using fused salt as reaction medium, there is provided liquid phase reactor environment,
Reaction temperature is reduced；Surfactant is used in reaction, it is to avoid the reunion between Sr titanate powder：Using fused salt as
Reaction medium, fused salt are dissolved in deionized water, easily collect Sr titanate powder, and fused salt can repeatedly reclaim use, green
Environmental protection；Sr titanate powder prepared by present example, particle diameter is little to be evenly distributed, purity is high, can produce in enormous quantities.
In the present invention, step 1) described in SrCO3Purity be more than 99.9%, the TiO2Purity 99.5% with
On.
In the present invention, step 1) described in fused salt select potassium fluoride, sodium chloride, potassium chloride, sodium nitrate, potassium nitrate, carbon
At least one in sour sodium, potassium carbonate, sodium sulphate, potassium sulfate.
Also, in the present invention, step 1) described in nonionic surfactant be Nonoxynol.
At 0.1～1 μm, crystal formation is cubic to the Sr titanate powder particle diameter distribution obtained by the preparation method of the present invention.
Description of the drawings
Fig. 1 is that embodiment 1 synthesizes SrTiO3X-ray diffractogram；
Fig. 2 is that embodiment 1 synthesizes SrTiO3SEM scanning electron microscope (SEM) photographs.
Specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following embodiments, it should be appreciated that following embodiments are only used for
The bright present invention, and the unrestricted present invention.
The invention provides a kind of method that employing molten-salt growth method prepares Sr titanate powder.The method is by SrCO3And TiO2After grinding
Fused-salt medium and nonionic surfactant are added, mixture is incubated into 4h～12h in 700～800 DEG C after being sufficiently mixed, will
Reacted mixture Jing multiple times of filtration, washing, fused salt are completely dissolved, are finally dried.The system
Preparation Method reaction temperature is low, process is simple, environmental protection, obtained Sr titanate powder complete crystallization, even particle size distribution.
The method of the present invention includes：By SrCO3With TiO2Mixture carries out heat instead in fused-salt medium at 700～800 DEG C
4～12h is answered, wherein, strontium carbonate and titanium dioxide mol ratio 1：1, SrCO3With TiO2Total mass ratio and fused salt, surface
Activator mass ratio is 1：5：3～1：10：6；By suction filtration after thermal response thing hot wash for several times, baking is then placed on
It is dried in case, obtains SrTiO3Powder.The quality testing of strontium titanates：The XRD analysis of the strontium titanates that molten-salt growth method is obtained；Strontium titanates
The sem analysis of powder.
Chemical reaction according to the present invention is as follows：
SrCO3=SrO+CO2
SrO+TiO2=SrTiO3。
The fused salt selects potassium fluoride, sodium chloride, potassium chloride, sodium nitrate, potassium nitrate, sodium carbonate, potassium carbonate, sulfuric acid
At least one in sodium, potassium sulfate.
There is advantages below as reaction medium using fused salt：Compared with conventional solid-state method, present example is made using fused salt
For reaction medium, there is provided liquid phase reactor environment, reaction temperature are reduced, and fused salt is dissolved in deionized water, easily collect
Sr titanate powder, and fused salt can repeatedly reclaim use, environmental protection.
Also, the nonionic surfactant is Nonoxynol.
Surfactant is used in the present invention, it is to avoid the reunion between Sr titanate powder.
The SrCO3With TiO2Mixture gross mass is 1 with the mass ratio of the fused salt：5～1：10.
Also, the SrCO3With TiO2Mixture quality is 1 with Nonoxynol mass ratio：3～1：6.
The Sr titanate powder crystal formation obtained by the preparation method of the present invention is cubic, and Size Distribution is at 0.1～1 μm.
Sr titanate powder prepared by present example, particle diameter is little to be evenly distributed, purity is high, can produce in enormous quantities.
It is characteristic of the invention that；Compared with conventional solid-state method, present example is using fused salt as reaction medium, there is provided
Liquid phase reactor environment, reaction temperature are reduced；Present example has used surfactant, it is to avoid between Sr titanate powder
Reunite；Fused salt used in present example is dissolved in deionized water, easily collects Sr titanate powder, and fused salt can repeat
Reclaim and use, environmental protection；Sr titanate powder prepared by present example, particle diameter is little to be evenly distributed, purity is high, can be with large quantities of
Amount production.Compared with prior art, the preparation method reaction temperature is low, process is simple, environmental protection, obtained strontium titanates
Powder complete crystallization, even particle size distribution.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Bright to be further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is of the invention
Some nonessential modifications and adaptations that the above is made belong to protection scope of the present invention.The specific technique ginseng of following examples
Number etc. is also only an example in OK range, i.e. those skilled in the art can be done in suitable scope by the explanation of this paper
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Using strontium carbonate and titanium dioxide as initial feed.Wherein the purity of strontium carbonate be 99.9% (mass percent), titanium dioxide
Purity be 99.5% (mass percent).Weigh in the balance and take 1.47g strontium carbonates, 0.79g titanium dioxide, 11.3 sodium chloride and fluorine
Change potassium, the wherein mass ratio of sodium chloride and potassium fluoride is 1：1,6.78g Nonoxynol, with mortar grinder very
Clock.It is subsequently placed in resistance furnace and 4h is reacted at 700 DEG C, subsequently lowers the temperature with stove.It is washed with deionized and suction filtration repeatedly five
It is secondary, until not having white precipitate to produce with silver nitrate detection.Then the product for having washed is dried 4h for 100 DEG C in baking oven.
Embodiment 2
Using strontium carbonate and titanium dioxide as initial feed.Wherein the purity of strontium carbonate be 99.9% (mass percent), titanium dioxide
Purity be 99.5% (mass percent).Weigh in the balance and take 1.47g strontium carbonates, 0.79g titanium dioxide, 13.56g sodium chloride and
The mass ratio of potassium nitrate, wherein sodium chloride and potassium nitrate is 2：1,9.04g Nonoxynol, with mortar grinder ten
Minute.It is subsequently placed in resistance furnace and 6h is reacted at 700 DEG C, subsequently lowers the temperature with stove.It is washed with deionized and suction filtration repeatedly five
It is secondary, until not having white precipitate to produce with silver nitrate detection.Then the product for having washed is dried 4h for 100 DEG C in baking oven.
Embodiment 3
Using strontium carbonate and titanium dioxide as initial feed.Wherein the purity of strontium carbonate be 99.9% (mass percent), titanium dioxide
Purity be 99.5% (mass percent).Weigh in the balance and take 1.47g strontium carbonates, 0.79g titanium dioxide, 15.82g sodium chloride and
The mass ratio of sodium carbonate, wherein sodium chloride and sodium carbonate is 1：2,11.3g Nonoxynols, with mortar grinder ten
Minute.It is subsequently placed in resistance furnace and 6h is reacted at 700 DEG C, subsequently lowers the temperature with stove.It is washed with deionized and suction filtration repeatedly five
It is secondary, until not having white precipitate to produce with silver nitrate detection.Then the product for having washed is dried 4h for 100 DEG C in baking oven.
Embodiment 4
Using strontium carbonate and titanium dioxide as initial feed.Wherein the purity of strontium carbonate be 99.9% (mass percent), titanium dioxide
Purity be 99.5% (mass percent).Weigh in the balance and take 1.47g strontium carbonates, 0.79g titanium dioxide, 18.08 sodium chloride and
The mass ratio of potassium carbonate, wherein sodium chloride and potassium carbonate is 1：3,13.56g Nonoxynols, use mortar grinder
Ten minutes.It is subsequently placed in resistance furnace and 6h is reacted at 700 DEG C, subsequently lowers the temperature with stove.Be washed with deionized and suction filtration repeatedly
Five times, until not having white precipitate to produce with silver nitrate detection.Then the product for having washed is dried 4h for 100 DEG C in baking oven.
Embodiment 5
Using strontium carbonate and titanium dioxide as initial feed.Wherein the purity of strontium carbonate be 99.9% (mass percent), titanium dioxide
Purity be 99.5% (mass percent).Weigh in the balance and take 1.47g strontium carbonates, 0.79g titanium dioxide, 22.6 sodium chloride and sulphur
The mass ratio of sour potassium, wherein sodium chloride and potassium sulfate is 1：1,13.56g Nonoxynol, with mortar grinder ten
Minute.It is subsequently placed in resistance furnace and 6h is reacted at 700 DEG C, subsequently lowers the temperature with stove.It is washed with deionized and suction filtration repeatedly five
It is secondary, until not having white precipitate to produce with silver nitrate detection.Then the product for having washed is dried 4h for 100 DEG C in baking oven.
Embodiment 6
Using strontium carbonate and titanium dioxide as initial feed.Wherein the purity of strontium carbonate be 99.9% (mass percent), titanium dioxide
Purity be 99.5% (mass percent).Weigh in the balance and take 1.47g strontium carbonates, 0.79g titanium dioxide, 22.6 sodium chloride and sulphur
The ratio of sour sodium, wherein sodium chloride and sodium sulphate is 1：1,9.04g Nonoxynol, with mortar grinder very
Clock.It is subsequently placed in resistance furnace and 6h is reacted at 700 DEG C, subsequently lowers the temperature with stove.It is washed with deionized and suction filtration repeatedly five
It is secondary, until not having white precipitate to produce with silver nitrate detection.Then the product for having washed is dried 4h for 100 DEG C in baking oven.
Above the present invention is described in detail, and specific example is applied in text and the present invention is illustrated, this
It is to be understood that for the ease of those skilled in the art and apply the present invention.Those skilled in the art can hold
Change places and various modifications are made to these embodiments, and the thought in the present invention is applied in other embodiment without passing through
Performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art are of the invention to take off
Show, the improvement and modification made for the present invention all should be within protection scope of the present invention.
Industrial applicability：Preparation method reaction temperature of the invention is low, process is simple, environmental protection, the strontium titanates of preparation
Powder, particle diameter is little to be evenly distributed, purity is high, can produce in enormous quantities.
Claims (6)
1. a kind of preparation method of Sr titanate powder, it is characterised in that the preparation method includes：
Step 1）It is 1 by molal weight ratio：1SrCO3And TiO2Mixture be well mixed with fused-salt medium and nonionic surfactant, in 700～800 DEG C react 4～12 hours, be cooled to room temperature, wherein, the SrCO3And TiO2Mixture gross mass and the fused salt mass ratio be 1：5～1：10, the SrCO3And TiO2Mixture gross mass and the nonionic surfactant mass ratio be 1：3～1：6；
Step 2）By step 1）The product washing drying of gained, obtains Sr titanate powder.
2. preparation method according to claim 1, it is characterised in that step 1）Described in SrCO3Purity be more than 99.9%, the TiO2Purity be more than 99.5%.
3. the preparation method according to any one of claim 1 or 2, it is characterised in that step 1）Described in fused salt from potassium fluoride, sodium chloride, potassium chloride, sodium nitrate, potassium nitrate, sodium carbonate, potassium carbonate, sodium sulphate, at least one in potassium sulfate.
4. the preparation method according to any one of claims 1 to 3, it is characterised in that step 1）Described in nonionic surfactant be Nonoxynol.
5. the preparation method according to any one of Claims 1 to 4, it is characterised in that step 2）In, by step 1）The product of gained is at least washed once, and 100 DEG C are dried 4～8 hours in an oven.
6. the preparation method according to any one of Claims 1 to 5, it is characterised in that the Sr titanate powder particle diameter distribution is at 0.1～1 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108620053A (en) * | 2017-07-17 | 2018-10-09 | 中国地质大学（北京） | A kind of method that molten-salt growth method prepares meta-titanium perborate-potassium tetratitanate composite catalyzing material |
| CN109928422A (en) * | 2018-08-14 | 2019-06-25 | 华北理工大学 | A kind of method that fused salt prepares potassium titanate crystal |
| CN112062567A (en) * | 2020-09-17 | 2020-12-11 | 中国科学院上海应用物理研究所 | Method for preparing zirconium-yttrium-doped barium cerate powder by using molten salt and powder obtained by method |
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| CN101423979A (en) * | 2008-09-02 | 2009-05-06 | 昆明健为建筑装饰工程有限公司 | Nanocrystal for two-phase coexistent of barium titanate and ferrate and preparation method thereof |
| CN103449511A (en) * | 2013-04-09 | 2013-12-18 | 深圳信息职业技术学院 | Strontium titanate submicron crystal and preparation method thereof |
| CN104628379A (en) * | 2013-11-06 | 2015-05-20 | 同济大学 | Highly-oriented lead-free piezoelectric textured ceramic material and preparation method and application thereof |
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| CN1931787A (en) * | 2006-09-29 | 2007-03-21 | 武汉理工大学 | Microwave molten salt process for synthesizing plate Sr3Ti2O7 crystal |
| CN1958885A (en) * | 2006-09-29 | 2007-05-09 | 武汉理工大学 | Microwave molten salt growth method for synthesizing sheet crystal SrTi03 |
| CN101423979A (en) * | 2008-09-02 | 2009-05-06 | 昆明健为建筑装饰工程有限公司 | Nanocrystal for two-phase coexistent of barium titanate and ferrate and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108620053A (en) * | 2017-07-17 | 2018-10-09 | 中国地质大学（北京） | A kind of method that molten-salt growth method prepares meta-titanium perborate-potassium tetratitanate composite catalyzing material |
| CN108620053B (en) * | 2017-07-17 | 2020-10-09 | 中国地质大学（北京） | Method for preparing sodium metatitanate-potassium tetratitanate composite catalytic material by molten salt method |
| CN109928422A (en) * | 2018-08-14 | 2019-06-25 | 华北理工大学 | A kind of method that fused salt prepares potassium titanate crystal |
| CN112062567A (en) * | 2020-09-17 | 2020-12-11 | 中国科学院上海应用物理研究所 | Method for preparing zirconium-yttrium-doped barium cerate powder by using molten salt and powder obtained by method |
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