CN104085922B - A kind of preparation method of high-purity Emission in Cubic sodium niobate nanometer powder - Google Patents
A kind of preparation method of high-purity Emission in Cubic sodium niobate nanometer powder Download PDFInfo
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- CN104085922B CN104085922B CN201410333060.5A CN201410333060A CN104085922B CN 104085922 B CN104085922 B CN 104085922B CN 201410333060 A CN201410333060 A CN 201410333060A CN 104085922 B CN104085922 B CN 104085922B
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Abstract
The invention discloses a kind of preparation method of high-purity Emission in Cubic sodium niobate nanometer powder, its step: (1) by niobium oxalate or ammonium niobium oxalate and sodium-chlor, according to molar ratio ingredient, be dissolved in dried up in; (2) grind in agate mortar, and drip dehydrated alcohol in process of lapping; (3) presoma obtained is dried in vacuum drying oven; (4) heated up in energy-conservation cabinet-type electric furnace by the precursor powder after oven dry, insulation, then naturally cools to room temperature; (5) by the mixing solutions centrifuge washing of the powder deionized water that obtains and dehydrated alcohol; (6) powder of gained is put into vacuum drying oven dry, namely obtain Emission in Cubic sodium niobate nanometer powder.The invention solves the difficulty that Emission in Cubic sodium columbate is difficult to prepare, the preparation technology adopted consuming time short, energy consumption is low, and being applicable to scale operation, prepared Emission in Cubic sodium niobate nanometer powder has high adsorption capacity, visible light-responded sensitive and photocatalysis efficiency advantages of higher.
Description
Technical field
The invention belongs to the inorganic nanometer functional material preparation of nano-powder (in the Materials science) technical field, relate to the sodium niobate nanometer powder that can be used for the fields such as device for non-linear optical, photochemical catalysis and solar cell, the specifically preparation method of the well-developed Emission in Cubic sodium niobate nanometer powder of a kind of high-purity crystal formation.
Background technology
Sodium columbate is a kind of low toxicity and has the perovskite structural material of high stability, owing to having good nonlinear optical response, piezoelectric property and photorefractive property, in the prospect that the fields such as nonlinear optics, photoelectronics and photochemical catalysis have a wide range of applications.There is multiple crystalline phase in sodium columbate crystal, mainly contains orthorhombic phase, Tetragonal, Emission in Cubic and water chestnut side's phase, and this several crystalline phase can undergo phase transition in certain temperature, and under room temperature, orthorhombic phase is the most stable.In recent years, the sodium columbate of orthorhombic phase has been widely used in photochemical catalysis research field due to good photochemical catalysis performance.Crystal theoretical is thought relative to orthorhombic phase sodium columbate, and Emission in Cubic sodium columbate has higher crystal symmetry and relative narrow optical band gap.Emission in Cubic has higher photocatalytic activity than the sodium columbate of orthorhombic phase to have report experimentally to prove in the recent period.At present, the preparation method of sodium columbate has a variety of, such as, and hydrothermal method, Via Polymeric Precursor Method, template and molten-salt growth method etc.But mostly the sodium columbate that aforesaid method is prepared is orthorhombic phase, rarely has the relevant report about high-purity Emission in Cubic sodium columbate preparation method.2012, the people such as LiPeng adopt a kind of typical sugar alcohol derivation polymerization oxidation method to synthesize the sodium niobate powder of Emission in Cubic, but the presoma in the method has to pass through the thermal treatment reaching 120 hours, and further under 600 degrees celsius oxidation within 5 hours, just can obtain sodium niobate powder.[see: PengLi, ShuxinOuyang, GuangchengXietal., TheEffectsofCrystalStructureandElectronicStructureonPhot ocatalyticH
2evolutionandCO
2reductionoverTwoPhasesofPerovskite-StructuredNaNbO
3j.Phys.Chem.C2012,116 (14): 7621 ~ 7628.] preparation process of above-mentioned Emission in Cubic sodium niobate nano structure is complicated and cost is higher, be unfavorable for scale operation, be also unfavorable for its application in fields such as photocatalyst, dye sensitization solar battery and gas sensors.Therefore, the present invention proposes a kind of simple general-purpose and the method for the controlled preparation high-purity Emission in Cubic sodium niobate nano structure of size.
Summary of the invention
For above-mentioned Problems existing, the object of this invention is to provide a kind of preparation method of high-purity Emission in Cubic sodium niobate nanometer powder.The method essential characteristic is that equipment is simple, easy and simple to handle, and economical, is applicable to large-scale production.The Emission in Cubic sodium niobate nanometer powder of preparation, not only thing phase purity is high, and narrow diameter distribution, has good thermostability and chemical stability.The Emission in Cubic sodium niobate nanometer powder that significantly prepared by this method has high adsorption capacity, visible light-responded sensitive and photocatalysis efficiency advantages of higher.
A preparation method for high-purity Emission in Cubic sodium niobate nanometer powder, the steps include:
(1) by niobium oxalate or ammonium niobium oxalate and sodium-chlor, be 0.06 ~ 0.25 batching according to mol ratio, be dissolved in 1 ~ 10 ml deionized water;
(2) grind 30 ~ 50 minutes in agate mortar, in process of lapping, drip 1 ~ 15 milliliter of dehydrated alcohol;
(3) presoma step (2) obtained is-50 ~-100 kPas in vacuum tightness in vacuum drying oven, and temperature is dry under 60 ~ 90 degrees celsius;
(4) precursor powder after oven dry is warming up to 300 ~ 500 degree celsius temperature in energy-conservation cabinet-type electric furnace, is incubated 2 ~ 5 hours, then naturally cools to 20 ~ 25 degrees Celsius;
(5) by the mixing solutions centrifuge washing 3 ~ 5 times of the powder deionized water that obtains in step (4) and dehydrated alcohol, the volume ratio of deionized water and dehydrated alcohol is 1:1 ~ 1:5, centrifugal speed is 6000 ~ 8000 revs/min, and centrifugation time is 4 ~ 7 minutes;
(6) powder of step (5) gained is put into vacuum drying oven, it is-50 ~-100 kPas in vacuum tightness, temperature is under the condition of 70 ~ 90 degrees Celsius dry 2 ~ 6 hours, obtains the high-purity and well-developed Emission in Cubic sodium niobate nanometer powder of crystal formation.
(7) thing phase, the crystalline structure of the powder using X-ray diffractometer detecting step (6) to obtain;
(8) transmission electron microscope is used to come pattern and the size of the powder that detecting step (6) obtains;
(9) ultraviolet-visible pectrophotometer is used to carry out the uv-visible absorption spectra of the powder that detecting step (6) obtains.
The present invention compared with prior art, has the following advantages and effect:
The present invention adopts low-temperature in-site solid phase method, using niobium oxalate or ammonium niobium oxalate and sodium-chlor as niobium source and sodium source, through grinding, low-temperature heat treatment and centrifuge washing and drying treatment, obtains the well-developed Emission in Cubic sodium niobate nanometer powder of crystal formation.The invention provides a kind of effective ways preparing Emission in Cubic sodium columbate, compared with traditional method, starting material used are stable, toxicity is low and economical, preparation technology consuming time short, energy consumption is low, and is applicable to scale operation.The Emission in Cubic sodium niobate nanometer powder prepared by the method has high adsorption capacity, visible light-responded sensitive and photocatalysis efficiency advantages of higher, for it to provide the necessary technical support in the large-scale application in the fields such as device for non-linear optical, photochemical catalysis and solar cell.
Accompanying drawing explanation
Fig. 1 is a kind of X ray diffracting spectrum of sodium niobate nanometer powder of the embodiment of the present invention 1;
Fig. 2 is a kind of transmission electron microscope photo of sodium niobate nanometer powder of the embodiment of the present invention 1;
Fig. 3 is a kind of uv-visible absorption spectra of sodium niobate nanometer powder of the embodiment of the present invention 3;
Fig. 4 is that a kind of sodium niobate nanometer powder of the embodiment of the present invention 2 is to the degradation efficiency of methylene blue dye.
Embodiment
Embodiment 1:
A preparation method for high-purity Emission in Cubic sodium niobate nanometer powder, the steps include:
(1) by niobium oxalate and sodium-chlor, according to mol ratio be 0.06 or 0.11 or 0.13 or 0.15 or 0.18 or 0.20 or 0.24 or 0.25 batching, be dissolved in 3 or 4 or 6 or 7 milliliters go dried up in;
(2) grind 30 or 35 or 40 or 45 or 50 minutes in agate mortar, in process of lapping, drip 5 or 6 or 7 or 8 or 10 milliliters of dehydrated alcohols;
(3) presoma step (2) obtained is in vacuum drying oven, and be-50 or-60 or-70 or-80 or-90 or-100 kPas in vacuum tightness, temperature is dry under 60 or 65 or 70 or 76 or 80 or 85 or 90 degrees celsius;
(4) precursor powder after oven dry is warming up to 350 or 380 or 400 or 420 or 430 or 450 or 480 or 500 degree celsius temperature in energy-conservation cabinet-type electric furnace, is incubated 2 or 3 or 4 or 5 hours, then naturally cools to 20 or 22 or 24 or 25 degrees Celsius;
(5) by the mixing solutions centrifuge washing 3 of the powder deionized water that obtains in step (4) and dehydrated alcohol or 4 or 5 times, the volume ratio of deionized water and dehydrated alcohol is 1:1, centrifugal speed is 8000 revs/min, and centrifugation time is 4 or 5 or 6 or 7 minutes;
(6) powder of step (5) gained is put into vacuum drying oven, be-50 or-65 or-75 or-85 or-95 or-100 kPas in vacuum tightness, temperature is under the condition of 70 or 74 or 78 or 83 or 87 or 90 degrees Celsius dry 3 or 4 or 5 or 6 hours, just obtains the well-developed Emission in Cubic sodium niobate nanometer powder of crystal formation.
(7) thing phase, the crystalline structure of the powder using X-ray diffractometer detecting step (6) to obtain;
(8) transmission electron microscope is used to come pattern and the size of the powder that detecting step (6) obtains;
(9) ultraviolet-visible pectrophotometer is used to carry out the uv-visible absorption spectra of the powder that detecting step (6) obtains.
It is simple that the inventive method has technology and equipment, easy to implement the method, easy to operate and safe, the features such as product preparation cost is low, is applicable to large-scale production.And the Emission in Cubic sodium niobate nanometer powder of preparation, thing phase purity is high, crystal development is complete, narrow diameter distribution, has good thermostability and chemical stability, importantly high adsorption capacity and have sensitiveer response to visible ray.
Embodiment 2:
A preparation method for high-purity Emission in Cubic sodium niobate nanometer powder, the steps include:
(1) by niobium oxalate and sodium-chlor, be 0.08 batching according to mol ratio, be dissolved in 2 or 3 or 4 milliliters go dried up in;
(2) grind 38 minutes in agate mortar, in process of lapping, drip 3 or 5 or 9 milliliters of dehydrated alcohols;
(3) presoma step (2) obtained is in vacuum drying oven, and be-50 or-55 or-62 or-68 or-74 or-78 or-86 or-92 or-100 kPas in vacuum tightness, temperature is dry under 60 or 66 or 72 or 78 or 84 or 90 degrees celsius;
(4) precursor powder after oven dry is warming up to 410 degree celsius temperature in energy-conservation cabinet-type electric furnace, is incubated 2 hours, then naturally cools to 20 ~ 25 degrees Celsius;
(5) by the mixing solutions centrifuge washing 3 times of the powder deionized water that obtains in step (4) and dehydrated alcohol, the volume ratio of deionized water and dehydrated alcohol is 1:2, and centrifugal speed is 8000 revs/min, and centrifugation time is 5 minutes;
(6) powder of step (5) gained is put into vacuum drying oven, be-50 or-58 or-66 or-64 or-72 or-77 or-84 or-88 or-96 or-100 kPas in vacuum tightness, temperature is under the condition of 80 degrees Celsius dry 5 hours, just obtains the well-developed Emission in Cubic sodium niobate nanometer powder of crystal formation.
(7) thing phase, the crystalline structure of the powder using X-ray diffractometer detecting step (6) to obtain;
(8) transmission electron microscope is used to come pattern and the size of the powder that detecting step (6) obtains;
(9) ultraviolet-visible pectrophotometer is used to carry out the uv-visible absorption spectra of the powder that detecting step (6) obtains.
Embodiment 3:
A preparation method for high-purity Emission in Cubic sodium niobate nanometer powder, the steps include:
(1) by niobium oxalate and sodium-chlor, be 0.07 batching according to mol ratio, be dissolved in 3 or 4 or 5 milliliters go dried up in;
(2) grind 36 minutes in agate mortar, in process of lapping, drip 4 or 5 or 7 milliliters of dehydrated alcohols;
(3) presoma step (2) obtained is in vacuum drying oven, and be-50 or-61 or-71 or-81 or-90 or-100 kPas in vacuum tightness, temperature is dry under the condition of 60 or 68 or 76 or 85 or 90 degrees Celsius;
(4) precursor powder after oven dry is warming up to 440 degree celsius temperature in energy-conservation cabinet-type electric furnace, is incubated 2 hours, then naturally cools to 20 ~ 25 degrees Celsius;
(5) by the mixing solutions centrifuge washing 3 times of the powder deionized water that obtains in step (4) and dehydrated alcohol, the volume ratio of deionized water and dehydrated alcohol is 1:3, and centrifugal speed is 7000 revs/min, and centrifugation time is 7 minutes;
(6) powder of step (5) gained is put into vacuum drying oven, be-50 or-60 or-66 or-79 or-87 or-94 or-100 kPas in vacuum tightness, temperature is under 70 degrees celsius dry 5 hours, just obtains the well-developed Emission in Cubic sodium niobate nanometer powder of crystal formation.
(7) thing phase, the crystalline structure of the powder using X-ray diffractometer detecting step (6) to obtain;
(8) transmission electron microscope is used to come pattern and the size of the powder that detecting step (6) obtains;
(9) ultraviolet-visible pectrophotometer is used to carry out the uv-visible absorption spectra of the powder that detecting step (6) obtains.
Embodiment 4:
A preparation method for high-purity Emission in Cubic sodium niobate nanometer powder, the steps include:
(1) by ammonium niobium oxalate and sodium-chlor, according to mol ratio be 0.07 or 0.09 or 0.10 or 0.12 or 0.14 or 0.16 or 0.19 or 0.20 or 0.22 or 0.23 batching, be dissolved in 2 or 3 or 4 or 5 or 6 or 7 milliliters go dried up in;
(2) grind 30 or 33 or 38 or 42 or 43 or 45 or 47 or 49 minutes in agate mortar, in process of lapping, drip 3 or 4 or 6 or 7 or 8 or 9 or 11 or 12 or 14 milliliters of dehydrated alcohols;
(3) presoma step (2) obtained is in vacuum drying oven, be-55 or-60 or-65 or-68 or-70 or-78 or-82 or-85 or-90 or-95 or-100 kPas in vacuum tightness, temperature is dry under 60 or 63 or 72 or 77 or 82 or 85 or 88 or 90 degrees celsius;
(4) precursor powder after oven dry is warming up to 380 or 400 or 420 or 430 or 450 or 480 or 500 degree celsius temperature in energy-conservation cabinet-type electric furnace, is incubated 2 or 3 or 4 or 5 hours, then naturally cools to 20 or 22 or 24 or 25 degrees Celsius;
(5) by the mixing solutions centrifuge washing 3 of the powder deionized water that obtains in step (4) and dehydrated alcohol or 4 or 5 times, the volume ratio of deionized water and dehydrated alcohol is 1:1 or 1:2, centrifugal speed is 7000 or 8000 revs/min, and centrifugation time is 4 or 5 or 6 or 7 minutes;
(6) powder of step (5) gained is put into vacuum drying oven, be-55 or-63 or-70 or-76 or-82 or-88 or-95 or-100 kPas in vacuum tightness, temperature is under the condition of 60 or 63 or 65 or 70 or 73 or 75 or 78 or 80 degrees Celsius dry 3 or 4 or 5 or 6 hours, just obtains the well-developed Emission in Cubic sodium niobate nanometer powder of crystal formation.
(7) thing phase, the crystalline structure of the powder using X-ray diffractometer detecting step (6) to obtain;
(8) transmission electron microscope is used to come pattern and the size of the powder that detecting step (6) obtains;
(9) ultraviolet-visible pectrophotometer is used to carry out the uv-visible absorption spectra of the powder that detecting step (6) obtains.
Claims (1)
1. a preparation method for high-purity Emission in Cubic sodium niobate nanometer powder, the steps include:
(1) by niobium oxalate or ammonium niobium oxalate and sodium-chlor, be 0.06 ~ 0.25 batching according to mol ratio, be dissolved in 1 ~ 10 milliliter go dried up in;
(2) grind 30 ~ 50 minutes in agate mortar, in process of lapping, drip 1 ~ 15 milliliter of dehydrated alcohol;
(3) presoma step (2) obtained, at vacuum drying oven, is-50 ~-100 kPas in vacuum tightness, and temperature is dry under the condition of 60 ~ 90 degrees Celsius;
(4) precursor powder after oven dry is warming up to 300 ~ 500 degrees Celsius in energy-conservation cabinet-type electric furnace, is incubated 2 ~ 5 hours, then naturally cools to 20 ~ 25 degrees Celsius;
(5) by the mixing solutions centrifuge washing 3 ~ 5 times of the powder deionized water that obtains in step (4) and dehydrated alcohol, the volume ratio of deionized water and dehydrated alcohol is 1:1 ~ 1:5, centrifugal speed is 6000 ~ 8000 revs/min, and centrifugation time is 4 ~ 7 minutes;
(6) powder of step (5) gained is put into vacuum drying oven, it is-50 ~-100 kPas in vacuum tightness, temperature is under the condition of 70 ~ 90 degrees Celsius dry 2 ~ 6 hours, obtains the high-purity and well-developed Emission in Cubic sodium niobate nanometer powder of crystal formation.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101327957A (en) * | 2008-07-29 | 2008-12-24 | 陕西科技大学 | Method for preparing NaNbO3 superfine power under low temperature |
| CN102030531A (en) * | 2010-12-31 | 2011-04-27 | 中国科学院上海硅酸盐研究所 | Method for preparing potassium sodium niobate nano powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101327957A (en) * | 2008-07-29 | 2008-12-24 | 陕西科技大学 | Method for preparing NaNbO3 superfine power under low temperature |
| CN102030531A (en) * | 2010-12-31 | 2011-04-27 | 中国科学院上海硅酸盐研究所 | Method for preparing potassium sodium niobate nano powder |
Non-Patent Citations (2)
| Title |
|---|
| "柠檬酸钠与草酸铌合成NaNbO3粉体的反应机理";卞玉波等;《化学工程师》;20111231(第3期);第56-58页 * |
| "铌酸钠粉体的低温合成及其结构表征";卞玉波等;《无机盐工业》;20101130;第42卷(第11期);第36-38页 * |
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