CN100429151C - Lanthanum stannate, europium stannate and its composite stannate nanopowder synthesis method - Google Patents
Lanthanum stannate, europium stannate and its composite stannate nanopowder synthesis method Download PDFInfo
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- CN100429151C CN100429151C CNB2006101546367A CN200610154636A CN100429151C CN 100429151 C CN100429151 C CN 100429151C CN B2006101546367 A CNB2006101546367 A CN B2006101546367A CN 200610154636 A CN200610154636 A CN 200610154636A CN 100429151 C CN100429151 C CN 100429151C
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- stannate
- europium
- lanthanum
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Abstract
The invention discloses a synthesizing method of lanthanum stannate, europium stannate and composite stannate nanometer powder, which comprises the following steps: dissolving lanthanum stannate and europium stannate with different molar rates or lanthanum stannate or europium stannate in the deionized water; stirring; adding sodium stannate or potassium stannate with the molar weight as the sum of lanthanum stannate and europium stannate in the solution; stirring; putting terminal solution into high-pressure autoclave; setting the filling density at 80-90%; disposing for 4-30h within 180-250 deg.c through hot water; centrifuging the disposed solution; cleaning; drying the product; obtaining the product with diameter at 15-35nm. The molecular formula of the product is La2-xEuxSn2O7 (x=02), which produces single and one-phase product.
Description
Technical field
The present invention relates to the synthetic method of a kind of stannic acid lanthanum, stannic acid europium or compound stannate nano powder.
Background technology
The pyrochlore-type oxide compound is that a series of molecular formula are A
2B
2O
7Oxygenatedchemicals, wherein A is divalence or Tricationic, B is tetravalence or pentavalent positively charged ion.Because this compounds has excellent heat, electricity, magnetic and catalytic performance, is subjected to people and pays close attention to especially always.Rare earth stannate is the important pyrochlore-type oxide compound of a class, and molecular formula is RE
2Sn
2O
7(RE=Y, La-Lu).In recent years studies show that rare earth stannate all has potential to use in fields such as lithium cell, catalysis, photoluminescence, ionophore and radioprotectives.Because the fusing point very high (＞2000 ℃) of rare earth stannate, they can be used as high temperature catalyst, and the application of uniqueness is arranged aspect control in the processing of vehicle exhaust.Simultaneously, europium is important luminescent activator, and europium ion activated luminescent material all has important use in fields such as luminescent lamp, Field Emission Display and plasma demonstrations.There is more functional alternative position in the lattice of pyrochlore constitution, substitutes the position at these and introduce other ion, will cause the change of performances such as material heat, light, electricity and catalysis.Therefore, the compound stannate nano powder of synthetic pyrochlore-type lanthanum europium of the present invention will be a kind of functional materials with potential application.
Preparation method's more complicated of traditional pyrochlore-type rare earth stannate, and reaction conditions is relatively harsher, generally needs tindioxide and corresponding rare earth oxide to carry out long solid state reaction at the high temperature more than 1400 ℃.By contrast, hydrothermal method has equipment and simple to operate, product advantages of good crystallization, environmental pollution is little and characteristics such as suitable scale operation, and advantage such as hydro-thermal synthetic powder has that purity height, degree of crystallinity height, particle diameter are little, narrow size distribution and stoichiometric ratio are good.Therefore, hydrothermal method is a synthesizing rare-earth stannate perfect method.People such as Moon have reported employing SnCl
4Be the synthetic stannic acid lanthanum (La of tin source hydro-thermal
2Sn
2O
7) method (J.Moon et al.J.Am.Ceram.Soc., 84,2531 (2001)), have not yet to see open report about the synthetic compound stannate nano powder of pyrochlore-type lanthanum europium of hydro-thermal.
Summary of the invention
The object of the present invention is to provide the synthetic method of a kind of stannic acid lanthanum, stannic acid europium or compound stannate nano powder, utilize rare earth stannate to have same crystal structure (pyrochlore constitution), characteristics that lattice parameter is close, adopt hydrothermal method, synthesized homogeneous, single-phase, any adjustable stannic acid lanthanum, stannic acid europium and the compound stannate nano powder thereof of lanthanum europium ratio.
The technical solution used in the present invention is that the step of this method is as follows:
1) lanthanum nitrate and the europium nitrate with different mol ratio is dissolved in the deionized water, and perhaps lanthanum nitrate or europium nitrate are dissolved in the deionized water, and the total mol concentration of control solution middle-weight rare earths nitrate is 0.01～0.2 mol, stirs;
2) adding mole number again in above-mentioned solution is the sodium stannate or the potassium stannate of lanthanum nitrate and europium nitrate mole number sum, stirs;
3) solution that will finally prepare is put into autoclave, and compactedness is 80～90%, and this autoclave was handled 4～30 hours in 180～250 ℃ of temperature ranges;
4), pyrochlore-type stannic acid lanthanum, stannic acid europium or compound stannate nano powder have just been obtained with solution centrifugal, the cleaning handled well, and the product drying.
Described powder homogeneous, single-phase, and lanthanum europium ratio is adjustable arbitrarily, and molecular formula is written as La
2-xEu
xSn
2O
7, x=0～2, powder is of a size of 15～35 nanometers.
The beneficial effect that the present invention has is: with lanthanum nitrate, europium nitrate, sodium stannate and potassium stannate as raw material, adopt hydro-thermal synthesis process, ratio by lanthanum nitrate lanthanum and europium nitrate in the conditioned reaction thing, realized pyrochlore-type stannic acid lanthanum, stannic acid europium and compound stannate nano powder thereof synthetic of homogeneous, single-phase, any lanthanum europium ratio, the product molecular formula can be written as La
2-xEu
xSn
2O
7(x=0～2), diameter of particle are 15～35 nanometers.
Description of drawings
Fig. 1 embodiment 1～5 products therefrom La
2-xEu
xSn
2O
7The XRD figure spectrum of (x=0,0.5,1,1.5,2): (a) embodiment 1 (x=0), (b) embodiment 2 (x=0.5), (c) embodiment 3 (x=1), (d) embodiment 4 (x=1.5), (e) embodiment 5 (x=2);
Fig. 2 is embodiment 1 gained nano-powder (La
2-xEu
xSn
2O
7(x=0)) transmission electron microscope photo;
Fig. 3 is embodiment 2 gained nano-powder (La
2-xEu
xSn
2O
7(x=0.5)) transmission electron microscope photo;
Fig. 4 is embodiment 3 gained nano-powder (La
2-xEu
xSn
2O
7(x=1)) transmission electron microscope photo;
Fig. 5 is embodiment 4 gained nano-powder (La
2-xEu
xSn
2O
7(x=1.5)) transmission electron microscope photo;
Fig. 6 is embodiment 5 gained nano-powder (La
2-xEu
xSn
2O
7(x=2)) transmission electron microscope photo.
Embodiment
Embodiment 1:
Synthetic La
2-xEu
xSn
2O
7(x=0), i.e. La
2Sn
2O
7With 0.692 gram lanthanum nitrate (La (NO
3)
36H
2O) be dissolved in 160 ml deionized water, the lanthanum nitrate volumetric molar concentration is 0.01 mol, stirs after 3 minutes, adds 0.478 gram potassium stannate (K again in above-mentioned solution
2SnO
33H
2O), the potassium stannate volumetric molar concentration is 0.01 mol, continues to stir after 5 minutes, obtains final solution, and this solution rare earth nitrate total mol concentration is 0.01 mol, does not contain europium nitrate, i.e. x=0.The above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, and the liner volume is 200 milliliters, and the control compactedness is 80%.This solution was handled 30 hours down at 180 ℃, the solution centrifugal of handling well, cleaning, and with the product drying, had obtained nano-powder.The XRD figure spectrum of this product is seen Fig. 1 (a), this collection of illustrative plates and stannic acid lanthanum (La
2Sn
2O
7) XRD standard card (JCPDS no.13-0082) fit like a glove, illustrate that product is La
2Sn
2O
7Fig. 2 is the transmission electron microscope photo of this product, can find out that therefrom product is a nanometer rod, about 15 nanometers of diameter.
Embodiment 2:
Synthetic La
2-xEu
xSn
2O
7(x=0.5), i.e. La
1.5Eu
0.5Sn
2O
7With 2.078 gram lanthanum nitrate (La (NO
3)
36H
2O) be dissolved in 160 ml deionized water, the lanthanum nitrate volumetric molar concentration is 0.03 mol, stirs after 3 minutes, adds 0.714 gram europium nitrate (Eu (NO again
3)
36H
2O), the volumetric molar concentration of europium nitrate is 0.01 mol, stirs after 3 minutes, adds 1.709 gram sodium stannate (Na again in above-mentioned solution
2SnO
33H
2O), the volumetric molar concentration of sodium stannate is 0.04 mol, continues to stir after 5 minutes, obtains final solution, and this solution middle-weight rare earths nitrate total mol concentration is 0.04 mol, and lanthanum europium ratio is 3: 1, i.e. x=0.5.The above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, and the liner volume is 200 milliliters, and the control compactedness is 90%.This solution was handled 20 hours down at 200 ℃, and the solution centrifugal of handling well, cleaning, and with the product drying, acquisition lanthanum europium ratio is 3: 1 the compound stannate nano powder of pyrochlore-type lanthanum europium, i.e. La
2-xEu
xSn
2O
7(x=0.5).Fig. 1 (b) is the XRD figure spectrum of this nano-powder, this collection of illustrative plates and La
2Sn
2O
7XRD figure spectrum similar, just the XRD peak position has small skew than Fig. 1 (a), this has caused that the lattice parameter variation causes because the part europium ion replaces lanthanum ion.This shows that this product is a kind of typical single-phase pyrochlore-type compound, i.e. La
1.5Eu
0.5Sn
2O
7Fig. 3 is the transmission electron microscope photo of this product, and this product is a nano particle as seen from Figure 3, about 20 nanometers of particle diameter.
Embodiment 3:
Synthetic La
2-xEu
xSn
2O
7(x=1), i.e. LaEuSn
2O
7With 6.928 gram lanthanum nitrate (La (NO
3)
36H
2O) be dissolved in 160 ml deionized water, the lanthanum nitrate volumetric molar concentration is 0.1 mol, stirs after 3 minutes, adds 7.136 gram europium nitrate (Eu (NO again
3)
36H
2O), the europium nitrate volumetric molar concentration is 0.1 mol, stirs after 3 minutes, adds 9.568 gram potassium stannate (K again in above-mentioned solution
2SnO
33H
2O), potassium stannate volumetric molar concentration 0.2 mol continues to stir after 5 minutes, obtains final solution, and this solution middle-weight rare earths nitrate total mol concentration is 0.2 mol, and lanthanum europium ratio is 1: 1, i.e. x=1.The above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, and the liner volume is 200 milliliters, and the control compactedness is 80%.This solution was handled 24 hours down at 200 ℃, and the solution centrifugal of handling well, cleaning, and with the product drying, acquisition lanthanum europium ratio is 1: 1 the compound stannate nano powder La of pyrochlore-type lanthanum europium
2-xEu
xSn
2O
7(x=1).Fig. 1 (c) is the XRD figure spectrum of this product, this collection of illustrative plates and La
2Sn
2O
7XRD figure spectrum similar, just the XRD peak position has small skew than Fig. 1 (a), this has caused that the lattice parameter variation causes because the part europium ion replaces lanthanum ion.This shows that this product is a kind of typical single-phase pyrochlore-type compound, i.e. LaEuSn
2O
7Fig. 4 is the transmission electron microscope photo of this product, and product is a nano particle as seen from Figure 4, about 35 nanometers of particle diameter.
Embodiment 4:
Synthetic La
2-xEu
xSn
2O
7(x=1.5), i.e. La
0.5Eu
1.5Sn
2O
7With 1.386 gram lanthanum nitrate (La (NO
3)
36H
2O) be dissolved in 160 ml deionized water, the lanthanum nitrate volumetric molar concentration is 0.02 mol, stirs after 3 minutes, adds 4.281 gram europium nitrate (Eu (NO again
3)
36H
2O), the europium nitrate volumetric molar concentration is 0.06 mol, stirs after 3 minutes, adds 3.418 gram sodium stannate (Na again in above-mentioned solution
2SnO
33H
2O), sodium stannate volumetric molar concentration 0.08 mol continues to stir after 5 minutes, obtains final solution, and this solution middle-weight rare earths nitrate total mol concentration is 0.08 mol, and lanthanum europium ratio is 1: 3, i.e. x=1.5.The above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, and the liner volume is 200 milliliters.This solution was handled 10 hours down at 200 ℃, and the solution centrifugal of handling well, cleaning, and with the product drying, acquisition lanthanum europium ratio is 1: 3 the compound stannate nano powder La of pyrochlore-type lanthanum europium
2-xEu
xSn
2O
7(x=1.5).Fig. 1 (d) is the XRD figure spectrum of this nano-powder, this collection of illustrative plates and La
2Sn
2O
7XRD figure spectrum similar, just the XRD peak position has small skew than Fig. 1 (a), this has caused that the lattice parameter variation causes because the part europium ion replaces lanthanum ion.This shows that this product is a kind of typical single-phase pyrochlore-type compound, i.e. La
0.5Eu
1.5Sn
2O
7Fig. 5 is the transmission electron microscope photo of this product, and product is a nano particle as seen from Figure 5, about 20 nanometers of particle diameter.
Embodiment 5:
Synthetic La
2-xEu
xSn
2O
7(x=2), i.e. Eu
2Sn
2O
7With 2.771 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 160 ml deionized water, the europium nitrate volumetric molar concentration is 0.04 mol, stirs after 3 minutes, adds 1.709 gram sodium stannate (Na again in above-mentioned solution
2SnO
33H
2O), the sodium stannate volumetric molar concentration is 0.04 mol, continues to stir after 5 minutes, obtains final solution, and this solution middle-weight rare earths nitrate total mol concentration is 0.04 mol, and does not contain lanthanum nitrate, i.e. x=2.The above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, and the liner volume is 200 milliliters, and the control compactedness is 80%.This solution was handled 4 hours down at 250 ℃, the solution centrifugal of handling well, cleaning, and with the product drying, just obtained stannic acid europium (Eu
2Sn
2O
7) nano-powder.Fig. 1 (e) is the XRD figure spectrum of product, and the standard x RD card of this collection of illustrative plates and stannic acid europium (JCPPDS no.13-0182) fits like a glove, and illustrates that product is stannic acid lanthanum (Eu
2Sn
2O
7).Fig. 6 is the transmission electron microscope photo of product, can find out that therefrom product is a nano particle, about 20 nanometers of particle diameter.
Claims (2)
1, the synthetic method of a kind of stannic acid lanthanum, stannic acid europium or compound stannate nano powder is characterized in that the step of this method is as follows:
1) lanthanum nitrate and the europium nitrate with different mol ratio is dissolved in the deionized water, and perhaps lanthanum nitrate or europium nitrate are dissolved in the deionized water, and the total mol concentration of control solution middle-weight rare earths nitrate is 0.01～0.2 mol, stirs;
2) adding mole number again in above-mentioned solution is the sodium stannate or the potassium stannate of lanthanum nitrate and europium nitrate mole number sum, stirs;
3) solution that will finally prepare is put into autoclave, and compactedness is 80～90%, and this autoclave was handled 4～30 hours in 180～250 ℃ of temperature ranges;
4), pyrochlore-type stannic acid lanthanum, stannic acid europium or compound stannate nano powder have just been obtained with solution centrifugal, the cleaning handled well, and the product drying.
2, the synthetic method of a kind of stannic acid lanthanum according to claim 1, stannic acid europium or compound stannate nano powder is characterized in that: described powder homogeneous, single-phase, and lanthanum europium ratio is adjustable arbitrarily, and molecular formula is written as La
2-xEu
xSn
2O
7, x=0～2, powder is of a size of 15～35 nanometers.
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| CN102906220A (en) * | 2010-06-09 | 2013-01-30 | 海洋王照明科技股份有限公司 | Oxide stannate luminescent materials and preparation methods thereof |
| CN104619813B (en) * | 2012-09-11 | 2016-08-24 | 海洋王照明科技股份有限公司 | Stannate luminescent material and preparation method thereof |
| US20150275083A1 (en) * | 2012-10-31 | 2015-10-01 | Ocean's King Lighting Science & Technology Co., Ltd | Silicate luminescent material and preparation method therefor |
| CN104261455B (en) * | 2014-09-23 | 2015-10-28 | 浙江大学 | A kind of preparation method of high purity stannic acid lanthanum nano-powder |
| CN104556208B (en) * | 2015-01-19 | 2016-08-24 | 陕西科技大学 | A kind of spherical Sm2sn2o7nanocrystalline preparation method |
| CN105969353B (en) * | 2016-07-29 | 2018-04-20 | 吉林大学 | One kind makes La2Sn2O7The reversible luminous method of material |
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| CN1544333A (en) * | 2003-11-28 | 2004-11-10 | 北京科技大学 | Nanocrystalline plumbum stannate powder preparation method |
| CN1792812A (en) * | 2006-01-09 | 2006-06-28 | 浙江理工大学 | Process for synthesizing spinel zine stannate nano rod |
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| CN1544333A (en) * | 2003-11-28 | 2004-11-10 | 北京科技大学 | Nanocrystalline plumbum stannate powder preparation method |
| CN1792812A (en) * | 2006-01-09 | 2006-06-28 | 浙江理工大学 | Process for synthesizing spinel zine stannate nano rod |
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