CN102070178A - Method for preparing yttrium oxide micro-nano-materials based on hydrothermal technology regulation and control - Google Patents
Method for preparing yttrium oxide micro-nano-materials based on hydrothermal technology regulation and control Download PDFInfo
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- CN102070178A CN102070178A CN 201110047695 CN201110047695A CN102070178A CN 102070178 A CN102070178 A CN 102070178A CN 201110047695 CN201110047695 CN 201110047695 CN 201110047695 A CN201110047695 A CN 201110047695A CN 102070178 A CN102070178 A CN 102070178A
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Abstract
The invention provides a method for preparing yttrium oxide micro-nano-materials based on hydrothermal technology regulation and control. In the method, the yttrium oxide micro-nano-materials with different appearances are prepared by a hydrothermal reaction. The preparation method specifically comprises the following steps of: first, adding a certain amount of urea into yttrium-containing inorganic acid salt solution, and performing the hydrothermal reaction on the solution in a stainless steel high-pressure reaction kettle with a lining made from polytetrafluoroethylene for a period of time under a certain temperature to obtain a precursor of micro-nano yttrium oxide; then, colleting a product, washing the product with water, and drying the washed product to obtain a white precursor; and finally, roasting the precursor in a muffle furnace, and dewatering and decomposing to obtain a micro-nano-structural Y2O3. The control of the appearances and the sizes of the product are realized by controlling the parameters such as the adding amount of the urea in a reaction system, the temperature and the time of the hydrothermal reaction and the like. The method has a simple and easily implemented process, high reproducibility, mild experiment conditions, low cost and low price, and is suitable for industrial large-scale production.
Description
Technical field
The present invention relates to a kind ofly prepare the method for different-shape yttrium oxide micro Nano material, belong to field of nanometer material technology by hydrothermal technique regulation and control.
Background technology
In recent years, have special performance-surface effects, volume effect, quantum size effect and the macro quanta tunnel effect etc. that are different from block materials and individual molecule owing to nano material and it causes people's great attention in the important application of all many-sides such as electronics, optics, chemical industry, pottery, biology and medicine.Nanoparticle with nano-scale structures feature comprises that stable cluster or artificial nanocrystalline, nano particle, nanotube, nano wire, nanometer individual layer and nanoporous etc. all can be used as the structural motif that makes up new function material.Along with the further investigation of people to nano material, discovery causes the critical size of the particulate that nano material character changes and inequality, the performance of material is not only relevant with the component of its physical/chemical own, environment for use, also with numerous relating to parameters relevant (C. Burda, X. B. Chen, R. Narayanan such as preparation method, surface tissue, exposure crystal faces with pattern, M. A. El-Sayed, Chem. Rev. 2005,105, and 1025).Therefore, the control of nano material is synthetic to be the basis of realizing material property and application thereof, effectively utilize nano material, must at first resolve the preparation problem of nano material.
Nano yttrium oxide is owing to not only have good heat-resisting, corrosion-resistant and high-temperature stability, also have unique physics and chemical property, therefore, be widely used among the high-tech material, as fields such as fuel cell, superconducting material, advanced structural ceramic, transmitters, thereby caused numerous investigators' very big interest.In in the past 10 years, chemistry and material scholar have prepared multiple yttrium oxide nano material, comprise structure (H. X. Mai, the Y. W. Zhang of nanometer rod, nanometer plate, microballoon, nanometer polyhedral and other pattern, R. Si, Z. G. Yan, L. D. Sun, L. P. You, C. H. Yan, J. Am. Chem. Soc. 2006,128,6426; Si R., Y. W. Zhang, L. P. You, C. H. Yan, Angew. Chem. Int. Ed. 2005,44,3256; Y. B. Mao, J. Y. Huang, R. Ostroumov, K. L. Wang, J. P. Chang, J. Phys. Chem. C 2008,112,2278; L. Li, C. K. Tsung, Z. Yang, G. D. Stucky, L. D. Sun, J. F. Wang, C. H. Yan, Adv. Mater. 2008,20,903) the control synthetic method that, is adopted mainly contains alkoxide hydrolysis, sol-gel method, spray heating decomposition, chemical Vapor deposition process, solid phase method etc.These preparation method's majorities have adopted template or have needed the very expensive organometallic compound of price, have increased the material preparation cost; In addition, these preparation methods realize that to yttrium oxide pattern, particle diameter and structure complete controlledly synthesis also has certain difficulty.
Summary of the invention
The objective of the invention is defective at existing yttrium oxide preparation method of nano material, provide a kind of technology simple, good reproducibility, cost is low and cheap, cost is low, be suitable for suitability for industrialized production and can realize the preparation method of nano yttrium oxide pattern, particle diameter and the complete controlledly synthesis of structure, prepared nanoparticle purity height, epigranular, pattern uniqueness.
For achieving the above object, the present invention adopts following technical scheme:
In containing yttrium inorganic acid salt solution, add earlier a certain amount of urea,, obtain the precursor of micro-nano yttrium oxide solution hydro-thermal reaction for some time under the certain temperature in the stainless steel autoclave that with the tetrafluoroethylene is liner; With product collection, wash with water then, dry back obtains white precursor; With precursor calcination process in retort furnace, the Y that obtains micro nano structure is decomposed in dehydration at last
2O
3
The technical program combines precipitation from homogeneous solution with hydrothermal technique method, under hydrothermal condition, slowly hydrolysis generates precipitation agent, with Y by means of urea
3+Homogeneous coprecipitation takes place, and the nanoparticle agglomeration of Sheng Chenging is few like this, easily disperses.In addition, when this method prepares nano material, can control the pattern and the size of particles of final product to modes such as the influence of pH, concentration, sedimentation speed, hydrothermal temperatures by the amount of control urea.
The described yttrium inorganic salt solution that contains is hydrochloride or nitrate;
The add-on of described urea is 0.5 ~ 5.0 g;
Described hydrothermal temperature is 140 ~ 180 oC;
The described hydro-thermal reaction time is 1 ~ 12 hour;
Described in retort furnace the temperature of calcination process be about 600 oC.
Compared with prior art, the present invention has following beneficial effect:
A) raw material sources of the present invention are extensive, simple, the good reproducibility of technology, and cost is low and cheap, and cost is low, be suitable for suitability for industrialized production;
B) preparation method of the present invention does not need to add the template and the catalyzer of any complexity, and is simple to operation;
C) preparation method of the present invention can realize the controlledly synthesis of nano yttrium oxide pattern, particle diameter and structure;
D) nano yttrium oxide pattern uniqueness, purity height, the particle aggregation phenomenon of material the present invention program preparation are few, easily disperse.
Description of drawings
Fig. 1 is the SEM photo of the Yttrium oxide material for preparing under the different condition.Wherein, (a b) is the dumbbell shaped yttrium oxide of 140 ° of C preparations; (c d) is the yttrium oxide of 180 ° of C preparations; (e) be the yttrium oxide microballoon; (f) be the yttrium oxide nanometer sheet.
Fig. 2 is under 140 ° of C and the 180 ° of C hydrothermal conditions, the XRD figure of the yttrium oxide precursor of preparation.Wherein, (a) be the dumbbell shaped yttrium oxide of 140 ° of C preparation; (b) be the yttrium oxide of 180 ° of C preparations; (c) be the yttrium oxide microballoon; (d) be the yttrium oxide nanometer sheet.
Fig. 3 is the XRD figure that obtains Yttrium oxide material after 600 ° of C calcinings.Wherein, (a) be the dumbbell shaped yttrium oxide of 140 ° of C preparation; (b) be the yttrium oxide of 180 ° of C preparations; (c) be the yttrium oxide microballoon; (d) be the yttrium oxide nanometer sheet.
Fig. 4 is the add-on of control urea, the SEM photo of the Yttrium oxide material of preparation.Wherein, (a) 0.5 g; (b) 1.0 g; (c) 1.5 g; (d) 3.0 g.
Fig. 5 is the control hydro-thermal synthetic time, the SEM photo of the Yttrium oxide material of preparation.
Embodiment
Below by example the method for preparing the yttrium oxide micro Nano material based on hydrothermal technique regulation and control of the present invention is described further.This example is being to implement under the prerequisite with the present invention program, has provided detailed embodiment and concrete operating process.
Embodiment 1
The preparation of dumbbell shaped yttrium oxide nano material: with 3.83 g Y (NO
3)
36H
2O and 0.5 g urea are dissolved in the 38 mL water, stir to form settled solution, transfer to 50 mL autoclave (polytetrafluoroethyllining lining, stainless steel casing) in, sealing, 140 ° of C hydrothermal treatment consists 12 hours, reaction finishes the back and takes out reactor, naturally cools to room temperature.With product collection, wash with water, drying obtains white precursor Y (OH) CO
3, XRD characterizes as shown in Figure 2.With material calcination process in 600 oC retort furnaces, the dehydration decomposition obtains dumbbell shaped nanometer Y at last
2O
3, collect to be measured.This sample brief note is YCHD-140.(Fig. 1-a, 1-b), XRD is shown in Fig. 3-a by the scanning electron microscope sign for the size of product and pattern.As Fig. 1-a, shown in the 1-b, about 50 ~ 70 μ m of YCHD-140 size have special dumbbell pattern, go up and form its secondary structure by many tiny irregular nano particles.
Embodiment 2
Press the preparation method of embodiment 1, just change 140 ° of C of described hydrothermal temperature into 180 ° of C, the precursor of acquisition characterizes as shown in Figure 2, and the SEM photo of the micron yttrium oxide structure that finally obtains is shown in Fig. 1-c and 1-d, XRD characterizes shown in Fig. 3-b, as seen from the figure Y
2O
3The dumbbell pattern remain unchanged substantially, but its secondary structure becomes the pane of rule.
Press the preparation method of embodiment 1, just the add-on with urea changes 1.0 g respectively into, dumbbell shaped nanometer Y
2O
3Change into microspheric Y
2O
3The SEM photo of product presents the microballoon of 2 ~ 4 μ m sizes shown in Fig. 1-e.XRD is shown in Fig. 3-c.
Embodiment 4
Press the preparation method of embodiment 1, just the add-on with urea changes 3.0 g respectively into, microspheric Y
2O
3Change into the Y of nanometer sheet type
2O
3The SEM photo of product is shown in Fig. 1-f, and products therefrom has the laminated structure pattern.XRD is shown in Fig. 3-d.
Embodiment 5
Press the preparation method of embodiment 1, just the add-on with urea changes 1.5 g respectively into.The SEM photo of product is shown in Fig. 4-c.Obtaining product YCHD-M is the mixture of microballoon and laminated structure.These results show that hydrothermal temperature and urea add dosage at Y
2O
3The control building-up process in play a part important.
Press the preparation method of embodiment 1, just changed 140 ° of C hydrothermal treatment consists into 140 ° of C hydrothermal treatment consists 9 hours in 12 hours respectively, 6 hours and 3 hours.The SEM photo of product as shown in Figure 5.
Embodiment 7
Implement relevant compound experiment, to understand different-shape Y
2O
3The growth mechanism of nanostructure (Fig. 4, Fig. 5).For dumbbell shaped YCHD-140, urea slowly decomposes under hydrothermal condition, begins crystallization nucleation when reaching certain pH value, takes place simultaneously to reunite with the reduction surface energy under a high energy non-equilibrium condition.Adjacent is nanocrystalline under the Van der Waals force effect, according to the spontaneous gathering growth of certain orientation.Can be clearly seen that from Fig. 5, globosity is the intermediate state that dumbbell shaped YCHD-140 pattern develops, prolongation along with the reaction times, it is ripe theoretical to follow Ostwald, and dissolving-recrystallization balance impels little particle to dissolve gradually, in saturated mother liquor, big particle is according to certain orientation, long more big more, finish up to urea decomposition, obtain to have the YCHD-140 dumbbell shaped of graded structure.Experimental result shows that in the higher environment of urea concentration, urea can play the effect of coating.Concerning the yttrium oxide microballoon, precipitation from homogeneous solution (PFHS) and agglomeration remain the key factor that influences its growth mechanism.Recently, Clutelcean(R. Custelcean,
Chem. Commun.2008,295) reported that in one piece of summary urea molecule both can be by the contributor of NH group as hydrogen bond, also can pass through the recipient of the lone-pair electron of C=O group as hydrogen bond, complementation good between these two kinds of groups can the oneself be cross-linked to form the two-dimensional layer framework, the reason of this may to be exactly yttrium oxide grow up under the excessive hydrothermal condition of urea layered nano-structure.
Claims (7)
1. method for preparing the yttrium oxide micro Nano material based on hydrothermal technique regulation and control, it is characterized in that: in containing the yttrium inorganic acid salt aqueous solution, add a certain amount of urea earlier, with solution hydro-thermal reaction for some time under the certain temperature in the stainless steel autoclave that with the tetrafluoroethylene is liner, obtain the precursor of micro-nano yttrium oxide; With product collection, wash with water then, dry back obtains white precursor; With precursor calcination process in retort furnace, the yttrium oxide that obtains micro nano structure is decomposed in dehydration at last.
2. according to claim 1ly prepare the method for yttrium oxide micro Nano material, it is characterized in that described method is a hydrothermal synthesis method based on hydrothermal technique regulation and control.
3. according to claim 1ly prepare the method for yttrium oxide micro Nano material, it is characterized in that the described yttrium inorganic salt solution that contains is hydrochloride or nitrate based on hydrothermal technique regulation and control.
4. according to claim 1ly prepare the method for yttrium oxide micro Nano material based on hydrothermal technique regulation and control, the add-on that it is characterized in that described urea is 0.5 ~ 5.0 g.
5. according to claim 1ly prepare the method for yttrium oxide micro Nano material, it is characterized in that described hydrothermal temperature is 140 ~ 180 oC based on hydrothermal technique regulation and control.
6. according to claim 1ly prepare the method for yttrium oxide micro Nano material, it is characterized in that the described hydro-thermal reaction time is 1 ~ 12 hour based on hydrothermal technique regulation and control.
7. according to claim 1ly prepare the method for yttrium oxide micro Nano material based on hydrothermal technique regulation and control, it is characterized in that described in retort furnace the temperature of calcination process be about 600 oC.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351234A (en) * | 2011-07-14 | 2012-02-15 | 浙江理工大学 | Hydro-thermal preparation method of dumbbell shape yttrium oxide gadolinium crystal |
| CN105776308A (en) * | 2016-04-08 | 2016-07-20 | 天津城建大学 | Micron-order spheres using rare earth yttrium oxide nanotubes as elements and preparation method thereof |
| CN105883888A (en) * | 2016-04-08 | 2016-08-24 | 天津城建大学 | Micron-scale flower-like sphere assembled with yttrium oxide nanosheets |
| CN106044835A (en) * | 2016-06-08 | 2016-10-26 | 广西科技大学 | Preparation method of nanoscale spherical yttrium oxide powder |
| RU2702588C1 (en) * | 2019-06-14 | 2019-10-08 | Федеральное государственное автономное образовательное учреждение высшего образования "Южно-Уральский государственный университет (национальный исследовательский университет)" ФГАОУ ВО "ЮУрГУ (НИУ)" | Method of producing yttrium oxide for ceramic articles |
| CN115490257A (en) * | 2022-08-31 | 2022-12-20 | 贵州大学 | N-doped submicron spherical Y 2 O 3 Preparation method of (1) |
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| CN1840480A (en) * | 2005-03-29 | 2006-10-04 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN101857263A (en) * | 2010-06-23 | 2010-10-13 | 东华大学 | Method for preparing nano indium oxide with controllable appearance by hydrothermal method |
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| CN1840480A (en) * | 2005-03-29 | 2006-10-04 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351234A (en) * | 2011-07-14 | 2012-02-15 | 浙江理工大学 | Hydro-thermal preparation method of dumbbell shape yttrium oxide gadolinium crystal |
| CN105776308A (en) * | 2016-04-08 | 2016-07-20 | 天津城建大学 | Micron-order spheres using rare earth yttrium oxide nanotubes as elements and preparation method thereof |
| CN105883888A (en) * | 2016-04-08 | 2016-08-24 | 天津城建大学 | Micron-scale flower-like sphere assembled with yttrium oxide nanosheets |
| CN106044835A (en) * | 2016-06-08 | 2016-10-26 | 广西科技大学 | Preparation method of nanoscale spherical yttrium oxide powder |
| RU2702588C1 (en) * | 2019-06-14 | 2019-10-08 | Федеральное государственное автономное образовательное учреждение высшего образования "Южно-Уральский государственный университет (национальный исследовательский университет)" ФГАОУ ВО "ЮУрГУ (НИУ)" | Method of producing yttrium oxide for ceramic articles |
| CN115490257A (en) * | 2022-08-31 | 2022-12-20 | 贵州大学 | N-doped submicron spherical Y 2 O 3 Preparation method of (1) |
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Application publication date: 20110525 |