CN102502761B - Method for preparing square tablet assembled spherical lanthanum sulfide microcrystals by microwave hydrothermal method - Google Patents
Method for preparing square tablet assembled spherical lanthanum sulfide microcrystals by microwave hydrothermal method Download PDFInfo
- Publication number
- CN102502761B CN102502761B CN2011103749441A CN201110374944A CN102502761B CN 102502761 B CN102502761 B CN 102502761B CN 2011103749441 A CN2011103749441 A CN 2011103749441A CN 201110374944 A CN201110374944 A CN 201110374944A CN 102502761 B CN102502761 B CN 102502761B
- Authority
- CN
- China
- Prior art keywords
- solution
- hydrothermal reaction
- hydrothermal
- distilled water
- reaction kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention relates to a method for preparing square tablet assembled spherical lanthanum sulfide microcrystals by a microwave hydrothermal method. The method comprises the steps that: lanthanum chloride heptahydrate is dissolved into distilled water to obtain solution A; sodium thiosulfate pentahydrate dissolved in distilled water to obtain solution B; the solution A is added into the solution B to obtain solution C; the solution C is poured into a hydrothermal reaction kettle, and then, the hydrothermal reaction kettle is sealed and is placed in a microwave hydrothermal reaction instrument; a temperature control mode is selected for hydrothermal reaction, and the materials are naturally cooled to the room temperature after reaction completion; and the hydrothermal reaction kettle is opened, and products are respectively and sequentially washed by the distilled water and absolute ethyl alcohol and are dried in an electric heating constant-temperature blowing drying box to obtain La2S3 microcrystals. The method has the advantages that the simple microwave hydrothermal method preparation process is adopted, the reaction is completed in one step in liquid phases, the later-period treatment is not needed, raw materials are easy to obtain, the preparation cost is lower, the reaction period is short, the repeatability is high, a spherical lanthanum sulfide structure with the diameter being 5mum is prepared, and the structure is in a hole sphere shape assembled by square-tablet-shaped lanthanum sulfide crystals with the length being 1.5mum, the width being 1mum and the thickens being 10 to 20nm.
Description
Technical field
The present invention relates to a kind of La
2S
3The preparation method of crystallite, relate to the cubic sheet of a kind of microwave-hydrothermal method preparation preparation and be assembled into spherical lanthanum sulphide microcrystal method.
Technical background
Lanthanum sulfide is the rare earth chalcogenide material, extensively should be for [G.D.Bagde such as rare earth alloy preparation, superconduction, magnetic cooling, magneticthin film, photoelectricity and trermoelectromotive force devices, H.M.Pathan, C.D.Lokhande, et al.Studies on Sprayed Lanthanum Sulphide (La
2S
3) Thin Films from Non-aqueous Medium.Applied Surface Science, 2005,252:1502-1509].La
2S
3In crystalline state, 3 kinds of different allotropy structure (α, beta, gamma-La are arranged
2S
3).Lanthanum sulfide is present in two kinds of crystalline modifications: low-temperature phase (α) is that quadrature phase and Emission in Cubic (γ) can obtain during higher than 1000 ℃ at temperature.Middle Tetragonal (β) is actually oxysulfide (La
10S
15-xO
x), it is that a part of oxygen has replaced sulphur.β-La
2S
3Oxysulfide (La normally
10S
14O
1-xS
x, 0<x<1), Sauerstoffatom is stablized Tetragonal.β-La
2S
3Be commonly used to do fluorescent agent.γ-La
2S
3A defective cube of Th
3P
4Structure, it is similar to CaLa
2S
4, it has shown strong color, makes it become a potential new pigment and replaces some poisonous pigment in plastics.
At present, many research teams have prepared lanthanum sulfide by the physics and chemistry technology, La
2S
3the preparation method of film mainly contains vapour deposition process [Lu Tian, Ti Ouyang, Kian Ping Loh, et al.La
2S
3thin films from metal organic chemical vapor deposition ofsingle-source precursor.Journal of Materials Chemistry, 2006, 16:272-277], atomic layer epitaxy method [Kaupo Kukli, Hannele Heikkinen, ErjaNykanen, et al.Deposition of lanthanum sulfide thin films by atomiclayer epitaxy.Journal of Alloys and Compounds, 1998, 275-277:10-14], spray pyrolysis [G.D.Bagde, S.D.Sartale, C.D.Lokhande.Deposition andannealing effect on lanthanum sulfide thin films by spray pyrolysis.ThinSolid Films, 2003, 445:1-6] etc., preparation La
2S
3nanocrystalline method has high temperature solid-state method [Michihiro Ohta, Haibin Yuan, Shinji Hirai, et al.Preparation of R
2S
3(R:La, Pr, Nd, Sm) powders by sulfurization.Journal of Alloys andCompounds, 2004,374:112-115] and solvent-thermal method [Kaibin Tang, Changhua An, Pingbo Xie, et al.Low-temperature synthesis and characterization of β-La
2S
3nanorods.Journal of Crystal Growth, 2002,245:304-308], these methods prepare La
2S
3the film required equipment is more expensive, and cost is higher, and safety coefficient is low, and technique is difficult to control.
Summary of the invention
The objective of the invention is to propose that a kind of reaction time is short, temperature of reaction is low, greatly reduces energy consumption, has saved cost, and simple to operate, and the cubic sheet of microwave-hydrothermal method preparation preparation that is applicable to scale operation is assembled into spherical lanthanum sulphide microcrystal method.
For achieving the above object, the technical solution used in the present invention is:
1) at first by the analytically pure seven water Lanthanum trichloride (LaCl of 1～4mmol
37H
2O) be dissolved in 10～40mL distilled water, stir and obtain solution A;
2) by the analytically pure five water Sulfothiorine (Na of 2.5～7.5mmol
25
2O
35H2O) be dissolved in 30～80mL distilled water, stir and obtain solution B;
3) A solution is joined in B solution, stirs, with the vinegar acid for adjusting pH value be 4.0～5.0 solution C;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 60～80%; Then seal hydrothermal reaction kettle, put it in microwave hydrothermal reaction; Select temperature control mode, controlling hydrothermal temperature is 90～130 ℃, reaction 20min～60min, and reaction naturally cools to room temperature after finishing;
5) open hydrothermal reaction kettle, product is washed 2～5 times successively with distilled water, dehydrated alcohol respectively, under 40～60 ℃, dry 1～3h obtains La in electric heating constant-temperature blowing drying box
2S
3Crystallite.
Because microwave-hydrothermal method is to utilize glassware for drinking water that permanent dipole moment is arranged, the dipole relaxation can occur in the microwave alternating field, in system inside, directly cause the loss of micro-wave energy, come water heating kettle is heated.Microwave-hydrothermal method is a kind of method for preparing fast the nanoparticle of narrow diameter distribution, form homogeneous, has the incomparable superiority of some other method.The present invention adopts simple microwave-hydrothermal method preparation technology, reaction once completes in liquid phase, do not need post-processed, raw material is easy to get, and preparation cost is lower, reaction time is short, repeatability is high, prepares the spherical lanthanum sulfide structure of diameter 5um, and this structure is by long 1.5um, wide 1um, thickness are about pertusate spherical that the square-sheet lanthanum sulfide crystalline substance of 10～20nm assembles.
The accompanying drawing explanation
Fig. 1 is the prepared La of embodiment 1
2S
3Brilliant X-ray diffraction (XRD) collection of illustrative plates, wherein X-coordinate is diffraction angle 2 θ, and unit is °, and ordinate zou is diffraction peak intensity, and unit is cps.
Fig. 2 is the prepared La of embodiment 1
2S
3Brilliant field emission scanning electron microscope (FE-SEM) photo.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
1) at first by the analytically pure seven water Lanthanum trichloride (LaCl of 2mmol
37H
2O) be dissolved in 10mL distilled water, stir and obtain solution A;
2) by the analytically pure five water Sulfothiorine (Na of 6mmol
2S
2O
35H2O) be dissolved in 50mL distilled water, stir and obtain solution B;
3) A solution is joined in B solution, stirs, with the vinegar acid for adjusting pH value be 4.0 solution C;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 70%; Then seal hydrothermal reaction kettle, put it in microwave hydrothermal reaction; Select temperature control mode, controlling hydrothermal temperature is 120 ℃, reaction 60min, and reaction naturally cools to room temperature after finishing;
5) open hydrothermal reaction kettle, product is washed 2～5 times successively with distilled water, dehydrated alcohol respectively, under 40 ℃, dry 1h obtains La in electric heating constant-temperature blowing drying box
2S
3Crystallite.
Prepared crystallite is La as shown in Figure 1
2S
3Crystallite.
Prepared La as shown in Figure 2
2S
3Crystallite is the glomerate structure of cubic sheet assembling.
Embodiment 2:
1) at first by the analytically pure seven water Lanthanum trichloride (LaCl of 3mmol
37H
2O) be dissolved in 20mL distilled water, stir and obtain solution A;
2) by the analytically pure five water Sulfothiorine (Na of 4.5mmo1
2S
2O
35H2O) be dissolved in 30mL distilled water, stir and obtain solution B;
3) A solution is joined in B solution, stirs, with the vinegar acid for adjusting pH value be 4.5 solution C;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 60%; Then seal hydrothermal reaction kettle, put it in microwave hydrothermal reaction; Select temperature control mode, controlling hydrothermal temperature is 100 ℃, reaction 30min, and reaction naturally cools to room temperature after finishing;
5) open hydrothermal reaction kettle, product is washed 2～5 times successively with distilled water, dehydrated alcohol respectively, under 50 ℃, dry 3h obtains La in electric heating constant-temperature blowing drying box
2S
3Crystallite.
Embodiment 3:
1) at first by the analytically pure seven water Lanthanum trichloride (LaCl of 1mmol
37H
2O) be dissolved in 30mL distilled water, stir and obtain solution A;
2) by the analytically pure five water Sulfothiorine (Na of 2.5mmol
2S
2O
35H2O) be dissolved in 60mL distilled water, stir and obtain solution B;
3) A solution is joined in B solution, stirs, with the vinegar acid for adjusting pH value be 5.0 solution C;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 80%; Then seal hydrothermal reaction kettle, put it in microwave hydrothermal reaction; Select temperature control mode, controlling hydrothermal temperature is 90 ℃, reaction 50min, and reaction naturally cools to room temperature after finishing;
5) open hydrothermal reaction kettle, product is washed 2～5 times successively with distilled water, dehydrated alcohol respectively, under 60 ℃, dry 1h obtains La in electric heating constant-temperature blowing drying box
2S
3Crystallite.
Embodiment 4:
1) at first by the analytically pure seven water Lanthanum trichloride (LaCl of 4mmol
37H
2O) be dissolved in 40mL distilled water, stir and obtain solution A;
2) by the analytically pure five water Sulfothiorine (Na of 7.5mmol
2S
2O
35H2O) be dissolved in 80mL distilled water, stir and obtain solution B;
3) A solution is joined in B solution, stirs, with the vinegar acid for adjusting pH value be 4.0 solution C;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 75%; Then seal hydrothermal reaction kettle, put it in microwave hydrothermal reaction; Select temperature control mode, controlling hydrothermal temperature is 130 ℃, reaction 20min, and reaction naturally cools to room temperature after finishing;
5) open hydrothermal reaction kettle, product is washed 2～5 times successively with distilled water, dehydrated alcohol respectively, under 55 ℃, dry 2h obtains La in electric heating constant-temperature blowing drying box
2S
3Crystallite.
Claims (1)
1. preparing square tablet assembled spherical lanthanum sulfide microcrystals by microwave hydrothermal method method is characterized in that:
1) at first by the analytically pure seven water Lanthanum trichloride (LaCl of 1～4mmol
37H
2O) be dissolved in 10～40mL distilled water, stir and obtain solution A;
2) by the analytically pure five water Sulfothiorine (Na of 2.5～7.5mmol
2S
2O
35H
2O) be dissolved in 30～80mL distilled water, stir and obtain solution B;
3) A solution is joined in B solution, stirs, with the vinegar acid for adjusting pH value be 4.0～5.0 solution C;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 60～80%; Then seal hydrothermal reaction kettle, put it in microwave hydrothermal reaction; Select temperature control mode, controlling hydrothermal temperature is 90～130 ℃, reaction 20min～60min, and reaction naturally cools to room temperature after finishing;
5) open hydrothermal reaction kettle, product is washed 2～5 times successively with distilled water, dehydrated alcohol respectively, under 40～60 ℃, dry 1～3h obtains La in electric heating constant-temperature blowing drying box
2S
3Crystallite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103749441A CN102502761B (en) | 2011-11-23 | 2011-11-23 | Method for preparing square tablet assembled spherical lanthanum sulfide microcrystals by microwave hydrothermal method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103749441A CN102502761B (en) | 2011-11-23 | 2011-11-23 | Method for preparing square tablet assembled spherical lanthanum sulfide microcrystals by microwave hydrothermal method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102502761A CN102502761A (en) | 2012-06-20 |
| CN102502761B true CN102502761B (en) | 2013-11-27 |
Family
ID=46214912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103749441A Active CN102502761B (en) | 2011-11-23 | 2011-11-23 | Method for preparing square tablet assembled spherical lanthanum sulfide microcrystals by microwave hydrothermal method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102502761B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518073B (en) * | 2016-10-18 | 2019-02-15 | 西北工业大学 | A kind of γ-La of high infrared transmittance2S3Infrared transparent ceramic preparation |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101104746A (en) * | 2007-08-07 | 2008-01-16 | 中国科学院长春应用化学研究所 | Red rare-earth lanthanum cerium sulfide dye and preparation method thereof |
| CN101698501A (en) * | 2009-10-30 | 2010-04-28 | 陕西科技大学 | Method for preparing floriform cadmium sulfide nano-particles in microwave hydrothermal mode |
-
2011
- 2011-11-23 CN CN2011103749441A patent/CN102502761B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN102502761A (en) | 2012-06-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | A cost-effective method to fabricate VO2 (M) nanoparticles and films with excellent thermochromic properties | |
| CN101412505B (en) | Preparation of high-purity tin diselenide nano-plate | |
| CN101844799B (en) | Preparation method of hexagon stannic disulphide nano slice | |
| CN102942223B (en) | Preparation method of hexagonal flaky NH4V3O8 microcrystals | |
| AU2020101474A4 (en) | A Method for Preparing Nano α-Fe2O3 from Solid Waste Containing Iron under Solvent-free | |
| Sobhani et al. | Morphological control of MnSe2/Se nanocomposites by amount of hydrazine through a hydrothermal process | |
| CN102502762B (en) | Method for preparing lanthanum sulfide crystallite with thin and laminar packed structure through microwave hydrothermal method | |
| CN109825873B (en) | Preparation method of single-crystal bismuth ferrite film | |
| CN103864139A (en) | Preparation method of three-dimensional layered multilevel flower-shaped stannic oxide microsphere | |
| CN102502793B (en) | Preparation method of rod-shaped SnS nanocrystals | |
| CN101602524A (en) | A kind of hydrothermal synthesis method of potassium tantalite powder | |
| CN102285681A (en) | Low-temperature hydrothermal synthesis method of ZnO nano shuttle | |
| Wang et al. | Solution synthesis of ZnO nanotubes via a template-free hydrothermal route | |
| CN104016408A (en) | Synthetic method of sodium niobate nanowire | |
| Kavitha et al. | Annealing effect on nickel oxide nanoparticles synthesized by sol-gel method | |
| CN102502761B (en) | Method for preparing square tablet assembled spherical lanthanum sulfide microcrystals by microwave hydrothermal method | |
| CN102390856B (en) | Method for preparing high-stability gamma-phase nanometer lanthanum sulfide powder in low temperature | |
| CN102509648B (en) | Preparation method for Ga-doped ZnO nanometer material | |
| CN104402065A (en) | Preparation method of spheroidic CoS2 nanometer powder | |
| CN103882558B (en) | A kind of perovskite structure AgNbO 3fiber and preparation method thereof | |
| Liu et al. | Synthesis of ZnGa2O4 octahedral crystallite by hydrothermal method with the aid of CTAB and its photocatalytic activity | |
| CN108910948A (en) | A kind of niobic acid tin nanometer sheet and preparation method thereof | |
| Hu et al. | Novel synthesis of CuO nanofiber balls and films and their UV–visible light filteration property | |
| CN102390859B (en) | Phonochemical method for preparing rod-shaped lanthanum sulphide microcrystal | |
| CN102390857B (en) | Method for preparing flaky microcrystalline La2S3 with hydrothermal process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201124 Address after: No.32, group 3, Fuzi village, Donghai Town, Qidong City, Nantong City, Jiangsu Province Patentee after: Qidong Shiji crop cooperatives Address before: 808, floor 8, building B, business center, gangzhilong science and Technology Park, No. 6, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Pengbo Information Technology Co.,Ltd. Effective date of registration: 20201124 Address after: 808, floor 8, building B, business center, gangzhilong science and Technology Park, No. 6, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Pengbo Information Technology Co.,Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang University Park No. 1 Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220307 Address after: 226000 No. 110, Xinfeng street, Donghai Town, Qidong City, Nantong City, Jiangsu Province Patentee after: Qidong Xincheng New Material Technology Co.,Ltd. Address before: No.32, group 3, Fuzi village, Donghai Town, Qidong City, Nantong City, Jiangsu Province Patentee before: Qidong Shiji crop cooperatives |