CN1559911A - Process for preparing hollow ball of single dispersion cadmium sulfide - Google Patents
Process for preparing hollow ball of single dispersion cadmium sulfide Download PDFInfo
- Publication number
- CN1559911A CN1559911A CNA2004100164968A CN200410016496A CN1559911A CN 1559911 A CN1559911 A CN 1559911A CN A2004100164968 A CNA2004100164968 A CN A2004100164968A CN 200410016496 A CN200410016496 A CN 200410016496A CN 1559911 A CN1559911 A CN 1559911A
- Authority
- CN
- China
- Prior art keywords
- ball
- cadmium
- monodisperse
- mol
- hollow
- 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.)
- Granted
Links
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 32
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims description 18
- 239000006185 dispersion Substances 0.000 title 1
- 238000004519 manufacturing process Methods 0.000 title 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 15
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 14
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 claims abstract description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000001509 sodium citrate Substances 0.000 claims abstract description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000005864 Sulphur Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 210000002700 urine Anatomy 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 3
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 3
- 238000001556 precipitation Methods 0.000 abstract 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000008139 complexing agent Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 7
- 229910052793 cadmium Inorganic materials 0.000 description 6
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 239000004793 Polystyrene Substances 0.000 description 4
- 239000011022 opal Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229920002223 polystyrene Polymers 0.000 description 4
- 238000000151 deposition Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000002003 electron diffraction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004038 photonic crystal Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 1
- 239000004991 Lytropic liquid crystal Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000224 chemical solution deposition Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method of preparing monodisperse cadmium sulphide hollow balls, adopting a chemical water bath precipitation method, including the following steps: 1) dispersing the uniform-sized silicon oxide ball in the deionized water solution by ultrasonic vibration, adding in sodium citrate as complexing agent and using ammonia water to regulate pH value to 8-13, stirring at constant temperature of 50 deg.C-90 deg.C by magnetic force, then adding in cadmium chloride and thiourea to react for 1-2 hours, so as to form a nuclear shell structure of cadmium sulphide coating silicon oxide ball; 2) using diluted hydrofluoric acid to corrode the kernel of the silicon oxide to obtain the hollow cadmium sulphide ball; 3) adopting centrifugal precipitation and ultrasonic dispersion to circularly wash the ball by the deionized water and anhydrous alcohol so as to eliminate reaction remnants, and then drying to obtain the monodisperse cadmium sulphide hollow ball. The made ball can act as structural basic element to prepare 3D photon crystals with high-refractive index contrast, large duty factor, and complete photonic bandgap.
Description
Technical field
The present invention relates to prepare the method for monodisperse CdS hollow ball.
Background technology
Photonic crystal is the artificial microstructure that can be compared with optical wavelength by its cycle that the material with differing dielectric constant (specific refractory power) is arranged according to certain spacial ordering.As " optical semiconductor ", photonic crystal has the function of unique adjusting light spread state, and, fields such as photon integrated, optical communication integrated at photoelectricity have boundless application prospect.In recent years, the research of three-D photon crystal has caused more and more investigators' interest, and preparation three-D photon crystal method commonly used is that monodispersity balls such as silica spheres or polystyrene are self-assembled into the opal structural with center of area solid matter under the certain force field action.But this preparation method is difficult to prepare large-area ordered structure, and this structure of preparing simultaneously can not satisfy the requirement (being dutycycle＞80% and index contrast＞2.8) that preparation has the photon crystal material of complete band gap; Also need in opal, to fill again high-index material, and then silicon-dioxide or polystyrene are removed with the method for preferential etch, obtain counter opal structure.
Has high refractive index hollow ball material (as Cadmium Sulfide) has center of area solid matter from composition as structural unit opal structural and utilize, can satisfy the requirement that preparation has the three-D photon crystal of complete photonic band gap, strengthen the photon band gap characteristic of this structure greatly.
Cadmium Sulfide (CdS) is that a kind of very important IV-VI family has direct wide bandgap semiconductor materials, is widely used in electronics, optoelectronic areas.Because this material has high relatively specific refractory power and superior optical property, also is widely used in the photonic material field in recent years.The preparation of hollow cadmium sulphide ball has several different methods, for example adopts lytropic liquid crystals, dithiocarbonic anhydride drop, polystyrene acid particles, both sexes three multipolymers etc. to be template, at first prepares nucleocapsid structure, template is removed obtained cadmium sufide hollow ball then.When the preparation nucleocapsid structure, need to carry out pre-treatment to examining the surface earlier, and because the template that adopts is not a monodispersity, the cadmium sufide hollow ball of these method preparations does not have monodispersity, and the thickness of ball wall is uncontrollable.
Summary of the invention
The objective of the invention is for obtaining to have the three-D photon crystal of complete photonic band gap, the method for the monodisperse CdS hollow ball that a kind of preparation has high refractive index is provided.
The method for preparing the monodisperse CdS hollow ball of the present invention, employing be chemical bath deposition, may further comprise the steps:
1) the uniform monodisperse silica sphere particle of particle diameter is dispersed in the deionized water solution with sonic oscillation, add Trisodium Citrate and do network and agent, and regulate pH value to 8～13 with ammoniacal liquor, 50 ℃～90 ℃ constant temperature magnetic agitation, add Cadmium chloride fine powder and sulphur urine then, the concentration that makes Cadmium chloride fine powder in the solution is 0.001 mol～0.01 mol, and the concentration of sulphur urine is 0.002 mol～0.02 mol, reacted 1～2 hour, and obtained the nucleocapsid structure of Cadmium Sulfide parcel silica spheres;
2) with the hydrofluoric acid corrode silicon dioxide core of dilution, obtain hollow cadmium sulphide ball;
3) adopt centrifugal deposition to add the ultra-sonic dispersion wash cycles with deionized water and dehydrated alcohol, remove reaction residue, oven dry obtains the monodisperse CdS hollow ball.
The hydrofluoric acid concentration that dilutes among the present invention is generally 1%～10%.Monodisperse silica sphere particle can be commercially available or by " Si Tuobu (Stober) method " preparation, particle diameter is that 10nm is to 1000nm.
The inventive method can be regulated the sphere diameter of hollow ball by changing the particle diameter of silicon-dioxide ball template; Change the concentration of Cadmium chloride fine powder and sulphur urine, can regulate the wall thickness of hollow ball.
Method of the present invention is template with the monodisperse silica sphere particle, and silica spheres is compared with polystyrene spheres and can high temperature heat-resistant be handled.By the deposition of chemical bath in alkaline aqueous solution, need not carry out pre-treatment to the silica spheres surface again, just can obtain nucleocapsid structure, method is simple.Chemical corrosion silica core then obtains the monodisperse CdS hollow ball of uniform particle diameter.The monodisperse CdS hollow ball that the present invention makes can be used as structural motif, and preparation has high-index contrast and the big three-D photon crystal of dutycycle, obtains having the three-D photon crystal of complete photonic band gap.Utilization has the hollow cadmium sulphide ball of high refractive index has center of area solid matter from composition as structural unit opal structural, the preparation method is simple, not only can satisfy the requirement that preparation has the three-D photon crystal of complete photonic band gap, strengthen the photon band gap characteristic of this structure greatly, can also regulate the residing position of photon band gap by the sphere diameter and the wall thickness that change hollow ball.
Description of drawings
Fig. 1 is a Cadmium Sulfide nucleocapsid structure transmission electron microscope photo, and wherein: figure a) for the transmission electron microscope photo of Cadmium Sulfide parcel silica spheres nucleocapsid structure, schemes b) be the transmission electron microscope photo of monodisperse hollow cadmium sulphide ball;
Fig. 2 is the transmission electron microscope photo of single cadmium sufide hollow ball, and the upper left corner is its electron diffraction;
Fig. 3 is the field emission scanning electron microscope photo of cadmium sufide hollow ball;
Fig. 4 is the XRD figure spectrum of hollow cadmium sulphide ball.
Embodiment
Embodiment:
1) monodisperse silica sphere particle that is 430nm with 300 milligrams of particle diameters is dispersed in the 250 ml deionized water solution with sonic oscillation, and the Trisodium Citrate that adds 10 milliliter of 0.1 mol is done network and agent, and regulates pH value to 11 with ammoniacal liquor.60 ℃ of constant temperature magnetic agitation, drip the sulphur urine of the Cadmium chloride fine powder of 10 milliliter of 0.1 mol and 50 milliliter of 0.04 mol then, react 2 hours, obtain nucleocapsid structure that Cadmium Sulfide wraps up silica spheres (a) as Fig. 1;
2) with 1 to 10 dilute hydrofluoric acid erosion removal silica core, obtain hollow cadmium sulphide ball;
3) adopt centrifugal deposition to add the ultra-sonic dispersion wash cycles with deionized water and dehydrated alcohol, remove reaction residue, 60 ℃ of oven dry obtain monodisperse CdS hollow ball (as Fig. 1 b).
Fig. 2 is the transmission electron microscope photo of the single cadmium sufide hollow ball that makes, has provided the electron diffraction spot simultaneously among the figure, and visible cadmium sulphide ball is a polycrystalline.
Fig. 3 is a use emission scan electron microscopic observation cadmium sufide hollow ball, has hollow structure really from visible its of wherein broken sample.
Products therefrom is XRD tests its crystalline structure, as shown in Figure 4, the component of visible resulting hollow ball is the Cadmium Sulfide with hexaplanar structure really.
Claims (1)
1. the method for preparing the monodisperse CdS hollow ball is characterized in that may further comprise the steps:
1) the uniform monodisperse silica sphere particle of particle diameter is dispersed in the deionized water solution with sonic oscillation, add Trisodium Citrate and do network and agent, and regulate pH value to 8～13 with ammoniacal liquor, 50 ℃～90 ℃ constant temperature magnetic agitation, add Cadmium chloride fine powder and sulphur urine then, the concentration that makes Cadmium chloride fine powder in the solution is 0.001 mol～0.01 mol, and the concentration of sulphur urine is 0.002 mol～0.02 mol, reacted 1～2 hour, and obtained the nucleocapsid structure of Cadmium Sulfide parcel silica spheres;
2) with the hydrofluoric acid corrode silicon dioxide core of dilution, obtain hollow cadmium sulphide ball;
3) adopt centrifugal deposition to add the ultra-sonic dispersion wash cycles with deionized water and dehydrated alcohol, remove reaction residue, oven dry obtains the monodisperse CdS hollow ball.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410016496 CN1226192C (en) | 2004-02-20 | 2004-02-20 | Process for preparing hollow ball of single dispersion cadmium sulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410016496 CN1226192C (en) | 2004-02-20 | 2004-02-20 | Process for preparing hollow ball of single dispersion cadmium sulfide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1559911A true CN1559911A (en) | 2005-01-05 |
| CN1226192C CN1226192C (en) | 2005-11-09 |
Family
ID=34440507
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410016496 Expired - Fee Related CN1226192C (en) | 2004-02-20 | 2004-02-20 | Process for preparing hollow ball of single dispersion cadmium sulfide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1226192C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331757C (en) * | 2005-11-23 | 2007-08-15 | 南京师范大学 | Process for preparing nano-grade cadmium sufide hollow ball |
| CN101058437B (en) * | 2007-04-10 | 2010-10-06 | 安徽大学 | Liquid state preparation method for nano cadmium sulfide hollow sphere |
| WO2010121488A1 (en) | 2009-04-21 | 2010-10-28 | 河北勇龙邦大新材料有限公司 | Method and device for producing hollow microspheres |
| CN101319404B (en) * | 2008-06-10 | 2012-05-16 | 浙江大学 | Method for preparation of hollow spherical cadmium sulfide nanocrystalline |
| CN104722775A (en) * | 2015-03-11 | 2015-06-24 | 浙江大学 | Two-dimensional hollow palladium nanocrystal and preparation method thereof |
| CN106513018A (en) * | 2016-09-30 | 2017-03-22 | 江苏大学 | Preparation method and application of ZnFe2O4@CdS composite photocatalyst with core-shell structure |
| CN111629993A (en) * | 2017-12-28 | 2020-09-04 | D.施华洛世奇两合公司 | Method and apparatus for manufacturing photonic crystal |
| TWI853797B (en) | 2017-12-28 | 2024-09-01 | 奧地利商施華洛世奇股份有限公司 | Method and apparatus for manufacturing photonic crystals |
-
2004
- 2004-02-20 CN CN 200410016496 patent/CN1226192C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331757C (en) * | 2005-11-23 | 2007-08-15 | 南京师范大学 | Process for preparing nano-grade cadmium sufide hollow ball |
| CN101058437B (en) * | 2007-04-10 | 2010-10-06 | 安徽大学 | Liquid state preparation method for nano cadmium sulfide hollow sphere |
| CN101319404B (en) * | 2008-06-10 | 2012-05-16 | 浙江大学 | Method for preparation of hollow spherical cadmium sulfide nanocrystalline |
| WO2010121488A1 (en) | 2009-04-21 | 2010-10-28 | 河北勇龙邦大新材料有限公司 | Method and device for producing hollow microspheres |
| CN104722775A (en) * | 2015-03-11 | 2015-06-24 | 浙江大学 | Two-dimensional hollow palladium nanocrystal and preparation method thereof |
| CN106513018A (en) * | 2016-09-30 | 2017-03-22 | 江苏大学 | Preparation method and application of ZnFe2O4@CdS composite photocatalyst with core-shell structure |
| CN106513018B (en) * | 2016-09-30 | 2019-08-02 | 江苏大学 | A kind of core-shell structure ZnFe2O4The preparation method and its usage of@CdS composite photo-catalyst |
| CN111629993A (en) * | 2017-12-28 | 2020-09-04 | D.施华洛世奇两合公司 | Method and apparatus for manufacturing photonic crystal |
| US11473213B2 (en) * | 2017-12-28 | 2022-10-18 | D. Swarovski Kg | Method and apparatus for manufacturing photonic crystals |
| CN111629993B (en) * | 2017-12-28 | 2024-01-30 | D.施华洛世奇两合公司 | Method and apparatus for fabricating photonic crystals |
| TWI853797B (en) | 2017-12-28 | 2024-09-01 | 奧地利商施華洛世奇股份有限公司 | Method and apparatus for manufacturing photonic crystals |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1226192C (en) | 2005-11-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Shi et al. | Growth of flower-like ZnO via surfactant-free hydrothermal synthesis on ITO substrate at low temperature | |
| CN100404411C (en) | Method for preparing nano powder of elementary substance by using reducing agent to reduce oxide | |
| CN102140691A (en) | Method for synthesizing vanadium acid zinc micro/nanowire material by adopting hydrothermal method | |
| JPS62223019A (en) | Crystalline tin-antimony oxide sol and production thereof | |
| CN101955222A (en) | Method for preparing anatase-phase titanium dioxide sol | |
| CN1226192C (en) | Process for preparing hollow ball of single dispersion cadmium sulfide | |
| CN110294495A (en) | A method of preparing TaO2F nanometer rods | |
| JP2022553585A (en) | Nano zirconium oxide powder, preparation method thereof, resulting dispersion, optical film | |
| CN103787405A (en) | Preparation method of rutile-phase tin dioxide sol | |
| Salim et al. | A Preliminary Study on Structural and Optical Properties of Heat Treated Nb 2 O 5 Nanostructure. | |
| CN1323759A (en) | Nanometer grade tetragonal-phase barium titanate powder and its prepn. | |
| CN101279208B (en) | Method for preparing Y type molecular sieve film | |
| CN103755958B (en) | A kind of preparation method of polyimides/CaCu 3 Ti 4 O coated with silver nano particle composite material | |
| CN1258823C (en) | Method for preparing monodisperse cadium sulfide-silicon dioxide nucleo capsid structure | |
| CN101367544B (en) | Preparation method for necklace shaped lead titanate nano wire | |
| CN110255619A (en) | Method for preparing molybdenum sulfide with three-dimensional hollow structure based on up-conversion nanoparticles | |
| CN1285512C (en) | Method for preparing In2O3 nanometer rod by sol-gel method | |
| CN1974485A (en) | Process of preparing nanomter zinc oxide/sulfide core-shell structure | |
| CN1240809C (en) | Method for preparing nano luminescent powder made from yttrium europium vanadate | |
| CN103043720B (en) | Preparation method of sub-nanometer yttrium vanadate powder | |
| CN100365170C (en) | SnO2 monodisperse nano monocrystal with square structure and synthesis method thereof | |
| CN108910947B (en) | Thin-sheet micro-nano (K, Na) NbO3Crystal and method for producing same | |
| Liao et al. | Shape-controllable synthesis of dendritic silver nanostructures at room temperature | |
| CN103771484B (en) | The preparation method of the regulatable Red copper oxide micron ball of a kind of particle diameter | |
| Dhahir et al. | Study the effect of PH variation on the particle size of SiO2 thin films |
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 | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |