CN104845622A - Method for preparing hexagonal phase upconversion nanometer material from ricinoleic acid - Google Patents
Method for preparing hexagonal phase upconversion nanometer material from ricinoleic acid Download PDFInfo
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Abstract
The invention discloses a method for preparing a hexagonal phase upconversion nanometer material from ricinoleic acid. The method comprises 1, weighing yttrium oxide, ytterbium oxide, erbium oxide and/or thulium oxide, and holmium oxide powder, and adding dilute hydrochloric acid into the materials to completely dissolve the materials so that a rare earth chloride solution is prepared, 2, at a room temperature, acutely stirring the rare earth chloride solution, ricinoleic acid and octadecene to obtain a microemulsion, slowly heating the microemulsion to remove water, carrying out stirring and naturally cooling the mixture to 50 DEG C, 3, keeping the temperature, slowly and dropwisely adding methanol solutions of sodium hydroxide and ammonium fluoride into the cooled product, carrying out stirring to obtain a microemulsion system and carrying out heating to remove methanol, and 4, feeding high purity argon (with purity of 99.999%) into the microemulsion system, carrying out fast heating, keeping the temperature for a certain time, carrying out natural cooling, adding excess cyclohexane into the microemulsion system, carrying out washing by a mixed solution of anhydrous ethanol and water, and carrying out vacuum drying to obtain light yellow powder. The method has the advantages of simple equipment, operation convenience, control easiness and high repetition rate. The product has the advantages of uniform product morphology, small product size, good dispersibility, pure hexagonal phase and strong green light (light purple light).
Description
Technical field
The present invention relates to a kind of method that six side's phase up-conversion nano materials prepared by ricinolic acid, be specially a kind of ricinolic acid and prepare six side phase NaYF
4: the method for Yb, Er and/or Tm, Ho up-conversion nano material, belongs to technical field of nanometer material preparation.
Background technology
Up-conversion luminescence nanomaterial refers to the solid chemical compound of doped with rare-earth elements, the metastable level of rare earth element is utilized to absorb multiple low-yield longer-wave photons, through multi-photon add and after launch high energy short-wave photons, thus making infrared light change visible ray into, this phenomenon and the Stokes law that we know are disagreed.Up-conversion luminescence nanomaterial generally comprises activator, sensitizing agent and matrix.NaYF
4be a kind of desirable upper conversion substrate material of discovered in recent years, main exist two kinds of crystalline structure as α-NaYF
4, β-NaYF
4, it is reported β-NaYF
4up-conversion luminescent material goes up one of the highest up-conversion luminescent material of efficiency of conversion up to now.Rare earth element er
3+there is abundant energy level and upper efficiency of conversion is high, the life-span is long, generally as the activator of up-conversion luminescence nanomaterial.And rare earth element y b
3+er can be passed to after absorbing energy
3+, be a kind of effective sensitizing agent.Rare earth nano material has stronger superiority in bio-imaging field because of the Upconversion luminescence of its uniqueness, as dark and little to biological tissue's damage in stable chemical nature, the high and low poison of signal to noise ratio, highly sensitive, lifeless matter background fluorescence interference, light penetration depth.The prerequisite of its biologic applications be obtain high quality, wetting ability, surface have can the up-conversion nanoparticles of functionalization functional group.
Common synthetic method utilizes the tensio-active agent of long alkyl chain such as Oleic Linoleic to control the coring and increment process of nanoparticle, to obtain the homogeneous nano material of pattern.Be all hydrophobic oleophilic oil as the up-conversion nanoparticles that hydrothermal method, thermal decomposition method etc. are synthesized, can only be dissolved in nonpolar organic solvent.As Zhang Yong seminar of Singapore utilizes the principle of low temperature nucleation high growth temperature, select oleic acid or linolic acid, successfully prepare hydrophobic up-conversion nanoparticles.Therefore, we utilize the principle of low temperature nucleation high growth temperature, ricinolic acid is selected to be tensio-active agent, successfully prepare the up-conversion nanoparticles of particle diameter about 40 nm, because its surface is with the hydroxyl of ricinolic acid part, effectively improve the wetting ability of up-conversion nanoparticles, and can make it can functionalization further, for its application at the biomedical sector such as biological monitoring, imaging is laid a good foundation.
Summary of the invention
The object of the invention is to provide a kind of Fast back-projection algorithm size controlled, pattern is homogeneous, good dispersity, the preparation method of six side's phase up-conversion nano materials that luminous is strong.
Concrete steps are:
(1) be 76 ~ 78:20: 2 ~ 4 take yttrium oxide, ytterbium oxide and Erbium trioxide powder according to Y:Yb:Er mol ratio, and to add mass percent concentration in mixed powder be that 1 ~ 5% dilute hydrochloric acid makes it to dissolve completely, be formulated as the rare-earth chlorination salts solution that concentration is 0.4 ~ 0.8 mol/L, described Erbium trioxide can part or all of oxidized thulium and/or Holmium trioxide replacement.
(2) at room temperature, vigorous stirring after the mixing of the rare-earth chlorination salts solution that 2 ml steps (1) are prepared, 6 ml chemical pure ricinolic acids and 15 ml chemical pure octadecylenes, form microemulsion phase, microemulsion phase is slowly warmed up to 100 DEG C of constant temperature to carry out dewatering 30 minutes to 120 ~ 140 DEG C after 10 minutes, then continues stirring and make it Temperature fall to 50 DEG C.
(3) 0.1 g sodium hydroxide and 0.148 g Neutral ammonium fluoride are dissolved in 10 ml anhydrous methanols make methanol solution.
Under (4) 50 DEG C of constant temperatures, in step (2) gains, slowly drip the methanol solution that step (3) makes, stir to form microemulsion system and heat up and remove methyl alcohol 30 minutes.
(5) in step (4) gains, pass into the high-purity argon gas 5 minutes that mass percent concentration is 99.999%, and rapid temperature increases to 300 ~ 330 DEG C, constant temperature is kept to make it naturally cooling after 1 ~ 2 hour, the chemical pure hexanaphthene adding 5 ~ 15ml when temperature drops to 80 DEG C makes product precipitate, cleaned 2 ~ 3 times with the mixing solutions of dehydrated alcohol and water respectively by throw out, vacuum-drying obtains the up-conversion nano material that pale yellow powder is pure six side's phases.
By the six side phase NaYF obtained
4: Yb, Er up-conversion nano material carries out transmission electron microscope (TEM), and X-ray diffraction analysis (XRD) and luminescent properties test characterize; Experimental result shows synthesized NaYF
4: Yb, Er, pattern is uniform six prisms, and size is about 40 nm, and crystalline phase is pure six side's phases, sends out green glow (pale purple light) strong.
The present invention is by rear-earth-doped, and selection ricinolic acid is tensio-active agent, and other solvent forms microemulsion system, and controllably the little pattern of synthesis particle size is even fast, productive rate is high, good dispersity, luminous six strong side phase NaYF
4: Yb, Er/Tm/Ho up-conversion nano material.The present invention can meet the demand of biological fluorescent labeling, bio-imaging, disease treatment material, for the biology practical application of up-conversion luminescent material is laid a good foundation.
Simple, easy to operate, the easy control of equipment required for the present invention, repetition rate are high; Product morphology is even, size is little, good dispersity, pure six side's phases, sends out green glow (pale purple light) strong.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 NaYF
4: the TEM figure of Yb, Er up-conversion nano material.
Fig. 2 is the embodiment of the present invention 1 NaYF
4: X-ray diffraction analysis (XRD) figure of Yb, Er up-conversion nano material.
Fig. 3 is the fluorescence spectrum figure of the embodiment of the present invention 1 NaYF4:Yb, Er up-conversion nano material, and in figure, illustration (a) is product NaYF
4: the fluorescence pictorial diagram of Yb, Er up-conversion nano material respectively in water and methylene dichloride under 980 nm excite (left: water, right: methylene dichloride).
Fig. 4 is the fluorescence spectrum figure of the embodiment of the present invention 2 NaYF4:Yb, Tm up-conversion nano material, and in figure, illustration (b) is product NaYF
4: the fluorescence pictorial diagram of Yb, Tm up-conversion nano material in central dispersion hexane under 980 nm laser excitations.
Fig. 5 is the fluorescence spectrum figure of the embodiment of the present invention 3 NaYF4:Yb, Ho up-conversion nano material, and in figure, illustration (c) is product NaYF
4: the fluorescence pictorial diagram of Yb, Ho up-conversion nano material in central dispersion hexane under 980 nm laser excitations.
Embodiment
Rare earth oxide of the present invention (ytterbium oxide, yttrium oxide, Erbium trioxide, trioxide, Holmium trioxide), ricinolic acid, Neutral ammonium fluoride, sodium hydroxide, octadecylene and methyl alcohol etc. are purchased from Shanghai Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment 1:
(1) be that 78:20:2 takes yttrium oxide, ytterbium oxide and Erbium trioxide powder according to Y:Yb:Er mol ratio, and in mixed powder, add mass percent concentration be that 3% dilute hydrochloric acid makes it to dissolve completely, be formulated as the rare-earth chlorination salts solution that concentration is 0.5 mol/L.
(2) at room temperature, vigorous stirring after the mixing of the rare-earth chlorination salts solution that 2 ml steps (1) are prepared, 6 ml chemical pure ricinolic acids and 15 ml chemical pure octadecylenes, form microemulsion phase, microemulsion phase is slowly warmed up to 100 DEG C of constant temperature to be warmed up to 140 DEG C after 10 minutes and to dewater 30 minutes, then continues stirring and make it Temperature fall to 50 DEG C.
(3) 0.1 g sodium hydroxide and 0.148 g Neutral ammonium fluoride are dissolved in 10 ml anhydrous methanols make methanol solution.
Under (4) 50 DEG C of constant temperatures, in step (2) gains, slowly drip the methanol solution that step (3) makes, stir to form microemulsion system and heat up and remove methyl alcohol 30 minutes.
(5) in step (4) gains, pass into the high-purity argon gas 5 minutes that mass percent concentration is 99.999%, and rapid temperature increases to 300 DEG C, constant temperature is kept to make it naturally cooling after 1 hour, the chemical pure hexanaphthene adding 10ml when temperature drops to 80 DEG C makes product precipitate, throw out is cleaned 2 times with the mixing solutions of dehydrated alcohol and water respectively, and vacuum-drying obtains the NaYF that pale yellow powder is pure six side's phases
4: Yb, Er up-conversion nano material.
NaYF as shown in Figure 1
4: the TEM figure of Yb, Er up-conversion nano material, show its favorable dispersity, size uniformity about 40 nm, pattern is uniform hexahedron.NaYF as shown in Figure 2
4: the XRD figure of Yb, Er up-conversion nano material, Fig. 2 display and six side's phase standard P DF cards (JCPDS 28-1192) consistent, illustrate that product is pure six side's phases.As shown in Figure 3 be NaYF
4: the fluorescence spectrum figure of Yb, Er up-conversion nano material, can see product NaYF from the illustration (a) of Fig. 3
4: Yb, Er have strong yellow green light in water, then do not have in methylene dichloride.
Embodiment 2:
(1) be that 78:20:2 takes yttrium oxide, ytterbium oxide and trioxide powder according to Y:Yb:Tm mol ratio, and in mixed powder, add mass percent concentration be that 3% dilute hydrochloric acid makes it to dissolve completely, be formulated as the rare-earth chlorination salts solution that concentration is 0.5 mol/L.
(2) at room temperature, vigorous stirring after the mixing of the rare-earth chlorination salts solution that 2 ml steps (1) are prepared, 6 ml chemical pure ricinolic acids and 15 ml chemical pure octadecylenes, form microemulsion phase, microemulsion phase is slowly warmed up to 100 DEG C of constant temperature to be warmed up to 140 DEG C after 10 minutes and to dewater 30 minutes, then continues stirring and make it Temperature fall to 50 DEG C.
(3) 0.1 g sodium hydroxide and 0.148 g Neutral ammonium fluoride are dissolved in 10 ml anhydrous methanols make methanol solution.
Under (4) 50 DEG C of constant temperatures, in step (2) gains, slowly drip the methanol solution that step (3) makes, stir to form microemulsion system and heat up and remove methyl alcohol 30 minutes.
(5) in step (4) gains, pass into the high-purity argon gas 5 minutes that mass percent concentration is 99.999%, and rapid temperature increases to 310 DEG C, constant temperature is kept to make it naturally cooling after 1.5 hours, the chemical pure hexanaphthene adding 15ml when temperature drops to 80 DEG C makes product precipitate, throw out is cleaned 3 times with the mixing solutions of dehydrated alcohol and water respectively, and vacuum-drying obtains the NaYF that pale yellow powder is pure six side's phases
4: Yb, Tm up-conversion nano material.
Product NaYF can be seen in the illustration (b) of Fig. 4
4: there is pale purple light in Yb, Tm.
Embodiment 3:
(1) be that 78:20:2 takes yttrium oxide, ytterbium oxide and Holmium trioxide powder according to Y:Yb:Ho mol ratio, and in mixed powder, add mass percent concentration be that 3% dilute hydrochloric acid makes it to dissolve completely, be formulated as the rare-earth chlorination salts solution that concentration is 0.5 mol/L.
(2) at room temperature, vigorous stirring after the mixing of the rare-earth chlorination salts solution that 2 ml steps (1) are prepared, 6 ml chemical pure ricinolic acids and 15 ml chemical pure octadecylenes, form microemulsion phase, microemulsion phase is slowly warmed up to 100 DEG C of constant temperature to be warmed up to 140 DEG C after 10 minutes and to dewater 30 minutes, then continues stirring and make it Temperature fall to 50 DEG C.
(3) 0.1 g sodium hydroxide and 0.148 g Neutral ammonium fluoride are dissolved in 10 ml anhydrous methanols make methanol solution.
Under (4) 50 DEG C of constant temperatures, in step (2) gains, slowly drip the methanol solution that step (3) makes, stir to form microemulsion system and heat up and remove methyl alcohol 30 minutes.
(5) in step (4) gains, pass into the high-purity argon gas 5 minutes that mass percent concentration is 99.999%, and rapid temperature increases to 300 DEG C, constant temperature is kept to make it naturally cooling after 1.5 hours, the chemical pure hexanaphthene adding 15ml when temperature drops to 80 DEG C makes product precipitate, throw out is cleaned 2 times with the mixing solutions of dehydrated alcohol and water respectively, and vacuum-drying obtains the NaYF that pale yellow powder is pure six side's phases
4: Yb, Ho up-conversion nano material.
Visible product NaYF in the illustration (c) of Fig. 5
4: there is strong green glow in Yb, Ho.
Embodiment 4:
(1) be that 76:20:2:1:1 takes yttrium oxide, ytterbium oxide, Erbium trioxide, trioxide and Holmium trioxide powder according to Y:Yb:Er:Tm:Ho mol ratio, and to add mass percent concentration in mixed powder be that 3% dilute hydrochloric acid makes it to dissolve completely, be formulated as the rare-earth chlorination salts solution that concentration is 0.5 mol/L.
(2) at room temperature, vigorous stirring after the mixing of the rare-earth chlorination salts solution that 2 ml steps (1) are prepared, 6 ml chemical pure ricinolic acids and 15 ml chemical pure octadecylenes, form microemulsion phase, microemulsion phase is slowly warmed up to 100 DEG C of constant temperature to be warmed up to 140 DEG C after 10 minutes and to dewater 30 minutes, then continues stirring and make it Temperature fall to 50 DEG C.
(3) 0.1 g sodium hydroxide and 0.148 g Neutral ammonium fluoride are dissolved in 10 ml anhydrous methanols make methanol solution.
Under (4) 50 DEG C of constant temperatures, in step (2) gains, slowly drip the methanol solution that step (3) makes, stir to form microemulsion system and heat up and remove methyl alcohol 30 minutes.
(5) in step (4) gains, pass into the high-purity argon gas 5 minutes that mass percent concentration is 99.999%, and rapid temperature increases to 300 DEG C, constant temperature is kept to make it naturally cooling after 1 hour, the chemical pure hexanaphthene adding 10ml when temperature drops to 80 DEG C makes product precipitate, throw out is cleaned 2 times with the mixing solutions of dehydrated alcohol and water respectively, and vacuum-drying obtains the NaYF that pale yellow powder is pure six side's phases
4: Yb, Er/Tm/Ho up-conversion nano material.
Claims (1)
1. a method for six side's phase up-conversion nano materials prepared by ricinolic acid, it is characterized in that concrete steps are:
(1) be 76 ~ 78:20: 2 ~ 4 take yttrium oxide, ytterbium oxide and Erbium trioxide powder according to Y:Yb:Er mol ratio, and to add mass percent concentration in mixed powder be that 1 ~ 5% dilute hydrochloric acid makes it to dissolve completely, be formulated as the rare-earth chlorination salts solution that concentration is 0.4 ~ 0.8 mol/L, the described Erbium trioxide part or all of oxidized thulium of energy and/or Holmium trioxide are replaced;
(2) at room temperature, vigorous stirring after the mixing of the rare-earth chlorination salts solution that 2 ml steps (1) are prepared, 6 ml chemical pure ricinolic acids and 15 ml chemical pure octadecylenes, form microemulsion phase, microemulsion phase is slowly warmed up to 100 DEG C of constant temperature to carry out dewatering 30 minutes to 120 ~ 140 DEG C after 10 minutes, then continues stirring and make it Temperature fall to 50 DEG C;
(3) 0.1 g sodium hydroxide and 0.148 g Neutral ammonium fluoride are dissolved in 10 ml anhydrous methanols make methanol solution;
Under (4) 50 DEG C of constant temperatures, in step (2) gains, slowly drip the methanol solution that step (3) makes, stir to form microemulsion system and heat up and remove methyl alcohol 30 minutes;
(5) in step (4) gains, pass into the high-purity argon gas 5 minutes that mass percent concentration is 99.999%, and rapid temperature increases to 300 ~ 330 DEG C, constant temperature is kept to make it naturally cooling after 1 ~ 2 hour, the chemical pure hexanaphthene adding 5 ~ 15ml when temperature drops to 80 DEG C makes product precipitate, cleaned 2 ~ 3 times with the mixing solutions of dehydrated alcohol and water respectively by throw out, vacuum-drying obtains the up-conversion nano material that pale yellow powder is pure six side's phases.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060130741A1 (en) * | 2001-07-30 | 2006-06-22 | Xiaogang Peng | High quality colloidal nanocrystals and methods of preparing the same in non-coordinating solvents |
| CN102030356A (en) * | 2010-10-26 | 2011-04-27 | 北京化工大学 | Method for preparing polychromatic luminous nanocrystalline of monodisperse NaYF4 |
| CN102154012A (en) * | 2011-03-01 | 2011-08-17 | 吉林大学 | Preparation method of small-sized NaYF4 nano substrate material with hexagonal phase by inducement |
| CN103450875A (en) * | 2013-08-30 | 2013-12-18 | 中国科学院化学研究所 | 800-nanometer continuous laser excited rare earth upconversion nanoparticles (UCNPs), and preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060130741A1 (en) * | 2001-07-30 | 2006-06-22 | Xiaogang Peng | High quality colloidal nanocrystals and methods of preparing the same in non-coordinating solvents |
| CN102030356A (en) * | 2010-10-26 | 2011-04-27 | 北京化工大学 | Method for preparing polychromatic luminous nanocrystalline of monodisperse NaYF4 |
| CN102154012A (en) * | 2011-03-01 | 2011-08-17 | 吉林大学 | Preparation method of small-sized NaYF4 nano substrate material with hexagonal phase by inducement |
| CN103450875A (en) * | 2013-08-30 | 2013-12-18 | 中国科学院化学研究所 | 800-nanometer continuous laser excited rare earth upconversion nanoparticles (UCNPs), and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 何本钊: "聚合物/稀土上转换发光纳米杂化材料的制备及性能研究", 《中国优秀硕士论文全文数据库，工程科技Ⅰ辑》 * |
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Application publication date: 20150819 |