Oil soluble nanometer scintillation crystal and preparation method thereof

A scintillation crystal, oil-soluble technology, applied in nanotechnology, crystal growth, nano-optics and other directions, can solve the problems of lack of high-quality nano-scintillation crystals, poor uniformity of crystal composition distribution, reduced crystal scintillation performance, etc., to achieve good scintillation performance. , the preparation method is simple and easy to implement, and the effect of reducing the detection cost

Inactive Publication Date: 2016-06-01
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned patents have obvious defects and deficiencies: First, the prepared cerium-doped lanthanum chloride bromide solid solution single crystal is a large-sized single crystal, and the distribution uniformity of crystal components is poor, which directly reduces the scintillation performance of the crystal. When the crystal size is reduced to nanometer After the size is increased, the distribution of crystal components is more uniform, which can improve the scintillation performance and stability of the crystal; the second is that the scintillation crystal is doped with cerium, which leads to weak fluorescence emission intensity of the scintillation crystal after X-ray excitation, and the fluorescence emission wavelength is short , the emission of short-wavelength fluorescence is easily hindered; third, the preparation method is complicated, and the crucible drop method requires high equipment precision and process parameters, which is difficult to control
Up to now, there are few reports on nano-scintillation crystals, the key reason is the lack of a simple, controllable, batch-ready method for preparing high-quality nano-scintillation crystals

Method used

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  • Oil soluble nanometer scintillation crystal and preparation method thereof
  • Oil soluble nanometer scintillation crystal and preparation method thereof
  • Oil soluble nanometer scintillation crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1La 0.9 f 3 :Tb 0.1 Oil-soluble nano-scintillation crystals

[0033] 1) Weigh 0.9mmol LaCl 3 ·7H 2 O and 0.1 mmol TbCl 3 ·6H 2 O, add 10ml of oleic acid and 8ml of octadecene to it, first raise the temperature to 100°C, then raise the temperature to 160°C under an argon atmosphere, and stir for 1h to obtain solution A;

[0034] 2) Solution A is cooled to room temperature, and 3 mmol NH 4 10ml of methanol solution of F, control the rotating speed of the peristaltic pump, and adjust the dropping rate to be 0.3ml / min to obtain solution B;

[0035] 3) Solution B was stirred and reacted at room temperature for 1 hour, then heated to 70°C, vacuumed to remove methanol, heated to 280°C at 10°C / min in an argon atmosphere, and reacted for 60 minutes to obtain a mixed liquid of oil-soluble nano-scintillation crystals;

[0036] 4) The oil-soluble nano-scintillation crystal mixture was cooled to room temperature, and then 3 times the volume of ethanol was added to th...

Embodiment 2

[0038] Example 2La 0.3 f 3 : Ce 0.6 Tb 0.1 Oil-soluble nano-scintillation crystals

[0039] 1) Weigh 0.3mmol LaCl 3 ·7H 2 O, 0.6mmol CeCl3 ·7H 2 O and 0.1 mmol TbCl 3 ·6H 2 O, add 12ml of oleic acid and 8ml of octadecene to it, first raise the temperature to at least 100°C, then raise the temperature to at least 160°C under an argon atmosphere, and stir for at least 1h to obtain solution A;

[0040] 2) Solution A is cooled to room temperature, and 3 mmol NH 4 F methanol solution 10ml, control the rotating speed of the peristaltic pump, adjust the dropping rate to be 0.8ml / min, obtain solution B;

[0041] 3) Solution B was stirred and reacted at room temperature for at least 1 hour, then heated to at least 70°C, vacuumed to remove methanol, heated to 260°C at 15°C / min in an argon atmosphere, and reacted for 120 minutes to obtain a mixed liquid of oil-soluble nano-scintillation crystals ;

[0042] 4) The oil-soluble nano-scintillation crystal mixture was cooled to roo...

Embodiment 3

[0043] Example 3La 0.8 f 3 :Tb 0.2 Oil-soluble nano-scintillation crystals

[0044] 1) Weigh 0.8mmol LaCl 3 ·7H 2 O and 0.2 mmol TbCl 3 ·6H 2 O, add 7ml of oleic acid and 8ml of octadecene to it, first raise the temperature to 100°C, then raise the temperature to 160°C under a nitrogen atmosphere, and stir for 1h to obtain solution A;

[0045] 2) Solution A is cooled to room temperature, and 3 mmol NH 4 10ml of methanol solution of F, control the rotating speed of the peristaltic pump, and adjust the dropping rate to be 0.5ml / min to obtain solution B;

[0046] 3) Solution B was stirred and reacted at room temperature for 1 hour, then heated to 70°C, vacuumed to remove methanol, heated to 280°C at 8°C / min under nitrogen atmosphere, and reacted for 80 minutes to obtain a mixed liquid of oil-soluble nano-scintillation crystals;

[0047] 4) The oil-soluble nano-scintillation crystal mixture was cooled to room temperature, and then 3 times the volume of ethanol was added to...

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Abstract

The invention relates to an oil soluble nanometer scintillation crystal and a preparation method thereof.LaCl3 and RECl3 lanthanide compounds are heated under the inert gas shielding and dissolved into an oleic acid and octadecene mixed solution, a NH4F methanol solution is added dropwisely at uniform speed on the stirring condition, a reaction is performed for 10-120 min at the temperature of 260-320 DEG C after methyl alcohol is removed, the oil soluble nanometer scintillation crystal with the average grain size being 4-10 nanometers is obtained, RE is the lanthanide Tb or lanthanides Tb and Ce, the oil soluble nanometer scintillation crystal of different fluorescence emission strengths is obtained by changing the varieties and / or ratio of the LaCl3 and the RECle lanthanide compounds, and the obtained oil soluble nanometer scintillation crystal has the advantages of being high in fluorescence intensity and good in fluorescence stability under X-ray irradiation excitation, and can be widely applied to the fields of biological medicine, material science and the like.

Description

technical field [0001] The invention relates to an oil-soluble nano-scintillation crystal and a preparation method thereof, belonging to the technical field of chemiluminescent materials. Background technique [0002] Scintillation crystals are a class of materials that can absorb high-energy rays and convert the energy into ultraviolet or visible photons. They are widely used in optical devices, nuclear medicine, nuclear detection and military fields. Chinese patent "A preparation method of cerium-doped lanthanum chloride bromide scintillation crystal", publication number: 102230215A, publication date: 2011-11-02, discloses a method using SOCl 2 with LaCl 3 ·7H 2 O, Ce 7H 2 Prepare cerium-doped lanthanum chloride bromide solid solution polycrystals with an aqueous solution of lanthanide compounds such as O, and then prepare cerium-doped lanthanum chloride bromide solid solution single crystals by using the crucible descent method. However, the above-mentioned patents ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85B82Y20/00B82Y40/00C30B29/12C30B7/14
CPCC09K11/7772B82Y20/00B82Y40/00C30B7/14C30B29/12
Inventor 杨祥良胡军唐永安
Owner HUAZHONG UNIV OF SCI & TECH
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