Method for preparing gadolinium ion doped lutetium sodium fluoride upconversion nano/micro crystal

A technique of sodium lutetium fluoride and ion doping, applied to chemical instruments and methods, luminescent materials, etc., to achieve the effect of enhanced up-conversion red light intensity, simple equipment, and easy operation

Inactive Publication Date: 2015-11-18
SUN YAT SEN UNIV
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Problems solved by technology

However, the current doping of NaLuF by Gd ions 4 The study of up-converting nano / micro crystals to specifically improve their red light luminous efficiency has not been reported yet.

Method used

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  • Method for preparing gadolinium ion doped lutetium sodium fluoride upconversion nano/micro crystal
  • Method for preparing gadolinium ion doped lutetium sodium fluoride upconversion nano/micro crystal
  • Method for preparing gadolinium ion doped lutetium sodium fluoride upconversion nano/micro crystal

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preparation example Construction

[0023] A method for preparing gadolinium ion-doped lutetium sodium fluoride up-conversion nano / micro-crystals with red light enhancement effect proposed by the present invention, specifically comprises the following steps:

[0024] 1) Mix the citric acid solution with deionized water, and after magnetic stirring, add lutetium nitrate, ytterbium nitrate, erbium nitrate, thulium nitrate, gadolinium nitrate solution in sequence, after stirring evenly, add sodium fluoride solution, and add the corresponding deionized Water, a white turbid liquid is formed after thorough stirring;

[0025] 2) Transfer the turbid liquid to a stainless steel reaction kettle with a liner for hydrothermal reaction;

[0026] 3) Centrifuge, wash, and dry the turbid liquid after the reaction in sequence to obtain the final product.

[0027] In this embodiment, in step 1), lutetium nitrate, ytterbium nitrate, gadolinium nitrate, erbium nitrate and thulium nitrate are dissolved in dilute nitric acid (30%) ...

Embodiment 1

[0032] Preparation of Gd ion-doped cubic NaLuF by hydrothermal method 4 Nanocrystalline.

[0033] Mix 1.5 ml of 2M citric acid solution with 10 ml of deionized water, and after magnetic stirring for 10 minutes, add (0.64 ml / 0.44 ml / 0.24 ml) 1M lutetium nitrate solution, 0.4 ml of 0.5M ytterbium nitrate solution, 1.5 ml of 0.1 M erbium nitrate solution, 0.1 mL 0.1 M thulium nitrate solution and (0 mL / 0.2 mL / 0.4 mL) 1M gadolinium nitrate solution, after 30 min magnetic stirring, 6 mL 1M sodium fluoride solution, and 10 mL deionized water, a white cloudy liquid was formed after stirring thoroughly for 30 minutes. The turbid liquid was transferred to a stainless steel reactor with a liner for hydrothermal reaction, the reaction temperature and time were 180°C and 12 hours, respectively. The cloudy solution after the reaction was centrifuged twice at 10,000 rpm, washed with deionized water and alcohol respectively, and finally dried at 60°C for 12 hours to obtain the product.

...

Embodiment 2

[0036] Preparation of Gd ion-doped mixed-phase NaLuF by hydrothermal method 4 crystals.

[0037] Mix 1.5 ml of 2M citric acid solution with 10 ml of deionized water, and after magnetic stirring for 10 minutes, add (0.64 ml / 0.44 ml / 0.24 ml / 0.04 ml) 1M lutetium nitrate solution, 0.4 ml 0.5M ytterbium nitrate solution, 1.5 ml of 0.1M erbium nitrate solution, 0.1 ml of 0.1M thulium nitrate solution and (0 ml / 0.2 ml / 0.4 ml / 0.6 ml) 1M gadolinium nitrate solution, after 30 minutes of magnetic stirring, add 8 ml of 1M sodium fluoride solution, And add 8 milliliters of deionized water, after fully stirring for 30 minutes, a white turbid solution is formed. The turbid liquid was transferred to a stainless steel reactor with a liner for hydrothermal reaction, the reaction temperature and time were 180°C and 12 hours, respectively. The cloudy solution after the reaction was centrifuged twice at 10,000 rpm, washed with deionized water and alcohol respectively, and finally dried at 60°C f...

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Abstract

The invention discloses a method for preparing a gadolinium ion doped lutetium sodium fluoride upconversion nano / micro crystal with a red light enhancement effect. The method comprises the steps that a citric acid solution and deionized water are mixed and magnetically stirred, then lutetium nitrate, ytterbium nitrate, erbium nitrate, thulium nitrate and gadolinium nitrate solutions are sequentially added, a sodium fluoride solution is added after even stirring, corresponding deionized water is added, and a white turbid solution is formed after full stirring; the turbid solution is transferred to a stainless steel reaction still with a bush to be subjected to a hydrothermal reaction; the reacted turbid solution is centrifuged, washed and dried to obtain the final product. The gadolinium ion doped lutetium sodium fluoride upconversion nano / micro crystal with the red light enhancement effect is prepared. The obtained material is good in dispersity, the upconversion red light intensity is greatly increased, and wide application prospects are achieved in the fields of biology, photovoltaics, display, infrared detection and the like. Equipment required by the preparation method is simple, operation and popularization are easy, and the method is suitable for large-scale production.

Description

technical field [0001] The invention relates to the field of luminescent materials, in particular to a method for preparing gadolinium ion-doped lutetium sodium fluoride up-conversion nano / micro crystals with red light enhancement effect. Background technique [0002] Rare-earth-doped upconversion luminescence is a process that converts low-energy photons into high-energy photons. Rare earth-doped upconversion luminescent materials have important potential applications in laser, display, photovoltaic, biological detection and other fields due to their low toxicity, photostability and high color purity. Because the red light band (600-700nm) can penetrate biological tissues well, this band is called "bio-optical window". However, the quantum yield of current upconversion luminescent materials is relatively low, which greatly restricts their practical application. At present, several methods can be used to improve the upconversion luminescence intensity of fluorescent materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 张曰理林浩阳生红徐德康李安明
Owner SUN YAT SEN UNIV
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