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
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[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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