CN110184648B - Method for preparing rare earth doped sodium yttrium tungstate crystal for quantitative calibration of substances - Google Patents
Method for preparing rare earth doped sodium yttrium tungstate crystal for quantitative calibration of substances Download PDFInfo
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- CN110184648B CN110184648B CN201910645710.2A CN201910645710A CN110184648B CN 110184648 B CN110184648 B CN 110184648B CN 201910645710 A CN201910645710 A CN 201910645710A CN 110184648 B CN110184648 B CN 110184648B
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Abstract
The invention discloses a method for preparing rare earth doped sodium yttrium tungstate crystal and applying the crystal to a laser crystal LA-ICP-MS micro-area analysis quantitative calibration substance, and specifically comprises the step of firstly preparing Na2CO3、Y2O3、WO3And mixing with other rare earth oxide powder, adding absolute ethyl alcohol, fully grinding the raw materials, transferring the raw materials into a crucible, placing the crucible in a muffle furnace for high-temperature sintering, carrying out high-temperature solid-phase reaction, and finally finishing crystal growth in a micro-pulling down crystal growth furnace to obtain the rare earth doped sodium yttrium tungstate crystal. The crystal material obtained by the invention has good compactness, transparent color and luster, no chromatic aberration and good distribution uniformity of the doped rare earth elements, and can be used as a LA-ICP-MS micro-area analysis quantitative calibration substance of the rare earth doped laser crystal material.
Description
Technical Field
The invention relates to the field of microelement micro-area analytical chemistry, in particular to a method for preparing rare earth doped sodium yttrium tungstate crystal and using the rare earth doped sodium yttrium tungstate crystal for LA-ICP-MS quantitative micro-area analysis of a laser crystal material.
Background
The laser crystal is a core component of the laser, and the working performance of the laser crystal can be improved by doping rare earth ions in the laser crystal. If the concentration and distribution information of the rare earth ions in the laser crystal can be accurately measured, scientific basis can be provided for detection and production of the laser crystal.
The quantitative correction of the rare earth elements in the laser crystal is a key technical problem influencing the analysis result, and the key point is to develop a LA-ICP-MS quantitative correction standard matched with a crystal sample matrix. However, such standard/reference materials are still lacking at home and abroad, and current research work can only use non-matrix-matched silicate calibration standards (such as NIST SRM 610 and the like) for quantitative calibration, which inevitably introduces systematic errors. It can be seen that the key scientific problem of adopting LA-ICP-MS to carry out accurate micro-area analysis on rare earth trace elements in a laser crystal sample is to prepare a LA-ICP-MS micro-area quantitative analysis correction standard matched with a laser crystal matrix.
Disclosure of Invention
Aiming at the problems, the invention synthesizes the rare earth doped sodium yttrium tungstate crystal by a crystal growth furnace (namely a micro-descending crystal growth furnace). The crystal obtained by the method has good compactness, transparent color and luster, no chromatic aberration and good distribution uniformity of the doped rare earth elements, and can be used as a LA-ICP-MS micro-area analysis quantitative calibration substance of a rare earth doped laser crystal material.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
(1) preparation of Na2CO3、Y2O3、WO3And other rare earth oxide powder mixtures except yttrium are placed in a mortar, and the powder mixture is fully ground after absolute ethyl alcohol is added;
(2) transferring the powder sample obtained in the step (1) into a crucible, putting the crucible into a muffle furnace for calcination, heating the powder sample from room temperature to 600-800 ℃ at a heating rate of 5-10 ℃/min, and keeping the temperature for a preset time; heating to 1000-1200 ℃ at the same speed, keeping the temperature for 12-24 hours to complete the high-temperature solid-phase reaction, and finally cooling to room temperature;
(3) transferring the calcined sample obtained in the step (2) into a crucible of a micro-pull-down crystal growth furnace, and completing crystal growth through the steps of charging, heating, seeding, isometric growth, pulling-off and cooling to obtain the rare earth doped sodium yttrium tungstate crystal which is used for laser crystal LA-ICP-MS micro-area analysis quantitative calibration substances.
Preferably, the doping proportion of the other rare earth oxides except yttrium in the step (1) is 0.01-0.1%.
Preferably, the anhydrous ethanol immersing the powder mixture is added to the mortar in the step (1).
Preferably, the muffle furnace temperature in the step (2) is specifically set as follows: heating from room temperature to 700 deg.C at a heating rate of 5 deg.C/min, holding the temperature for 6 hr, heating from 700 deg.C to 1000 deg.C at the same rate of 5 deg.C/min, holding the temperature for 12 hr, and cooling to room temperature.
Preferably, the high-temperature solid-phase reaction in the step (2) is as follows:
Na2CO3+xRE2O3+(1-x)Y2O3+4WO3＝2NaRExY(1-x)(WO4)2+CO2↑。
preferably, the micro-pulling-down crystal growth furnace program in the step (3) is set as follows: the temperature-raising power is from 0W to 1500-1800W, the temperature-raising time is 8-12 h, then the temperature-raising power is increased to 2000W again in a program-controlled manner, the temperature-raising time is 1-5 h, when the melting liquid appears in the crucible of the micro-pulling crystal generation furnace, the program-controlled temperature-raising is stopped, and NaY (WO) is used4)2Seeding the seed crystal; during crystal growth, increasing power by program control at a rate of 1-3W/h to enable the crystal to grow in an equal diameter way for 24-48 h; after the melt in the crucible is completely crystallized, pulling off the crystal; the cooling program is set as follows: 2000-2500W to 0W, and the use time is 20-30 h.
Preferably, the program of the micro-descending crystal growth furnace in the step (3) is set as follows: the temperature-rising power is from 0W to 1700W, the time of use is 10h, the power of the seeding process is raised to 1800W, the program-controlled temperature-rising power is set again from 1800W to 2000W, the time of use is 2h, when the power is 1960W, the appearance of liquid flow is observed, the program-controlled temperature rise is stopped, and the seeding is carried out by using seed crystals; when the crystal grows, the power is increased by program control at the rate of 1.3W/h to ensure that the crystal grows in an equal diameter way for 48 h; after the material in the crucible is completely fed, pulling off the crystal; the cooling program is set as follows: 2050W to 1300W, 10h in use, 1300W to 0W and 10h in use.
Preferably, the rare earth doped sodium yttrium tungstate crystal synthesized in the step (3) is in a strip shape, the length is 10-30 mm, and the width is 1-5 mm.
Preferably, the length of the rare earth doped sodium yttrium tungstate crystal synthesized in the step (3) is 25mm, and the width of the rare earth doped sodium yttrium tungstate crystal is 3 mm.
Compared with the prior art, the technical scheme adopted by the invention at least has the following advantages:
1. the rare earth doped sodium yttrium tungstate crystal matrix prepared by the invention is composed of sodium yttrium tungstate, and the error caused by matrix mismatching in LA-ICP-MS detection is avoided.
2. The crystal material obtained by the invention has good compactness, and the edge of the laser ablation pit has no obvious collapse and melting phenomena.
3. The rare earth element in the rare earth doped sodium yttrium tungstate crystal prepared by the invention has good distribution uniformity and meets the requirement of being used as a calibration substance.
Drawings
FIG. 1 is a physical diagram of the rare earth doped sodium yttrium tungstate crystal in example 1.
FIG. 2 is an XRD pattern of the rare earth doped sodium yttrium tungstate crystal in example 1.
FIG. 3 is a line scanning signal diagram of a representative rare earth element LA-ICP-MS in the rare earth-doped sodium yttrium tungstate crystal in example 1.
Detailed Description
The present invention will be further illustrated by the following examples, but is not limited thereto.
Example 1
A method for preparing rare earth doped sodium yttrium tungstate crystal and using the rare earth doped sodium yttrium tungstate crystal for LA-ICP-MS micro-area analysis quantitative calibration material of laser crystal material comprises the following specific steps:
(1) respectively weighing 0.0016g of lanthanum oxide, cerium oxide and praseodymium oxide, 0.0017g of neodymium oxide and samarium oxide, 0.0018g of europium oxide, gadolinium oxide, terbium oxide and dysprosium oxide, 0.0019g of holmium oxide, erbium oxide and thulium oxide, 0.0020g of ytterbium oxide and lutetium oxide, 1.1132g of yttrium oxide, 0.5352g of anhydrous sodium carbonate and 4.6370g of tungsten trioxide; grinding the weighed medicines for 1h, and dripping a plurality of drops of alcohol into an agate mortar during grinding to ensure that the medicines are fully ground and mixed;
(2) and transferring the fully ground medicine into a clean corundum crucible, and then performing high-temperature calcination by using a muffle furnace to finish the high-temperature solid-phase reaction. Muffle furnace temperature was set to: heating to 700 deg.C at 5 deg.C/min, holding the temperature for 12 hr, heating from 700 deg.C to 1000 deg.C at the same speed of 5 deg.C/min, holding the temperature for 12 hr, and cooling to room temperature to obtain the final product;
(3) transferring the calcined medicine into a crucible of a micro-pulling-down crystal growth furnace for charging, carrying out crystal growth operation, and setting the program of the micro-pulling-down crystal growth furnace: setting the programmed heating power from 0W to 1700W, heating for 10h, after the seeding process power is raised to 1800W, setting the programmed heating power from 1800W to 2000W again, using the power for 2h, when the power is 1960W, observing the occurrence of liquid flow, stopping the programmed heating, and using the seed crystal to perform seeding. When the crystal grows, the power is programmed and increased at the rate of 1.3W/h to ensure that the crystal grows for 48h in an equal diameter way. After the material in the crucible is completely fed, the crystal is pulled off. The temperature reduction program is set to be 2050W to 1300W, and the time is 10 h; 1300W to 0W, and 10 h.
The physical diagram of the rare earth doped sodium yttrium tungstate crystal prepared in the embodiment is shown in fig. 1, and it can be found that the prepared rare earth doped sodium yttrium tungstate crystal has uniform color and no obvious color difference.
The XRD pattern of the rare earth doped sodium yttrium tungstate crystal prepared in this example is shown in FIG. 2, and it can be seen from FIG. 2 that the chemical composition of the matrix of the synthesized crystal is sodium yttrium tungstate.
LA-ICP-MS test: and (3) after the synthesized crystal is subjected to target making, grinding and polishing, and after all indexes of the instrument are tuned to be normal, performing a line scanning denudation analysis test on the synthesized crystal sample. In the case of line scan ablation analysis, the laser ablation spot diameter was 60 μm and the line scan rate was 10 μm · s-1The gas background acquisition time is 20s, the sample signal acquisition time is 160s, and the obtained LA-ICP-MS line scanning signal diagram of the rare earth doped calcium tungstate crystal is shown in FIG. 3, it can be known from FIG. 3 that the signal curve of each rare earth element is smooth, and the relative standard deviation of the element signal intensity ratio of each rare earth element after internal standard correction is less than 10%, which indicates that the distribution uniformity of the rare earth elements in the calcium tungstate crystal is good.
Example 2
A method for preparing rare earth doped sodium yttrium tungstate crystal and using the rare earth doped sodium yttrium tungstate crystal for LA-ICP-MS micro-area analysis quantitative calibration material of laser crystal material comprises the following specific steps:
(1) respectively weighing 0.0048g of lanthanum oxide, cerium oxide and praseodymium oxide, 0.0051g of neodymium oxide and samarium oxide, 0.0054g of europium oxide, gadolinium oxide, terbium oxide and dysprosium oxide, 0.0057g of holmium oxide, erbium oxide and thulium oxide, 0.0060g of ytterbium oxide and lutetium oxide, 1.1132g of yttrium oxide, 0.5352g of anhydrous sodium carbonate and 4.6370g of tungsten trioxide; grinding the weighed medicines for 1h, adding absolute ethyl alcohol for immersing the medicines into an agate mortar during grinding, and grinding for one and a half hours to ensure that the medicines are fully ground and mixed;
(2) and transferring the fully ground medicine into a clean corundum crucible, and then performing high-temperature calcination by using a muffle furnace to finish the high-temperature solid-phase reaction. Muffle furnace temperature was set to: heating to 750 deg.C at 8 deg.C/min, holding the temperature for 12 hr, heating from 750 deg.C to 1100 deg.C at the same speed of 8 deg.C/min, holding the temperature for 14 hr, and cooling to room temperature to take out the medicine;
(3) transferring the calcined medicine into a crucible of a micro-pulling-down crystal growth furnace for charging, carrying out crystal growth operation, and setting the program of the micro-pulling-down crystal growth furnace: setting the programmed heating power from 0W to 1600W, heating for 9h, setting the programmed heating power from 1800W to 2000W again after the seeding process power is raised to 1800W, stopping the programmed heating when the melting liquid appears in the crucible of the micro-pulling crystal generation furnace for 2h, and using NaY (WO)4)2And (5) seed crystal seeding removal. When the crystal grows, the power is programmed and increased at the rate of 2W/h to ensure that the crystal grows for 36h in an isodiametric way. And pulling out the crystal when the melt in the crucible is completely crystallized. The temperature reduction program is set to be 2250W to 0W, and the time is 36h, so that the rare earth doped sodium yttrium tungstate crystal is prepared and used for LA-ICP-MS quantitative micro-area analysis of the laser crystal material.
Claims (8)
1. A preparation method of rare earth doped sodium yttrium tungstate crystal for laser crystal LA-ICP-MS micro-area analysis quantitative calibration substance is characterized by comprising the following steps:
(1) preparation of Na2CO3、Y2O3、WO3And other rare earth oxide powder mixtures other than yttrium,placing the powder mixture in a mortar, adding absolute ethyl alcohol, and fully grinding the powder mixture, wherein the other rare earth oxides except yttrium are lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide and lutetium oxide;
(2) transferring the powder sample obtained in the step (1) into a crucible, putting the crucible into a muffle furnace for calcination, heating the powder sample from room temperature to 600-800 ℃ at a heating rate of 5-10 ℃/min, and keeping the temperature for a preset time; heating to 1000-1200 ℃ at the same speed, keeping the temperature for 12-24 hours to complete the high-temperature solid-phase reaction, and finally cooling to room temperature;
(3) transferring the calcined sample obtained in the step (2) into a crucible of a micro-pull-down crystal growth furnace, and completing crystal growth through the steps of charging, heating, seeding, isometric growth, pulling-off and cooling to obtain a rare earth doped sodium yttrium tungstate crystal which is used for laser crystal LA-ICP-MS micro-area analysis quantitative calibration material;
the program of the micro-pulling-down crystal growth furnace in the step (3) is set as follows: the temperature-raising power is from 0W to 1500-1800W, the temperature-raising time is 8-12 h, then the temperature-raising power is increased to 2000W again in a program-controlled manner, the temperature-raising time is 1-5 h, when the melting liquid appears in the crucible of the micro-pulling crystal generation furnace, the program-controlled temperature-raising is stopped, and NaY (WO) is used4)2Seeding the seed crystal; during crystal growth, increasing power by program control at a rate of 1-3W/h to enable the crystal to grow in an equal diameter way for 24-48 h; after the melt in the crucible is completely crystallized, pulling off the crystal; the cooling program is set as follows: 2000-2500W to 0W, and the use time is 20-30 h.
2. The preparation method of the rare earth doped sodium yttrium tungstate crystal for the laser crystal LA-ICP-MS micro-area analysis quantitative calibration substance, as claimed in claim 1, wherein the doping proportion of other rare earth oxides except yttrium in the step (1) is 0.01% -0.1%.
3. The method for preparing a rare earth doped sodium yttrium tungstate crystal for laser crystal LA-ICP-MS micro-domain analysis quantitative calibration substance as claimed in claim 1, wherein absolute ethyl alcohol for immersing the powder mixture is added into the mortar in the step (1).
4. The preparation method of the rare earth doped sodium yttrium tungstate crystal for the laser crystal LA-ICP-MS micro-area analysis quantitative calibration substance as claimed in claim 1, wherein the muffle furnace temperature in the step (2) is specifically set as follows: heating from room temperature to 700 deg.C at a heating rate of 5 deg.C/min, holding the temperature for 6 hr, heating from 700 deg.C to 1000 deg.C at the same rate of 5 deg.C/min, holding the temperature for 12 hr, and cooling to room temperature.
5. The preparation method of the rare earth doped sodium yttrium tungstate crystal for the laser crystal LA-ICP-MS micro-area analysis quantitative calibration substance as claimed in claim 1, wherein the high temperature solid phase reaction in the step (2) is as follows:
Na2CO3+ xRE2O3+ (1-x)Y2O3+ 4WO3=2 NaRE x Y x(1-) (WO4)2+CO2↑。
6. the method for preparing the rare earth doped sodium yttrium tungstate crystal for the laser crystal LA-ICP-MS micro-area analysis quantitative calibration substance as claimed in claim 1, wherein the micro-pulling-down crystal growth furnace program in the step (3) is set as follows: the temperature-rising power is from 0W to 1700W, the time of use is 10h, the power of the seeding process is raised to 1800W, the program-controlled temperature-rising power is set again from 1800W to 2000W, the time of use is 2h, when the power is 1960W, the appearance of liquid flow is observed, the program-controlled temperature rise is stopped, and the seeding is carried out by using seed crystals; when the crystal grows, the power is increased by program control at the rate of 1.3W/h to ensure that the crystal grows in an equal diameter way for 48 h; after the material in the crucible is completely fed, pulling off the crystal; the cooling program is set as follows: 2050W to 1300W, 10h in use, 1300W to 0W and 10h in use.
7. The preparation method of the rare earth doped sodium yttrium tungstate crystal for the laser crystal LA-ICP-MS micro-area analysis quantitative calibration substance, as claimed in claim 1, wherein the rare earth doped sodium yttrium tungstate crystal synthesized in the step (3) is in a strip shape, the length is 10-30 mm, and the width is 1-5 mm.
8. The method for preparing a rare earth doped sodium yttrium tungstate crystal for laser crystal LA-ICP-MS micro-area analysis quantitative calibration substance according to claim 7, wherein the length of the rare earth doped sodium yttrium tungstate crystal synthesized in the step (3) is 25mm, and the width of the rare earth doped sodium yttrium tungstate crystal is 3 mm.
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