CN114540935A - Rare earth praseodymium borate crystal material and preparation method thereof - Google Patents
Rare earth praseodymium borate crystal material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a rare earth praseodymium borate crystal material and a preparation method thereof, wherein the rare earth metal borate crystal material is Pr [ B ]5O8(OH)]NO3·2H2O crystal belonging to P21The/c space group. The preparation method comprises the following steps: adding boric acid, praseodymium nitrate hexahydrate, alumina and deionized water into a polytetrafluoroethylene lining, uniformly mixing, reacting for one day at 260 ℃ under the condition of autogenous pressure, then cooling to 240 ℃ and continuing to react for 4 days to obtain rare earth praseodymium borate Pr [ B ]5O8(OH)]NO3·2H2And O crystal material. The compound is synthesized by medium-temperature hydrothermal, the synthesis steps are simple, the obtained crystal has high quality, is not deliquescent in air and insoluble in water, a specific structure can be obtained by single crystal diffraction test, the energy consumption in the synthesis process is low, and the adopted raw materials are easy to obtain and have low price. Obtained rare earth borate compoundHas the characteristic luminescence property of Pr.
Description
Technical Field
The invention belongs to the technical field of crystal materials, and particularly relates to a rare earth praseodymium borate crystal material and a preparation method thereof.
Background
The rare earth borate is widely concerned and researched in recent years, and the binary system can combine the characteristics of rare earth and borate to obtain a material with excellent performance and is applied to the fields of multiband photoluminescence, laser, nonlinear optics, biosensors, medical diagnosis and the like. Boron coordinates with oxygen in the borate structure to form two basic configurations, BO respectively3Triangular configuration and BO4Tetrahedral configuration, both basic configurations being further passed through a common oxygenAtoms can form a variety of boron oxygen anion clusters, so that the borate has a very diverse structure, is rich in configuration suitable for selection, has a low melting point, is simple and effective in a synthesis method, is relatively low in cost, and can be combined with various types of cations, such as organic cations, alkali or alkaline earth metal ions and the like, so that various functional materials are formed. The rare earth has special 4f orbital electrons and is coated with an outer layer 5s25p6The track electron shields, has higher luminous purity and can be used as a luminous center. When the rare earth compound is used as a luminescent material, the luminous intensity, the luminous wavelength and the like of the rare earth compound are influenced by a substrate combined with the rare earth compound, and the selection of a proper substrate can enhance the luminous intensity and adjust the luminous wavelength. The rare earth cations are combined with boric acid anion clusters with rich structural varieties, so that the material with good luminous performance can be obtained.
The high-temperature solid-phase synthesis method is a main method for obtaining rare earth borate, and the hydrothermal synthesis method with relatively low temperature is difficult to obtain rare earth borate crystals because rare earth ions have high charges and are relatively concentrated when combined with polyborate ion clusters according to the Lux-Flood acid-base theory, so that a stable structure is difficult to form, and crystallization is difficult (chem. Mater.2003,15, 2253-. In addition, because the reaction environment of the borate crystal obtained under the hydrothermal condition is between alkaline and weakly acidic, rare earth ions are easy to hydrolyze under the condition to become precipitates, and the rare earth borate crystal is difficult to form.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the rare earth praseodymium borate crystal material and the preparation method thereof, the rare earth borate crystal is obtained by a hydrothermal synthesis method at a lower temperature, the energy consumption in the synthesis process is lower, and the adopted raw materials are easy to obtain and have low price. The obtained rare earth borate compound has the characteristic luminescence property of Pr.
In order to solve the technical problems, the invention adopts the following technical scheme:
a rare-earth praseodymium borate crystal material is prepared from Pr B5O8(OH)]NO3·2H2O crystal, Pr [ B ]5O8(OH)]NO3·2H2The O crystal belongs to P21The/c space group.
Further, the Pr [ B ]5O8(OH)]NO3·2H2The O crystal contains one 3-valent rare earth Pr ion, 5 crystallographically independent 3-valent B ions, 9O ions connected with B, 1 nitrate ion, two crystal water molecules, and 5B ions are connected with 9O ions to form one [ B ] ion5O8(OH)]Polyanion cluster, which can be seen as 3 BOs3Triangle and two BOs4The tetrahedron shares vertex angle oxygen to form, the anion cluster can be used as a basic construction unit, each unit is connected with other 4 units to form a two-dimensional layered B-O structure on an ac plane, and rare earth Pr is filled in a window of the two-dimensional layered B-O structure.
The preparation method of the rare earth praseodymium borate crystal material comprises the following steps: uniformly mixing 15mmol of boric acid, 1mmol of praseodymium nitrate hexahydrate, 1mmol of aluminum oxide and 3mL of deionized water in a polytetrafluoroethylene lining with the volume of 23mL, reacting for one day at the temperature of 260 ℃, then cooling to 240 ℃ and continuing to react for 4 days to obtain light green regular flaky crystal rare earth praseodymium borate Pr [ B ]5O8(OH)]NO3·2H2And O crystal material.
Preferably, the molar ratio of the boric acid to the praseodymium nitrate hexahydrate to the alumina is 15:1: 1.
Preferably, 2-4mL of deionized water is needed based on 1mmol of praseodymium nitrate hexahydrate.
Further, 3mL of deionized water was required based on 1mmol of praseodymium nitrate hexahydrate.
The rare earth neodymium borate near-infrared luminescent crystal material of the invention is prepared by the following steps: uniformly mixing 15mmol of boric acid, 1mmol of praseodymium nitrate hexahydrate, 1mmol of aluminum oxide and 3mL of deionized water in a polytetrafluoroethylene lining with the volume of 23mL, reacting for one day at 260 ℃ under the condition of autogenous pressure (pressure generated by internal air and water vapor), then cooling to 240 ℃ and continuing to react for 4 days to obtain light green regular flaky crystal rare earth praseodymium borate Pr [ B ] of the green regular flaky crystal5O8(OH)]NO3·2H2O crystalA bulk material.
The invention has the beneficial effects that: many rare earth borate compounds are reported, but most of the rare earth borate compounds are in powder morphology, and the products with the reported crystal morphology have completely different crystallographic parameters and completely different physicochemical properties due to different connection modes. In the hydrothermal reaction process, boric acid and praseodymium nitrate hexahydrate are both melted to form a molten state at 260 ℃, the form of boric acid ion clusters is changed after the molten boric acid is combined with alumina, the boric acid is combined with molten rare earth, 3ml of added water is added, the water enables reaction raw materials to finally form a uniform mixture in a reaction kettle, the reaction is carried out at a set temperature and under autogenous pressure, and after the reaction is finished and cooled to room temperature, Pr [ B ] is obtained by natural crystallization5O8(OH)]NO3·2H2And O crystal material.
The compound is synthesized by medium-temperature hydrothermal, the synthesis steps are simple, the obtained crystal has high quality, is not deliquescent in air and insoluble in water, a specific structure can be obtained by single crystal diffraction test, the energy consumption in the synthesis process is low, and the adopted raw materials are easy to obtain and have low price. The obtained rare earth borate compound has the characteristic luminescence property of Pr.
Drawings
FIG. 1 shows a compound Pr [ B ]5O8(OH)]NO3·2H2An asymmetric unit of O;
FIG. 2 shows a compound Pr [ B ]5O8(OH)]NO3·2H2A two-dimensional B-O layer structure of O;
FIG. 3 shows a compound Pr [ B ]5O8(OH)]NO3·2H2Cell stacking diagram of O;
FIG. 4 shows a compound Pr [ B ]5O8(OH)]NO3·2H2O powder diffractogram (experimental values for the upper curve and simulated values for the lower curve);
FIG. 5 shows a compound Pr [ B ]5O8(OH)]NO3·2H2O fluorescence spectrum (excitation wavelength 400 nm).
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
The preparation method of the rare earth praseodymium borate crystal material comprises the following steps: uniformly mixing 15mmol of boric acid, 1mmol of praseodymium nitrate hexahydrate, 1mmol of aluminum oxide and 3mL of deionized water in a polytetrafluoroethylene lining with the volume of 23mL, reacting for one day at the temperature of 260 ℃, then cooling to 240 ℃ and continuing to react for 4 days to obtain light green regular flaky crystal rare earth praseodymium borate Pr [ B ]5O8(OH)]NO3·2H2And O crystal material.
In the hydrothermal reaction process, boric acid and praseodymium nitrate hexahydrate are melted at 260 ℃ to form a molten state, the state of boric acid ion clusters is changed after the molten boric acid is combined with alumina, so that the boric acid is combined with molten rare earth, 3ml of added water is added, the water enables reaction raw materials to finally form a uniform mixture in a reaction kettle, the reaction is carried out at a set temperature and a self-generated pressure, and after the reaction is finished and cooled to room temperature, the product is naturally crystallized to form the product. Under the condition of other unchanged conditions, when the water adding amount is changed, the rare earth praseodymium borate crystal material can be obtained between 2 and 4mL of water.
The present invention adopts medium temperature hydrothermal process and specific reaction condition to synthesize new rare earth metal borate Pr B5O8(OH)]NO3·2H2O crystal, the main crystallographic parameters of which are shown in Table 1. Compound Pr [ B5O8(OH)]NO3·2H2The O crystal belongs to P21The/c space group has an asymmetric unit structure shown in figure 1, and comprises one 3-valent rare earth Pr ion, 5 crystallographically independent 3-valent B ions, 9O ions connected with B, 1 nitrate ion and two crystal water molecules. 5B ions are linked with 9O ions to form a [ B ]5O8(OH)]Polyanion cluster, which can be seen as 3 BOs3Triangle and two BOs4Tetrahedron shared roofAngle oxygen formation. The anion cluster can be used as a basic construction unit, each unit is connected with 4 other units to form a two-dimensional layered B-O structure on an ac plane, and rare earth Pr is filled in a window of the two-dimensional layered B-O structure (figure 2). As shown in the cell stacking diagram (FIG. 3), the space between the layered B-O structures is filled with nitrate ions and crystal water.
The bond length of B-O bond in the compound is divided into two types, one is BO3Triangular structure, and B-O bond length in the range of
BO of another B type with four oxygens4In the tetrahedral structure, the bond length of the B-O bond is in the range of
In the meantime. The N-O bond length of the nitrate ions is within the range
Pr is coordinated with 10 oxygen atoms, and the bond length of the Pr-O bond is in the range of
In the meantime. These bond length values are consistent with reported crystal data for rare earth borates.
Compound Pr [ B5O8(OH)]NO3·2H2The crystal of O is tested by powder XRD, as shown in figure 4, in the range of 9-50 degrees, the diffraction peak of powder experiment and the peak position of theoretical diffraction peak can be in one-to-one correspondence, which proves that the obtained compound is pure phase. The visible light emission performance of the compound is shown in FIG. 5, under the condition that the excitation wavelength is 400nm, the characteristic emission peaks of Pr appear in the range of 450-850nm, which are 461nm, 476nm, 493nm and 611nm, 694nm respectively correspond to the rare earth Pr ions3H4→3P2、3H4→3P1、3H4→3P0And1D2→3H4、3P0→3F3the characteristic emission peak generated by the transition indicates that the compound can be used as a potential photoluminescence material.
TABLE 1 Compound Pr [ B5O8(OH)]NO3·2H2O crystallography data sheet
The invention obtains rare earth borate crystal by a hydrothermal synthesis method at lower temperature, selects and uses aluminum oxide or zinc oxide, the aluminum, the zinc and oxygen are combined to form Al-O tetrahedron and Zn-O tetrahedron structures, the structures are easy to be combined with a boron-oxygen cluster framework, and aims to add aluminum-zinc oxide serving as a reaction raw material into boric acid and rare earth, change the inherent reaction environment of the rare earth and the boric acid, thereby obtaining the rare earth borate crystal in the hydrothermal synthesis.
According to the invention, alumina, zinc oxide, boric acid and praseodymium nitrate are selected as reaction raw materials, a proper amount of deionized water is added as a medium to carry out hydrothermal reaction, a reaction vessel is a reaction kettle with a built-in 23mL polytetrafluoroethylene lining, and a series of comparative experiments are carried out, wherein the specific experiments are shown in Table 2.
TABLE 2 series of comparative tests
As shown in Table 2, experiment No. 6 successfully obtained the Pr [ B ] compound of the present invention5O8(OH)]NO3·2H2The crystal of O is obtained by a one-step hydrothermal synthesis method, the crystal appearance is light green sheet, the crystal is small, the surface cracks are more, the crystal cell parameters are determined by single crystal experiment tests, but the analysis is difficult. Based on the condition of successfully obtaining crystals, 15mmol of boric acid, 1mmol of praseodymium nitrate hexahydrate and alumina are adopted1mmol, 3mL deionized water is evenly mixed in a polytetrafluoroethylene lining with the volume of 23mL, the mixture reacts for one day under the condition of 260 ℃ and autogenous pressure (pressure generated by internal air and water vapor), and then the temperature is reduced to 240 ℃ to continue the reaction for 4 days, so that light green regular flaky crystals with high quality are obtained. In the hydrothermal reaction process, boric acid and praseodymium nitrate hexahydrate are melted at 260 ℃ to form a molten state, the state of boric acid ion clusters is changed after the molten boric acid is combined with alumina, so that the boric acid is combined with molten rare earth, 3ml of added water is added, the water enables reaction raw materials to finally form a uniform mixture in a reaction kettle, the reaction is carried out at a set temperature and a self-generated pressure, and after the reaction is finished and cooled to room temperature, the product is naturally crystallized to form the product. Under otherwise unchanged conditions, the amount of water added was varied and it was found that crystals of the product of the invention could be obtained between 2 and 4mL of water.
Many rare earth borate compounds are reported, but most of the rare earth borate compounds are in powder morphology, and the products with the reported crystal morphology have completely different crystallographic parameters and completely different physicochemical properties due to different connection modes. The compound in the invention is synthesized by medium-temperature hydrothermal, the synthesis steps are simple, the obtained crystal has higher quality, is not deliquescent in air and insoluble in water, the specific structure can be obtained by single crystal diffraction test, the energy consumption in the synthesis process is lower, and the adopted raw materials are easy to obtain and have low price. The obtained rare earth borate compound has the characteristic luminescence property of Pr.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A rare earth praseodymium borate crystal material is characterized in that: the above-mentionedThe rare-earth metal borate crystal material is Pr [ B ]5O8(OH)]NO3·2H2O crystal, Pr [ B ]5O8(OH)]NO3·2H2The O crystal belongs to P21The/c space group.
2. The rare earth praseodymium borate crystalline material of claim 1, wherein: the Pr [ B ]5O8(OH)]NO3·2H2The O crystal contains one 3-valent rare earth Pr ion, 5 crystallographically independent 3-valent B ions, 9O ions connected with B, 1 nitrate ion, two crystal water molecules, and 5B ions are connected with 9O ions to form one [ B ] ion5O8(OH)]Polyanion cluster, which can be seen as 3 BOs3Triangle and two BOs4The tetrahedron shares vertex angle oxygen to form, the anion cluster can be used as a basic construction unit, each unit is connected with other 4 units to form a two-dimensional layered B-O structure on an ac plane, and rare earth Pr is filled in a window of the two-dimensional layered B-O structure.
3. The method for preparing a rare earth praseodymium borate crystal material as set forth in claim 1 or 2, characterized by comprising the steps of: adding boric acid, praseodymium nitrate hexahydrate, alumina and deionized water into a polytetrafluoroethylene lining, uniformly mixing, reacting for one day at 260 ℃, then cooling to 240 ℃ and continuing to react for 4 days to obtain light green regular flaky crystal rare earth praseodymium borate Pr [ B ]5O8(OH)]NO3·2H2O crystal material.
4. A method for preparing a near-infrared luminescent crystalline material of rare earth neodymium borate according to claim 3, characterized in that: the molar ratio of the boric acid to the praseodymium nitrate hexahydrate to the aluminum oxide is 15:1: 1.
5. A method for preparing a near-infrared luminescent crystalline material of rare earth neodymium borate according to claim 3, characterized in that: 2-4mL of deionized water is needed based on 1mmol of praseodymium nitrate hexahydrate.
6. The method for preparing a rare earth neodymium borate near-infrared luminescent crystal material according to claim 5, characterized in that: 3mL of deionized water is needed based on 1mmol of praseodymium nitrate hexahydrate.
7. A method of producing a near infrared luminescent crystalline material of rare earth neodymium borate according to claim 5, characterised in that the typical production steps are as follows: uniformly mixing 15mmol of boric acid, 1mmol of praseodymium nitrate hexahydrate, 1mmol of aluminum oxide and 3mL of deionized water in a polytetrafluoroethylene lining with the volume of 23mL, reacting for one day at 260 ℃, then cooling to 240 ℃ and continuing to react for 4 days to obtain light green regular flaky crystal rare earth praseodymium borate Pr [ B ]5O8(OH)]NO3·2H2And O crystal material.
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Cited By (3)
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| DE102021133467A1 (en) | 2021-12-16 | 2023-06-22 | Endress+Hauser Conducta Gmbh+Co. Kg | Calibration standard, sensor arrangement and use |
| CN116163156A (en) * | 2023-01-05 | 2023-05-26 | 广东华凯科技股份有限公司 | Heat-conducting flame-retardant fiber material and preparation method thereof |
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