CN113247957B - Method for synthesizing barium manganese carbonate-trigonosterite solid solution at high temperature and high pressure - Google Patents
Method for synthesizing barium manganese carbonate-trigonosterite solid solution at high temperature and high pressure Download PDFInfo
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Abstract
The invention discloses a method for synthesizing barium-manganese carbonate-trigonellite solid solution at high temperature and high pressure, which usesAnalytically pure manganese carbonate MnCO 3 And analytically pure calcium carbonate CaCO 3 Grinding and mixing the raw materials uniformly according to a molar ratio of (1-x): x to obtain a precursor of calcium manganese carbonate (Mn) through a high-temperature high-pressure reaction 1‑x Ca x ) CO; using analytically pure barium carbonate BaCO 3 And precursor calcium manganese carbonate (Mn) 1‑x Ca x )CO 3 Mixing the raw materials in a molar ratio of 1:1 to obtain barium manganese carbonate-trigonal barium calcite solid solution Ba (Mn) 1‑x Ca x )(CO 3 ) 2 ，0<x<1, the discovery connects the current discontinuous phase diagrams, and provides important experimental basis for constructing a complete three-way barium-containing double carbonate family.
Description
Technical Field
The invention relates to the field of research of earth science and mineralogy, and relates to a method for synthesizing a barium manganese carbonate-trigonotite solid solution at high temperature and high pressure.
Background
Bis-carbonate AB (CO) 3 ) 2 Structure, composition and properties are the focus of current quantitative research on carbonate minerals. BaCa (CO) barium calcium stone 3 ) 2 The mineral is a bicarbonate mineral widely existing in nature, the crystal structure of the mineral is complex, and various homogeneous and heterogeneous images exist, wherein the periclase is an important crystal form. BaMg (CO) of Babai marble family double carbonate of trigonal crystal system 3 ) 2 、BaFe(CO 3 ) 2 And BaMn (CO) 3 ) 2 Is discovered in nature and experimental research successively, and the present research shows that the barium dolomite family can form three-terminal complete solid solution Ba (Mg, Fe, Mn) (CO) 3 ) 2 . On the basis, if the tripartite blanc fixe is added to the sequence, the sequence is represented by BaMg (CO) 3 ) 2 、BaFe(CO 3 ) 2 、BaMn(CO 3 ) 2 And tripartite BaCa (CO) 3 ) 2 Can be expanded to a complete trigonal barium-containing bicarbonates family, which is analogous to the complete calcite family MgCO 3 -FeCO 3 -MnCO 3 -CaCO 3 . However, threeSquare BaCa (CO) 3 ) 2 The crystal structure of (a) is not completely homogeneous, although it is similar to the barite group. Currently, similar but heterogeneous tripartite BaCa (CO) 3 ) 2 Is it able to form a solid solution with carbonates of the barium dolomite group? This problem is not clear in the field of mineralogy research and still requires experimental validation.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a method for synthesizing barium-manganese carbonate-trigonocellum solid solution at high temperature and high pressure, which fills the blank of the current research.
The technical scheme is a method for synthesizing barium manganese carbonate-trigonellite solid solution at high temperature and high pressure, which comprises the following steps:
step 1, using analytically pure manganese carbonate MnCO 3 And analytically pure calcium carbonate CaCO 3 Grinding and uniformly mixing the raw materials by a molar ratio of (1-x) x to serve as initial raw materials;
step 2, pressing the mixture powder in the step 1 into a cylinder with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping a cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, placing the sample in an h-BN tube, and using the h-BN as a pressure transmission medium;
step 3, assembling the h-BN pipe provided with the sample in the step 2 in a high-pressure synthesis assembly block and placing the h-BN pipe in a cubic apparatus large press for high-temperature high-pressure reaction;
and 4, after the high-temperature high-pressure reaction is finished, taking out the sample in the step 3, stripping off gold foil on the surface of the sample, and grinding into powder to obtain a precursor of calcium manganese carbonate (Mn) 1-x Ca x )CO 3 ；
Step 5, using analytically pure barium carbonate BaCO 3 And precursor calcium manganese carbonate (Mn) 1-x Ca x )CO 3 Mixing the raw materials in a molar ratio of 1:1 as a starting material, pressing the mixture into a cylindrical shape with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping the cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, and placing the sample in an h-BN tube by using the h-BN as a pressure transmission medium;
step 6, assembling the h-BN pipe provided with the sample in the step 5 in a high-pressure synthesis assembly block and placing the h-BN pipe in a cubic apparatus large press for high-temperature high-pressure reaction;
step (ii) of7, after the high-temperature high-pressure reaction is finished, taking out the sample, stripping off gold foil on the surface of the sample, and grinding the sample into powder to obtain the barium manganese carbonate-trigonal barium calcium stone solid solution Ba (Mn) 1-x Ca x )(CO 3 ) 2 。
Further, the manufacturing method of the h-BN pipe in the step 2 is the same as that in the step 6, and the specific operation is as follows: drilling a phi 5mm hole in the center of a phi 10mm h-BN rod on a lathe to form an h-BN tube, inserting a sample into the tube, and sealing two ends of the h-BN tube by using phi 5mm h-BN sheets with the thickness of 2 mm.
Further, the method for assembling the h-BN pipe in the high-pressure synthesis assembly block in the step 3 and the step 7 is the same, and the specific operation comprises the following steps: selecting a pyrophyllite block, and punching a phi 12mm circular through hole in the center of the pyrophyllite block; a circular graphite heating furnace with the outer diameter of 12mm and the inner diameter of phi 10mm is sleeved in the circular through hole; placing a 10mm h-BN tube sealed sample in the middle of a graphite heating furnace; the upper end and the lower end of the round graphite heating furnace are sealed by pyrophyllite plugs.
Further, the high-temperature high-pressure reaction condition in the step 3 is 1GPa, 700 ℃, the reaction time is 2 hours, and the quenching and the slow pressure relief are carried out for more than 30 minutes after the reaction is finished.
Further, the high-temperature high-pressure reaction conditions in the step 6 are that the high-temperature high-pressure reaction conditions are 1GPa, 700 ℃, the reaction time is 6 hours, quenching is carried out after the reaction is finished, and the pressure is rapidly released within 3 minutes.
Further, the synthetic product obtained in the step 7 is barium manganese carbonate-trigonal barium calcium stone solid solution Ba (Mn) 1- x Ca x )(CO 3 ) 2 Pure phase, 0<x<1, no other impurities.
Further, the barium manganese carbonate-trigonal barium calcium stone solid solution Ba (Mn) obtained in the step 7 1-x Ca x )(CO 3 ) 2 Is trigonal, the lattice parameter
The invention has the advantages that:
the innovation point of the invention is that the invention synthesizes for the first timeFrom the barium dolomite family of end members BaMn (CO) 3 ) 2 -tripartite barite BaCa (CO) 3 ) 2 Continuous solid solution of Ba (Mn) 1-x Ca x )(CO 3 ) 2 ，0<x<1, the technical problem of the existing barium-containing dicarbonate research is solved, and the guarantee is provided for further quantitative research of physicochemical properties. The invention has the beneficial effect that BaMg (CO) in the phase diagram of the barium-containing double carbonate component of the three parties 3 ) 2 、BaFe(CO 3 ) 2 And BaMn (CO) 3 ) 2 The phase region is completely continuous, but from BaMn (CO) 3 ) 2 To three-party BaCa (CO) 3 ) 2 The phase region of (a) is also discontinuous. The invention provides a continuous solid solution Ba (Mn) 1-x Ca x )(CO 3 ) 2 ，0<x<1, connecting the current discontinuous phase diagrams, constructing a complete tripartite barium-containing double carbonate family, and finding out the solid solution rule of tripartite barium-calcium stone and barium-dolomite family: (1) tripartite blanc fixe can only be combined with BaMn (CO) in the barium dolomite group 3 ) 2 Form a continuous solid solution with BaMg (CO) 3 ) 2 Or BaFe (CO) 3 ) 2 A solid solution cannot be formed. (2) According to Ba (Mn) 1-x Ca x )(CO 3 ) 2 As a result of powder X-ray, the diffraction angle 2 theta was in the range of 0 to 70 deg., and all diffraction peaks shifted to a low angle with an increase in the content of calcium, wherein the intensities of the (003), (101), (015), (113) and (021) diffraction peaks decreased with an increase in the content of Ca, up to three-way BaCa (CO) 3 ) 2 Completely disappeared while the other diffraction peaks were unchanged in intensity.
Detailed Description
Example 1
High-temperature high-pressure synthesis of barium manganese carbonate-trigonoceltide solid solution Ba (Mn) 0.1 Ca 0.9 )(CO 3 ) 2 The method comprises the following steps:
step 1, using analytically pure manganese carbonate MnCO 3 And analytically pure calcium carbonate CaCO 3 Grinding and uniformly mixing the raw materials as initial raw materials according to the molar ratio of 1: 9;
step 2, pressing the mixture powder in the step 1 into a cylinder with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping a cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, placing the sample in an h-BN tube, and using the h-BN as a pressure transmission medium;
step 3, assembling the h-BN pipe provided with the sample in the step 2 in a high-pressure synthesis assembly block, placing the h-BN pipe in a cubic apparatus large press for high-temperature and high-pressure reaction, wherein the reaction conditions are 1GPa and 700 ℃, the reaction time is 2 hours, quenching is carried out after the reaction is finished, and then the pressure is slowly released within 30 minutes;
and 4, after the high-temperature high-pressure reaction is finished, taking out the sample in the step 3, stripping off gold foil on the surface of the sample, and grinding into powder to obtain a precursor of calcium manganese carbonate (Mn) 0.1 Ca 0.9 )CO 3 ；
Step 5, using analytically pure barium carbonate BaCO 3 And precursor calcium manganese carbonate (Mn) 0.1 Ca 0.9 )CO 3 Mixing the raw materials in a molar ratio of 1:1 as a starting material, pressing the mixture into a cylindrical shape with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping the cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, and placing the sample in an h-BN tube by using the h-BN as a pressure transmission medium;
step 6, assembling the h-BN pipe provided with the sample in the step 5 in a high-pressure synthesis assembly block and placing the h-BN pipe in a cubic apparatus large press for high-temperature and high-pressure reaction, wherein the high-temperature and high-pressure reaction conditions are 1GPa and 700 ℃, the reaction time is 6 hours, and quenching and rapid pressure relief are carried out within 3 minutes after the reaction is finished;
step 7, taking out the sample, stripping off gold foil on the surface of the sample, and grinding into powder to obtain barium manganese carbonate-trigonal barium calcium stone solid solution Ba (Mn) 0.1 Ca 0.9 )(CO 3 ) 2 。
Example 2
High-temperature high-pressure synthesis of barium manganese carbonate-trigonoceltide solid solution Ba (Mn) 0.9 Ca 0.1 )(CO 3 ) 2 The method comprises the following steps:
step 1, using analytically pure manganese carbonate MnCO 3 And analytically pure calcium carbonate CaCO 3 Grinding and uniformly mixing the raw materials as initial raw materials according to a molar ratio of 9: 1;
step 2, pressing the mixture powder in the step 1 into a cylinder with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping a cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, placing the sample in an h-BN tube, and using the h-BN as a pressure transmission medium;
step 3, assembling the h-BN pipe provided with the sample in the step 2 in a high-pressure synthesis assembly block, placing the h-BN pipe in a cubic apparatus large press for high-temperature and high-pressure reaction, wherein the reaction conditions are 1GPa and 700 ℃, the reaction time is 2 hours, quenching is carried out after the reaction is finished, and then the pressure is slowly released within 40 minutes;
and 4, after the high-temperature high-pressure reaction is finished, taking out the sample in the step 3, stripping off gold foil on the surface of the sample, and grinding into powder to obtain a precursor of calcium manganese carbonate (Mn) 0.9 Ca 0.1 )CO 3 ；
Step 5, using analytically pure barium carbonate BaCO 3 And precursor calcium manganese carbonate (Mn) 0.9 Ca 0.1 )CO 3 Mixing the raw materials in a molar ratio of 1:1 as a starting material, pressing the mixture into a cylindrical shape with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping the cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, and placing the sample in an h-BN tube by using the h-BN as a pressure transmission medium;
step 6, assembling the h-BN pipe provided with the sample in the step 5 in a high-pressure synthesis assembly block and placing the h-BN pipe in a cubic apparatus large press for high-temperature and high-pressure reaction, wherein the high-temperature and high-pressure reaction conditions are 1GPa and 700 ℃, the reaction time is 6 hours, and quenching and rapid pressure relief are carried out within 3 minutes after the reaction is finished;
step 7, taking out the sample, stripping off gold foil on the surface of the sample, and grinding into powder to obtain barium manganese carbonate-trigonal barium calcium stone solid solution Ba (Mn) 0.9 Ca 0.1 )(CO 3 ) 2 。
Example 3
High-temperature high-pressure synthesis of barium manganese carbonate-trigonoceltide solid solution Ba (Mn) 0.5 Ca 0.5 )(CO 3 ) 2 The method comprises the following steps:
step 1, using analytically pure manganese carbonate MnCO 3 And analytically pure calcium carbonate CaCO 3 Grinding and uniformly mixing the raw materials as initial raw materials according to the molar ratio of 1: 1;
step 2, pressing the mixture powder in the step 1 into a cylinder with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping a cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, placing the sample in an h-BN tube, and using the h-BN as a pressure transmission medium;
step 3, assembling the h-BN pipe provided with the sample in the step 2 in a high-pressure synthesis assembly block, placing the h-BN pipe in a cubic apparatus large press for high-temperature and high-pressure reaction, wherein the reaction conditions are 1GPa and 700 ℃, the reaction time is 2 hours, quenching is carried out after the reaction is finished, and then the pressure is slowly released within 30 minutes;
and 4, after the high-temperature high-pressure reaction is finished, taking out the sample in the step 3, stripping off gold foil on the surface of the sample, and grinding into powder to obtain a precursor of calcium manganese carbonate (Mn) 0.5 Ca 0.5 )CO 3 ；
Step 5, using analytically pure barium carbonate BaCO 3 And precursor calcium manganese carbonate (Mn) 0.9 Ca 0.1 )CO 3 Mixing the raw materials in a molar ratio of 1:1 as a starting material, pressing the mixture into a cylindrical shape with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping the cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, and placing the sample in an h-BN tube by using the h-BN as a pressure transmission medium;
step 6, assembling the h-BN pipe provided with the sample in the step 5 in a high-pressure synthesis assembly block and placing the h-BN pipe in a cubic apparatus large press for high-temperature and high-pressure reaction, wherein the high-temperature and high-pressure reaction conditions are 1GPa and 700 ℃, the reaction time is 6 hours, and quenching and rapid pressure relief are carried out within 3 minutes after the reaction is finished;
step 7, taking out the sample, stripping off gold foil on the surface of the sample, and grinding into powder to obtain barium manganese carbonate-trigonal barium calcium stone solid solution Ba (Mn) 0.5 Ca 0.5 )(CO 3 ) 2 。
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. 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 (5)
1. A method for synthesizing a barium manganese carbonate-trigonotite solid solution at high temperature and high pressure is characterized by comprising the following steps:
step 1, using analytically pure manganese carbonate MnCO 3 And analytically pure calcium carbonate CaCO 3 Grinding and uniformly mixing the raw materials by a molar ratio of (1-x) x to serve as initial raw materials;
step 2, pressing the mixture powder in the step 1 into a cylinder with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping a cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, placing the sample in an h-BN tube, and using the h-BN as a pressure transmission medium;
step 3, assembling the h-BN pipe provided with the sample in the step 2 in a high-pressure synthesis assembly block and placing the h-BN pipe in a cubic apparatus large press for high-temperature and high-pressure reaction, wherein the reaction conditions are 1GPa and 700 ℃, the reaction time is 2 hours, and the h-BN pipe is quenched after the reaction is finished and is slowly decompressed within more than 30 minutes;
and 4, after the high-temperature high-pressure reaction is finished, taking out the sample in the step 3, stripping off gold foil on the surface of the sample, and grinding into powder to obtain a precursor of calcium manganese carbonate (Mn) 1-x Ca x )CO 3 ；
Step 5, using analytically pure barium carbonate BaCO 3 And precursor calcium manganese carbonate (Mn) 1-x Ca x )CO 3 Mixing the raw materials in a molar ratio of 1:1 as a starting material, pressing the mixture into a cylindrical shape with the diameter of 5 multiplied by 3mm by using a tablet press, wrapping the cylindrical sample by using a gold foil with the thickness of 0.02mm as a sample, and placing the sample in an h-BN tube by using the h-BN as a pressure transmission medium;
step 6, assembling the h-BN pipe provided with the sample in the step 5 in a high-pressure synthesis assembly block and placing the h-BN pipe in a cubic apparatus large press for high-temperature and high-pressure reaction under the reaction conditions of 1GPa and 700 ℃ for 6 hours, quenching after the reaction is finished and rapidly releasing pressure within 3 minutes; and 7, after the high-temperature high-pressure reaction is finished, taking out the sample, stripping off gold foil on the surface of the sample, and grinding the sample into powder to obtain the barium manganese carbonate-trigonal barium calcium stone solid solution Ba (Mn) 1-x Ca x )(CO 3 ) 2 。
2. The method for synthesizing the barium manganese carbonate-trigonal barium calcite solid solution at high temperature and high pressure according to claim 1, wherein the manufacturing method of the h-BN tube in the step 2 is the same as that in the step 5, and the specific operations are as follows: drilling a phi 5mm hole in the center of a phi 10mm h-BN rod on a lathe to form an h-BN tube, inserting a sample into the tube, and sealing two ends of the h-BN tube by using phi 5mm h-BN sheets with the thickness of 2 mm.
3. The method for synthesizing the barium manganese carbonate-trigonal xonotlite solid solution at high temperature and high pressure according to claim 1, wherein the method for assembling the h-BN tube in the high-pressure synthesis assembly block in the steps 3 and 6 is the same, and the specific operations comprise: selecting a pyrophyllite block, and punching a phi 12mm circular through hole in the center of the pyrophyllite block; a circular graphite heating furnace with the outer diameter of 12mm and the inner diameter of phi 10mm is sleeved in the circular through hole; placing a 10mm h-BN tube sealed sample in the middle of a graphite heating furnace; the upper end and the lower end of the round graphite heating furnace are sealed by pyrophyllite plugs.
4. The method for synthesizing the barium manganese carbonate-trigonosterite solid solution at high temperature and high pressure according to claim 1, wherein the synthetic product obtained in the step 7 is barium manganese carbonate-trigonosterite solid solution Ba (Mn) 1-x Ca x )(CO 3 ) 2 Pure phase, 0<x<1, no other impurities.
5. The method for synthesizing the barium-manganese-trigonosterite solid solution at high temperature and high pressure according to claim 1, wherein the barium-manganese-trigonosterite solid solution Ba (Mn) obtained in step 7 1-x Ca x )(CO 3 ) 2 Is trigonal, the lattice parameter
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| CN108793259A (en) * | 2018-06-15 | 2018-11-13 | 中国科学院地球化学研究所 | A method of synthesizing nemalite at high temperature under high pressure |
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| CN107640787B (en) * | 2017-09-04 | 2019-04-02 | 中国科学院地球化学研究所 | A method of preparing mangandolomite at high temperature under high pressure |
| CN108642565B (en) * | 2018-06-15 | 2019-07-26 | 中国科学院地球化学研究所 | A method of carbonate synthesis barium manganese monocrystalline at high temperature under high pressure |
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| CN108793259A (en) * | 2018-06-15 | 2018-11-13 | 中国科学院地球化学研究所 | A method of synthesizing nemalite at high temperature under high pressure |
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