CN113860320B - Method for synthesizing aqueous plagioclase solid solution at high temperature and high pressure - Google Patents
Method for synthesizing aqueous plagioclase solid solution at high temperature and high pressure Download PDFInfo
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- 229910052655 plagioclase feldspar Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 36
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 24
- 239000006104 solid solution Substances 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 85
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052802 copper Inorganic materials 0.000 claims abstract description 55
- 239000010949 copper Substances 0.000 claims abstract description 55
- 239000011521 glass Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 23
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 10
- 229910052661 anorthite Inorganic materials 0.000 claims abstract description 8
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002474 experimental method Methods 0.000 claims abstract description 8
- 229910052656 albite Inorganic materials 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims description 17
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 16
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 238000005498 polishing Methods 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000003466 welding Methods 0.000 claims description 6
- 229910052580 B4C Inorganic materials 0.000 claims description 5
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000000704 physical effect Effects 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 238000005553 drilling Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 235000012431 wafers Nutrition 0.000 claims 3
- 239000011734 sodium Substances 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000010433 feldspar Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 229910052599 brucite Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000000454 talc Substances 0.000 description 5
- 229910052623 talc Inorganic materials 0.000 description 5
- 235000012222 talc Nutrition 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 230000006399 behavior Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for synthesizing a water-containing plagioclase solid solution at high temperature and high pressure, which comprises the following steps: according to the mole ratio of albite and anorthite in the plagioclase solid solution, 4:1, respectively weighing initial raw materials with the stoichiometric ratio of albite to anorthite and grinding and mixing the initial raw materials uniformly in alcohol by an agate mortar, and drying the mixture in an oven; synthesizing the plagioclase glass at high temperature; crushing plagioclase glass in a platinum crucible with plagioclase glass on a tablet press, putting the plagioclase glass into a high-frequency vibration ball mill, grinding the plagioclase glass into powder with uniform particles, and then putting the powder into a baking oven for baking; preparing a primary copper tube and a secondary copper tube; assembling an aqueous sample; high-temperature high-pressure synthesis and assembly; placing the assembly blocks on a hexahedral top large press to synthesize an aqueous sample under the conditions of high temperature and high pressure so as to obtain a finished product; the method solves the technical problems that the sample size is limited, the water content of the sample is controlled inaccurately, the experiment cost is high and the like in the synthesis of the water-containing plagioclase solid solution in the prior art.
Description
Technical Field
The invention belongs to the field of geochemistry research of high-temperature high-pressure experiments, and particularly relates to a method for synthesizing a water-containing plagioclase solid solution at high temperature and high pressure.
Background
Plagioclase is the main nominally anhydrous mineral of the crust, and usually contains small amounts of OH and H 2 Structural water in the form of O is present in an amount of from tens to thousands of ppm. The presence of water affects not only the physical and chemical properties of plagioclase, such as mechanical, elastic properties, electrical conductivity, thermal conductivity, diffusion of elements, ordering/disorder of Al/Si, etc., but also the presence of water has important significance for circulation of the water in the subsurface crust, formation and evolution of the crust, stability of rock ring and rheological results in research.
The range of water content in natural plagioclase is limited, and the change of water content is often related to factors such as temperature, pressure, oxygen loss and the like. If a natural sample is adopted to develop the research on the correlation of the water content and the physical property and chemical behavior of plagioclase, the research is likely to be limited by the limited water content change in the natural sample, and the accuracy and the credibility of the research are difficult to ensure. Experimental synthesis of plagioclase with different water content is an effective method to solve this problem. At present, the water-containing synthesis experiment of the nominal anhydrous mineral mainly adopts the following two modes: (1) talcum and brucite are water sources; the two kinds of water-containing minerals are added to two ends of the sample, and water fluid released by dehydration reaction of the minerals is diffused into the sample under high temperature and high pressure, so that the water-containing sample is synthesized. The water content change in the synthetic sample is achieved by adjusting the weight ratio of talc to brucite to control the amount of water fluid released after dehydration of the talc and brucite occurs. (2) distilled or deionized water as a water source; a certain amount of distilled water was added to the metal tube containing the sample, after which the sealed metal tube was welded, and free water was allowed to diffuse into the lattice of the sample under high temperature and high pressure. In the method (1), water in the sample enters the sample through high-temperature dehydration and diffusion of talcum and brucite, so that the water content at two ends of the sample which directly contacts with talcum and brucite can be higher than that in the middle of the sample, and the water content on the longitudinal section of the sample can be uneven. Thus, the method is limited to smaller aqueous sample syntheses, meaning that the size of the aqueous sample may be limited. The method (2) uses water fluid as a water source, the water quantity added in the sample assembly process is easy to calculate accurately, the added water can be uniformly distributed around the sample particles, the water content in the synthesized sample can be uniformly distributed, and the size of the synthesized sample is not limited. The method adopts a single-bag or double-bag metal tube (a gold tube or a platinum tube) to package the sample, the metal tube wall is usually thinner, the sealing is easy to be not tight in the welding process of the sample tube, and the water in the sample leaks in the high-temperature high-pressure pressing process. Meanwhile, a metal pipe can be welded through in the laser welding sealing process, so that water in a sample is lost due to high-temperature evaporation, and the water content in the synthesized sample is difficult to be guaranteed to be a target value. In addition, the cost of the gold tube or the platinum tube is high, the size needs to be customized, and the processing period is long.
In summary, the existing methods for artificially synthesizing water-containing samples have certain defects, such as too small synthetic size, inaccurate control of water content in the synthesized samples, high experimental cost and the like.
The invention comprises the following steps:
the invention aims to solve the technical problems that: the method for synthesizing the water-containing plagioclase solid solution at high temperature and high pressure is provided, so that the technical problems of limited sample size, inaccurate control of the water content of the sample, high experiment cost and the like in the synthesis technology of the water-containing plase solid solution in the prior art are solved. The technical scheme of the invention is as follows:
a method for synthesizing aqueous plagioclase solid solution at high temperature and high pressure, comprising:
step 1, according to the albite (NaAlSi) in the plagioclase feldspar solid solution 3 O 8 ) Anorthite (CaAl) 2 Si 2 O 8 ) Respectively weighing the initial raw materials of the stoichiometric ratio of the albite and the anorthite corresponding to the weight of the raw materials to obtain Al 2 O 3 、SiO 2 、Na 2 CO 3 、CaCO 3 Grinding and mixing the oxide powder in alcohol uniformly by an agate mortar, and drying the mixture in a baking oven at 200 ℃;
step 2, synthesizing plagioclase glass at high temperature: pressing the mixture powder in the step 1 into a cylinder with the diameter of 13 multiplied by 2mm, placing a sample in a platinum crucible, and placing the sample in a high-temperature furnace for decarbonizing reaction to obtain plagioclase glass at high temperature;
step 3, crushing the plagioclase glass in a platinum crucible filled with plagioclase glass on a tablet press, putting the plagioclase glass into a high-frequency vibration ball mill, grinding the plagioclase glass into powder with uniform particles, and then putting the powder into a baking oven for baking; the particle size is 5-10 mu m;
step 4, preparing a primary copper tube and a secondary copper tube: preparing a first red copper inner tube with an inner diameter of 6mm, a wall thickness of 0.5mm, a height of 12mm and a bottom thickness of 0.5; preparing a red copper outer tube II with the inner diameter of 7.05mm, the wall thickness of 0.5mm, the height of 12.5mm and the bottom thickness of 0.5 mm;
step 5, assembling an aqueous sample: rolling a gold foil with the thickness of 0.05mm into a tube, putting the tube into a first red copper inner tube, putting a gold foil wafer with the same thickness at the bottom, filling the plagioclase glass powder prepared in the step 3 into the first red copper inner tube prepared in the step 4, compacting sample powder after adding distilled water or deionized water into the tube by a liquid-transferring gun, and sealing the sample powder by the gold foil wafer; reversely buckling the red copper outer tube II with the inner diameter of 7.05mm prepared in the step 4 with the red copper inner tube I filled with the sample, and sealing the joint of the two copper tubes by using a laser welding machine;
step 6, high-temperature high-pressure synthesis and assembly: placing the sealed copper tube in the step 5 into a high-temperature high-pressure assembly block with the periphery composed of h-BN tubes and h-BN plug pressure transmission media;
step 7, placing the assembly block on a hexahedral top large press, and synthesizing a water-containing sample under the conditions of high temperature and high pressure;
and 8, after the step 7 is finished, turning off heating current to quench and cool, and slowly reducing the pressure to normal temperature to obtain a finished product.
The method for carrying out the decarbonizing reaction in the high-temperature furnace comprises the following steps: decarbonizing at 1000-1200 deg.c for 10-12 hr, raising the temperature to 1600 deg.c, melting the mixture to glass state and lowering the temperature to room temperature; the high-temperature furnace is a closed high-temperature furnace.
The method for drying in the oven in the step 3 is as follows: drying in a 100 ℃ oven for two hours; after drying, the sample is placed in an oven to be dried until the sample is assembled.
The method for synthesizing the water-containing sample under the high-temperature and high-pressure condition in the step 7 comprises the following steps: synthesizing a water-containing sample at 1100-1200 ℃ and 1-2 GPa; the reaction time is 6-10h.
The high-temperature high-pressure synthesis and assembly method in the step 6 comprises the following steps:
and 6.1, manufacturing an h-BN tube: processing an h-BN rod with the diameter of 11mm into an h-BN tube with the inner diameter of phi 8mm and the outer diameter of phi 11mm on a lathe, polishing the inner diameter by sand paper, putting sealed red copper filled with a sample into the h-BN tube, and plugging both ends by h-BN discs with the diameter of phi 11mm and the thickness of 2 mm;
step 6.2, manufacturing a heater: processing a graphite heating furnace with the inner diameter of phi 11mm, the outer diameter of 13mm and the height of 32.5mm on a lathe;
step 6.3, processing pyrophyllite: selecting a cubic pyrophyllite block with the side length of 32.5mm, and punching a circular through hole with the diameter of 13mm in the center;
step 6.4, assembling: placing a graphite heating furnace in a pyrophyllite block, then placing a red copper sealing tube filled with a sample into a boron carbide tube, and placing the red copper sealing tube and the boron carbide tube together in the graphite heating furnace, wherein two ends of the red copper sealing tube are respectively sealed by a boron nitride plug and a pyrophyllite plug in sequence;
and 6.5, drilling a small hole in the middle of the edge of the pyrophyllite block, and placing a thermocouple which can be directly contacted with the sample copper pipe for accurately controlling the experiment temperature.
It also includes:
step 9, taking out the sample in the step 8, cutting the copper tube by using a diamond wire cutting machine, taking out the sample, polishing the surface of the sample into a cylinder shape, and measuring relevant physical properties;
step 10, performing powder XRD measurement on the sample obtained in the step 9, and analyzing and comparing the obtained result to determine that the sample is plagioclase crystal, is a triclinic system and has a space group of C- ī;
and 10, cutting the obtained sample into a slice, polishing the two sides of the slice to obtain a thickness of 300 mu m, and measuring the water content and distribution of the sample by using a Fourier infrared spectrometer to obtain a result which shows that the sample has characteristic peaks of structural water and is uniformly distributed.
In the step 5, when distilled water or deionized water is added by a pipette, the water is in the following amount: 0.1-0.5. Mu.l.
The invention has the beneficial effects that:
according to the invention, the gold foil is rolled into the straight cylinder to serve as the inner tube directly contacting with the sample, so that the conventional gold tube or platinum tube is replaced, the cost is reduced, the manufacturing is simple, the limitation of the size of the noble metal tube is avoided, and the sample tubes with different sizes can be rolled at will; meanwhile, the copper tube outside the gold foil tube is convenient to process, the cost is very low, and the primary copper tube and the secondary copper tube with the bottom with certain thickness are sleeved together and welded, so that water in a sample can be completely sealed, and the water content of the sample is accurately controlled due to the loss of water in the welding process and the high-temperature high-pressure pressing process is avoided; the synthesized sample has larger size, and can be polished into various sizes according to measurement requirements for various analysis tests. The synthesized water-containing plagioclase sample has the characteristics of large sample size, uniform particle size, high purity, uniform water distribution and the like, and provides important sample support for experimental study of physical properties, geochemical behaviors and circulation of middle and lower crust water.
The method solves the technical problems that the sample size is limited, the water content of the sample is controlled inaccurately, the experiment cost is high and the like in the synthesis of the water-containing plagioclase solid solution in the prior art.
Description of the drawings:
FIG. 1 is a scanning electron microscope image of the prepared water-containing plagioclase.
The specific embodiment is as follows:
examples: an aqueous plagioclase solid solution (An 20 ，Na 0.8 Ca 0.2 Al 1.2 Si 2.8 O 8 ) Comprising the steps of:
step 1, according to the albite (NaAlSi) in the plagioclase feldspar solid solution 3 O 8 ) Anorthite (CaAl) 2 Si 2 O 8 ) The molar ratio of (2) is 4:1, respectively weighing the initial raw materials of the stoichiometric ratio of the albite and the anorthite corresponding to the weight as Al 2 O 3 ,SiO 2 ,Na 2 CO 3 And CaCO (CaCO) 3 Grinding and uniformly mixing high-purity oxide powder in alcohol by using an agate mortar, and drying in a 200 ℃ oven for 4 hours;
the oxide raw materials are selected based on the fact that the raw materials are relatively simple in composition, some impurity elements are not added, and the cost is low; meanwhile, the corrosion is avoided, and the safety is ensured; unlike some acid-base reagents, corrosiveness can be created during the manufacturing process.
Step 2, synthesizing plagioclase glass at high temperature: in order to obtain a pure glass sample and avoid the residue of the initial raw materials, the mixture powder in the step 1 is pressed into a cylinder with the diameter of 13 multiplied by 2mm by a tablet press, so that the raw materials are in closer contact and react more fully at high temperature to generate a pure glass phase; after being in close contact, the initial raw materials are fully reacted at a high temperature, then the sample is placed in a platinum crucible, the platinum crucible is placed in a high temperature furnace, decarbonized at 1000-1200 ℃ for reaction for 10-12h, then the temperature is raised to 1600 ℃ to enable the mixture to be molten into a glassy state, and then the temperature is reduced to room temperature; the decarbonizing reaction is carried out in the closed high-temperature furnace, so that impurities and moisture are not introduced in the cooling process; ensures the preparation of transparent, bubble-free and residual reactant-free homogeneous glass.
Step 3, preparing plagioclase glass powder: step 2, obtaining transparent uniform glass without bubbles and residual reactants, crushing the glass on a tablet press by a platinum crucible filled with transparent plagioclase glass, and then putting the glass into a high-frequency vibration ball mill to be ground into uniform powder with the particle size of 5-10 mu m; and then drying in a 100 ℃ oven for about two hours, wherein the sample is always dried in the oven until the sample is assembled.
Step 4, preparing a primary copper tube and a secondary copper tube: preparing a first red copper inner tube with an inner diameter of 6mm, a wall thickness of 0.5mm, a height of 12mm and a bottom thickness of 0.5; preparing a red copper outer tube II with the inner diameter of 7.05mm, the wall thickness of 0.5mm, the height of 12.5mm and the bottom thickness of 0.5 mm; and the primary copper tubes and the secondary copper tubes with different sizes are required to be arranged according to the sizes of the sample sizes so as to match the sizes of the samples.
Step 5, assembling an aqueous sample: rolling a gold foil with the thickness of 0.05mm into a tube, putting the tube into the first red copper inner tube processed in the step 4, putting a gold foil wafer with the same thickness at the bottom, filling the plagioclase glass powder prepared in the step 3 into the first red copper inner tube prepared in the step 4, and adding 0.1-0.5 mu l of distilled water or deionized water into the tube by a liquid-transfering gun for synthesizing plagioclase with different water contents; according to the different amounts of water added, the plagioclase solid solutions with different water contents can be obtained.
During assembly, water is distributed on the surfaces of sample powder particles to form adsorbed water, then the sample powder is compacted, the water has fluidity, and the adsorbed water is uniformly present among the sample particles after the sample powder is compacted; and sealing with gold foil wafer; reversely buckling the red copper outer tube II with the inner diameter of 7.05mm prepared in the step 4 with the red copper inner tube I filled with the sample, and sealing the joint of the two copper tubes by using a laser welding machine;
step 6, high-temperature high-pressure synthesis and assembly: placing the sealed copper tube in the step 5 into a high-temperature high-pressure assembly block with the periphery composed of an h-BN tube and an h-BN plug pressure transmission medium, wherein the h-BN is hexagonal boron nitride; then placing the assembly block on a hexahedral top large press, and synthesizing a water-containing sample under the conditions that the temperature is 1100-1200 ℃ and the pressure is 1-2GPa, wherein the reaction time is 6-10h; the water-adsorbed plagioclase glass is converted into water-containing plagioclase crystals, which can be synthesized under the high-temperature and high-pressure conditions of the present invention. In the high-temperature high-pressure synthesis process, adsorbed water can enter a sample lattice to form structural water to occupy lattice positions. The temperature, pressure and time listed in the invention are synthesis conditions, and the conditions are key parameters of successful synthesis.
The high-temperature high-pressure synthesis device in the step 6 relates to the processing of h-BN tube, heater and medium-transmitting pyrophyllite blocks, and the specific operation comprises the following steps:
and 6.1, manufacturing an h-BN tube: processing an h-BN rod with the diameter of 11mm into an h-BN tube with the inner diameter of phi 8mm and the outer diameter of phi 11mm on a lathe, slightly polishing the inner diameter by sand paper, putting sealed red copper with a sample into the h-BN tube, and using h-BN discs with the diameter of phi 11mm and the thickness of 2mm at two ends;
step 6.2, manufacturing a heater: processing a graphite heating furnace with the inner diameter of phi 11mm, the outer diameter of 13mm and the height of 32.5mm on a lathe;
step 6.3, processing pyrophyllite: selecting a cubic pyrophyllite block with the side length of 32.5mm, and punching a circular through hole with the diameter of 13mm in the center;
step 6.4, assembling: the graphite heater is placed in pyrophyllite block, then the red copper sealing tube filled with the sample is placed in the boron carbide tube, and the red copper sealing tube and the graphite tube are placed together, and the two ends of the red copper sealing tube are sequentially sealed by the boron nitride plug and the pyrophyllite plug.
Step 6.5, drilling a small hole in the middle of the edge of the pyrophyllite block, and placing a thermocouple which can be directly contacted with the sample copper pipe for accurately controlling the experiment temperature;
step 7, after the step 6 is completed, turning off heating current to quench and cool, and then slowly reducing the pressure;
step 8, taking out the sample in the step 7, cutting the copper tube by using a diamond wire cutting machine, polishing the surface of the taken sample into a cylinder, and measuring related physical properties such as electrical property, elasticity and thermodynamic property;
step 9, performing powder XRD measurement on the sample obtained in the step 8, and analyzing and comparing the obtained result to determine that the sample is plagioclase crystal which is a triclinic system and the space group is C- ī;
and 10, cutting a sample obtained in the step 8 into small slices, polishing the two sides of the sample to a thickness of about 300 mu m, and measuring the water content and distribution of the sample by using a Fourier infrared spectrometer to obtain a result which shows that the sample has characteristic peaks of structural water and is uniformly distributed.
Claims (5)
1. A method for synthesizing aqueous plagioclase solid solution at high temperature and high pressure, comprising:
step 1, according to sodium feldspar NaAlSi in the plagioclase feldspar solid solution 3 O 8 And anorthite CaAl 2 Si 2 O 8 Respectively weighing the initial raw materials of the stoichiometric ratio of the albite and the anorthite corresponding to the weight of the raw materials to obtain Al 2 O 3 、SiO 2 、Na 2 CO 3 、 CaCO 3 Grinding and mixing the oxide powder in alcohol uniformly by an agate mortar, and drying the mixture in a baking oven at 200 ℃;
step 2, synthesizing plagioclase glass at high temperature: pressing the mixture powder in the step 1 into a cylinder with the diameter of 13 multiplied by 2mm, placing a sample in a platinum crucible, and placing the sample in a high-temperature furnace for decarbonizing reaction to obtain plagioclase glass at high temperature;
step 3, crushing the plagioclase glass in a platinum crucible filled with plagioclase glass on a tablet press, putting the plagioclase glass into a high-frequency vibration ball mill, grinding the plagioclase glass into powder with uniform particles, and then putting the powder into a baking oven for baking; the particle size is 5-10 mu m;
step 4, preparing a primary copper tube and a secondary copper tube: preparing a first red copper inner tube with an inner diameter of 6mm, a wall thickness of 0.5mm and a height of 12mm and a bottom thickness of 0.5; preparing a red copper outer tube II with the inner diameter of 7.05mm, the wall thickness of 0.5mm, the height of 12.5mm and the bottom thickness of 0.5 mm;
step 5, assembling an aqueous sample: rolling a gold foil with the thickness of 0.05 and mm into a tube, putting the tube into a first red copper inner tube, putting a gold foil wafer with the same thickness at the bottom, filling the plagioclase glass powder prepared in the step 3 into the first red copper inner tube prepared in the step 4, compacting sample powder after adding distilled water or deionized water into the tube by a pipette, and sealing the tube by the gold foil wafer; reversely buckling the red copper outer tube II with the inner diameter of 7.05mm prepared in the step 4 with the red copper inner tube I filled with the sample, and sealing the joint of the two copper tubes by using a laser welding machine; when distilled water or deionized water is added by a pipette, the water is in the following amount: 0.1-0.5. Mu.L;
step 6, high-temperature high-pressure synthesis and assembly: placing the sealed copper tube in the step 5 into a high-temperature high-pressure assembly block with the periphery composed of h-BN tubes and h-BN plug pressure transmission media;
step 7, placing the assembly block on a hexahedral top large press, and synthesizing a water-containing sample under the conditions of high temperature and high pressure; the method for synthesizing the water-containing sample under the high-temperature and high-pressure condition comprises the following steps: synthesizing a water-containing sample at 1100-1200 ℃ and 1-2 GPa; the reaction time is 6-10h;
and 8, after the step 7 is finished, turning off heating current to quench and cool, and slowly reducing the pressure to normal temperature to obtain a finished product.
2. The method for synthesizing the aqueous plagioclase solid solution at high temperature and high pressure according to claim 1, wherein: the method for carrying out the decarbonizing reaction in the high-temperature furnace comprises the following steps: decarbonizing at 1000-1200 deg.c for 10-12 hr, raising the temperature to 1600 deg.c, melting the mixture to glass state and lowering the temperature to room temperature; the high-temperature furnace is a closed high-temperature furnace.
3. The method for synthesizing the aqueous plagioclase solid solution at high temperature and high pressure according to claim 1, wherein: the method for drying in the oven in the step 3 is as follows: drying in a 100 ℃ oven for two hours; after drying, the sample is placed in an oven to be dried until the sample is assembled.
4. The method for synthesizing the aqueous plagioclase solid solution at high temperature and high pressure according to claim 1, wherein: the high-temperature high-pressure synthesis and assembly method in the step 6 comprises the following steps:
and 6.1, manufacturing an h-BN tube: processing an h-BN rod with the diameter of 11mm into an h-BN tube with the inner diameter of phi 8mm and the outer diameter of phi 11mm on a lathe, polishing the inner diameter by sand paper, putting sealed red copper filled with a sample into the h-BN tube, and plugging both ends by using h-BN wafers with the thickness of phi 11mm and 2 mm;
step 6.2, manufacturing a heater: processing a graphite heating furnace with the inner diameter of phi 11mm, the outer diameter of 13mm and the height of 32.5mm on a lathe;
step 6.3, processing pyrophyllite: selecting a cubic pyrophyllite block with the side length of 32.5 and mm, and punching a circular through hole with the diameter of 13mm in the center;
step 6.4, assembling: placing a graphite heating furnace in a pyrophyllite block, then placing a red copper sealing tube filled with a sample into a boron carbide tube, and placing the red copper sealing tube and the boron carbide tube together in the graphite heating furnace, wherein two ends of the red copper sealing tube are respectively sealed by a boron nitride plug and a pyrophyllite plug in sequence;
and 6.5, drilling a small hole in the middle of the edge of the pyrophyllite block, and placing a thermocouple which can be directly contacted with the sample copper pipe for accurately controlling the experiment temperature.
5. The method for synthesizing the aqueous plagioclase solid solution at high temperature and high pressure according to claim 1, wherein: further comprises:
step 9, taking out the sample in the step 8, cutting the copper tube by using a diamond wire cutting machine, taking out the sample, polishing the surface of the sample into a cylinder shape, and measuring relevant physical properties;
step 10, performing powder XRD measurement on the sample obtained in the step 9, and analyzing and comparing the obtained result to determine that the sample is plagioclase crystal, is a triclinic system and has a space group of C- ī; the obtained sample is cut into a slice, the thickness of the cut sample is 300 mu m after double-sided polishing, then the water content and distribution of the sample are measured by a Fourier infrared spectrometer, and the result shows that the sample has characteristic peaks of structural water and is uniformly distributed.
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| CN101164754A (en) * | 2006-10-18 | 2008-04-23 | 润弘精密工程事业股份有限公司 | Dry stirring light compartment wall grouting material |
| CN101570408A (en) * | 2009-05-26 | 2009-11-04 | 中冶实久建设有限公司 | Xigeda formation land rock mixed filling material and application thereof |
| US20110048286A1 (en) * | 2008-02-29 | 2011-03-03 | Allen Pratt | Cementitious compositions containing feldspar and pozzolanic particulate material, and method of making said composition |
| CN107337426A (en) * | 2017-07-10 | 2017-11-10 | 黑龙江火山岩科技有限公司 | Volcanic rock ceramic article and preparation method thereof |
| CN110082174A (en) * | 2019-04-09 | 2019-08-02 | 中国科学院地球化学研究所 | A kind of method of artificial synthesized plagioclase fluid inclusion |
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| CN101164754A (en) * | 2006-10-18 | 2008-04-23 | 润弘精密工程事业股份有限公司 | Dry stirring light compartment wall grouting material |
| US20110048286A1 (en) * | 2008-02-29 | 2011-03-03 | Allen Pratt | Cementitious compositions containing feldspar and pozzolanic particulate material, and method of making said composition |
| CN101570408A (en) * | 2009-05-26 | 2009-11-04 | 中冶实久建设有限公司 | Xigeda formation land rock mixed filling material and application thereof |
| CN107337426A (en) * | 2017-07-10 | 2017-11-10 | 黑龙江火山岩科技有限公司 | Volcanic rock ceramic article and preparation method thereof |
| CN110082174A (en) * | 2019-04-09 | 2019-08-02 | 中国科学院地球化学研究所 | A kind of method of artificial synthesized plagioclase fluid inclusion |
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