CN107400916A - A kind of method for growing dolomite monocrystalline at high temperature under high pressure - Google Patents
A kind of method for growing dolomite monocrystalline at high temperature under high pressure Download PDFInfo
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- CN107400916A CN107400916A CN201710788071.6A CN201710788071A CN107400916A CN 107400916 A CN107400916 A CN 107400916A CN 201710788071 A CN201710788071 A CN 201710788071A CN 107400916 A CN107400916 A CN 107400916A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/12—Single-crystal growth directly from the solid state by pressure treatment during the growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
Abstract
The invention discloses a kind of method for growing dolomite monocrystalline at high temperature under high pressure, it uses analytically pure magnesia, calcium carbonate powder and anhydrous oxalic acid ground and mixed to be uniformly used as initiation material, mixture is pressed into cylinder using tablet press machine, then cylindrical sample is filled in platinum pipe, both ends are sealed using welding gun, using h BN as transmission medium, the sample that platinum seals is placed in h BN pipes, in high-pressure synthesis assembles block and the big press of cubic apparatus will be placed on carries out high-temperature high-voltage reaction mounted in the sample assembly of h BN pipes;Reacted sample is taken out, opens platinum pipe using diamond cutting knife, natural air drying selects dolomite monocrystalline under the microscope, and rhombus tabular, 50 100 μm of average-size, 200 μm of full-size is presented in crystal.The present invention solves the difficult technical barrier of current dolomite crystal growth.
Description
Technical field:
The present invention relates to mineral material to synthesize field, more particularly to a kind of side for growing dolomite monocrystalline at high temperature under high pressure
Method.
Background technology:
In recent years, greenhouse gases CO2Into atmospheric thermodynamics, the problem of causing global warming, gets more and more people's extensive concerning, carbon
For hydrochlorate mineral as carbon storehouse maximum in earth's layers, its circulating effect in earth system global carbon system, institute
So that the stability of the carbonate mineral in sedimentary rock and its existing morphological research are even more important.Dolomite is as a kind of heavy
Common carbonate mineral in product rock, its chemical composition is CaCO3·MgCO3, because dolomite heat endurance is poor so that its
Crystal growth is extremely difficult, forefathers are relatively fewer to the research of the Forming Mechanism of dolomite, so far and prosthetic dolomite monocrystalline
Growth and the report of single crystal diffraction structured data.Natural dolomite sample typically all contains Fe2+、Mn2+、Zn2+It is right Deng impurity
The property research of dolomite in itself influences bigger.Therefore, the method for exploring artificial synthesized high-purity dolomite is research white clouds
The necessary basis of stone.
The content of the invention
The technical problem to be solved in the present invention is:A kind of method for growing dolomite monocrystalline at high temperature under high pressure is provided, with
Solve the difficult technical barrier of current dolomite crystal growth, meanwhile, this method has that experimental implementation is simple, experiment condition is easily-controllable
The features such as processed.
Technical solution of the present invention:
Step 1, using analytically pure magnesia, calcium carbonate powder and anhydrous oxalic acid ground and mixed uniformly it is used as starting former
Material;
Step 2, using tablet press machine mix powder is pressed into cylinder, then filled in cylindrical sample in platinum pipe,
Both ends are sealed using welding gun;
Step 3, by platinum seal sample be placed in h-BN pipes, using h-BN as transmission medium;
Step 4, in high-pressure synthesis assembles block and the big press of cubic apparatus will be placed on enter mounted in the sample assembly of h-BN pipes
Row high-temperature high-voltage reaction, the temperature of high-temperature high-voltage reaction is 400 DEG C -700 DEG C, pressure 0.2-1GPa, reaction time 12-30
Individual hour;
Step 5, reacted sample taken out, use diamond cutting knife to open platinum pipe, natural air drying sample, Ran Hou
Dolomite monocrystalline is selected under microscope.
The concrete operations of step 3 are:One hole of h-BN rods centre drill is made h-BN pipes on lathe, by platinum sealing
Sample is filled in pipe, and both ends seal by h-BN pieces.
The method mounted in the sample assembly of h-BN pipes in high-pressure synthesis assembles block is included described in step 4:
Step 4.1, one piece of pyrophyllite block is chosen, a manhole is made at pyrophyllite block center;
Step 4.2, in one circular graphitic heating furnace of manhole inner sleeve;
Step 4.3, the sample for placing among graphite heater furnace the h-BN seals of tube;
Step 4.4, by circular graphitic heating furnace upper and lower ends with pyrophillite plug seal.
Thermocouple is provided with high-pressure synthesis assembling block described in step 4.
Dolomite monocrystalline described in step 5 is single thing phase, free from admixture phase.
Dolomite monocrystalline described in step 5 is trigonal crystal structure, and space group is R-3c (no.167), lattice parameter Rhombus tabular, 60-100 μm of average-size, 200 μm of full-size is presented in crystal.
Beneficial effects of the present invention:
The present invention combine geochemical knowledge background, i.e., in sedimentary rock under conditions of certain temperature, pressure, calcium from
Son and magnesium ion are slowly formed the principle of dolomite, tested under environment existing for water and carbon dioxide and biological agent
The forming process of room condition Imitating dolomite, the chemical equation that this experiment is related to are:
CaCO3+MgO+H2C2O4- CaCO3·MgCO3+CO+H2O
H2C2O4- H2O+CO2+CO
Wherein, excessive oxalic acid provides the CO that dolomite can be stabilized2Atmosphere, while be also dolomite crystal growth
Provide the fluid of water.
Compared to natural dolomite, because it contains Fe2+、Mn2+、Zn2+Deng impurity, existing report detects natural white clouds
Stone degree of purity is extremely difficult to 90%, in addition, natural dolomite containing a large amount of impurity due to easily absorbing water weathering.Present invention growth
The process of dolomite monocrystalline, laboratory environment is pure, and sample is in sealed environment, is not contacted with impurity, obtained dolomite
Monocrystalline is pure substance, not hygroscopic, and chemical stability is good, and important guarantor is provided for the anisotropic research of dolomite monocrystalline
Barrier, solves the difficult technical barrier of current dolomite crystal growth.In addition, the method for the present invention have operating process it is simple,
The advantages such as easily-controlled experimental conditions.
Embodiment:
A kind of method for growing dolomite monocrystalline at high temperature under high pressure, it includes:
Step 1:Use analytically pure magnesia, calcium carbonate powder and anhydrous oxalic acid (1:1:1.3) ground and mixed is uniformly made
For initiation material;
Step 2:Mix powder is pressed into 5 × 3mm of Φ cylinders using tablet press machine, cylindrical sample is then filled in into Φ
5mm, thick 0.1mm platinum pipe in, both ends are sealed using welding gun;
Step 3, by platinum seal sample be placed in h-BN pipes, using h-BN as transmission medium;
Step 4, in high-pressure synthesis assembles block and the big press of cubic apparatus will be placed on enter mounted in the sample assembly of h-BN pipes
Row high-temperature high-voltage reaction, the temperature of high-temperature high-voltage reaction is 400 DEG C -700 DEG C, pressure 0.2-1GPa, reaction time 12-30
Individual hour;
Step 5, reacted sample taken out, use diamond cutting knife to open platinum pipe, natural air drying sample, Ran Hou
Dolomite monocrystalline is selected under microscope.
The concrete operations of step 3 are:The hole for the h-BN rod centre drill Φ 5mm that size is Φ 10mm is made h- on lathe
BN is managed, and the sample that platinum seals is filled in pipe, and both ends take the h-BN pieces that Φ 5mm thickness is 2mm to seal.
The method mounted in the sample assembly of h-BN pipes in high-pressure synthesis assembles block is included described in step 4:
Step 4.1, one piece of pyrophyllite block is chosen, a Φ 12mm manhole is made at pyrophyllite block center;
Step 4.2, in one external diameter Φ 12mm of manhole inner sleeve, internal diameter Φ 10mm circular graphitic heating furnace;
Step 4.3, place among graphite heater furnace Φ 10mm the h-BN seals of tube sample;
Step 4.4, by circular graphitic heating furnace upper and lower ends with pyrophillite plug seal.
Thermocouple is provided with high-pressure synthesis assembling block described in step 4.
Dolomite monocrystalline described in step 5 is single thing phase, free from admixture phase.
Dolomite monocrystalline described in step 5 is trigonal crystal structure, and space group is R-3c (no.167), lattice parameter Rhombus tabular, 60-100 μm of average-size, 200 μm of full-size is presented in crystal.
Embodiment 1
With analytically pure magnesia, calcium carbonate powder and anhydrous oxalic acid stoichiometrically mol ratio 1:1:1.3 match somebody with somebody abrasive lapping
It is well mixed to be used as initiation material, mixture (about 0.25g) end is pressed into cylinder (Φ 5mm × 3mm) using powder compressing machine,
Sample is filled in Φ 5mm, thick 0.1mm platinum pipe, both ends are sealed using welding gun.It is using h-BN as transmission medium, platinum is close
The sample of envelope is placed in h-BN pipes:The hole for the h-BN rod centre drill Φ 5mm that size is Φ 10mm is made h-BN pipes on lathe,
The sample that platinum seals is filled in pipe, both ends take the h-BN pieces that Φ 5mm thickness is 2mm to seal, and complete high pressure assembling block.High pressure
Assemble block assembling mode:
1. a diameter of 12mm manhole is made at 32 × 32mm pyrophyllite block center;
2. one external diameter of set is 12mm inside the manhole of pyrophyllite block, internal diameter is 10mm graphite heater furnace;
It is to be entered with a diameter of 10mm pyrophillite plug up and down 3. putting the sample in h-BN pipes among graphite heater furnace
Row closure.
So far, high pressure assembling block is completed, and the size that its mesohigh assembling block is related to can be according to the sample in h-BN pipes
The size of product specifically determines;In the assembling block, pyrophillite and h-BN make transmission medium, and graphite furnace makees heating furnace, and thermocouple is made
Temperature regulating device.The advantages of high pressure of the present invention assembling block is:1. use thermocouple temperature control, the temperature that heating system is fed back by thermocouple
Degree regulation heating power, so as to change temperature, this method can realize the immediately monitoring to temperature, suitable for temperature survey essence
Degree requires high experiment;2. pyrophillite has good pressure transmission, machining property, heat insulation as one-level transmission medium
Property and insulating properties, h-BN are a kind of low sheraing materials, as two level transmission medium, make the pressure ratio in cavity more uniform, and its
Good airproof performance;3. graphite furnace is high as heating furnace, temperature homogeneity.
Assembling block is put into the big press of cubic apparatus and carries out high-temperature high-voltage reaction, sets pressure as 1GPa, design temperature is
700 DEG C, reaction time 12h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, platinum is opened using diamond cutting knife
Jin Guan, by sample natural air drying, dolomite monocrystalline is selected under the microscope.
Embodiment 2
With analytically pure magnesia, calcium carbonate powder and anhydrous oxalic acid stoichiometrically mol ratio 1:1:1.3 match somebody with somebody abrasive lapping
It is well mixed to be used as initiation material, mixture (about 0.25g) end is pressed into cylinder (Φ 5mm × 3mm) using powder compressing machine,
Sample is filled in Φ 5mm, thick 0.1mm platinum pipe, both ends are sealed using welding gun.It is using h-BN as transmission medium, platinum is close
The sample of envelope is placed in h-BN pipes:The hole for the h-BN rod centre drill Φ 5mm that size is Φ 10mm is made h-BN pipes on lathe,
The sample that platinum seals is filled in pipe, both ends take the h-BN pieces that Φ 5mm thickness is 2mm to seal, and complete high pressure assembling block.High pressure
Assemble block assembling mode:
1. a diameter of 12mm manhole is made at 32 × 32mm pyrophyllite block center;
2. one external diameter of set is 12mm inside the manhole of pyrophyllite block, internal diameter is 10mm graphite heater furnace;
It is to be entered with a diameter of 10mm pyrophillite plug up and down 3. putting the sample in h-BN pipes among graphite heater furnace
Row closure.
So far, high pressure assembling block is completed, and the size that its mesohigh assembling block is related to can be according to the sample in h-BN pipes
The size of product specifically determines;In the assembling block, pyrophillite and h-BN make transmission medium, and graphite furnace makees heating furnace, and thermocouple is made
Temperature regulating device.The advantages of high pressure of the present invention assembling block is:1. use thermocouple temperature control, the temperature that heating system is fed back by thermocouple
Degree regulation heating power, so as to change temperature, this method can realize the immediately monitoring to temperature, suitable for temperature survey essence
Degree requires high experiment;2. pyrophillite has good pressure transmission, machining property, heat insulation as one-level transmission medium
Property and insulating properties, h-BN are a kind of low sheraing materials, as two level transmission medium, make the pressure ratio in cavity more uniform, and its
Good airproof performance;3. graphite furnace is high as heating furnace, temperature homogeneity.
Assembling block is put into the big press of cubic apparatus and carries out high-temperature high-voltage reaction, sets pressure as 0.2GPa, design temperature
For 400 DEG C, reaction time 30h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, opened using diamond cutting knife
Platinum pipe, by sample natural air drying, dolomite monocrystalline is selected under the microscope.
Embodiment 3
With analytically pure magnesia, calcium carbonate powder and anhydrous oxalic acid stoichiometrically mol ratio 1:1:1.3 match somebody with somebody abrasive lapping
It is well mixed to be used as initiation material, mixture (about 0.25g) end is pressed into cylinder (Φ 5mm × 3mm) using powder compressing machine,
Sample is filled in Φ 5mm, thick 0.1mm platinum pipe, both ends are sealed using welding gun.It is using h-BN as transmission medium, platinum is close
The sample of envelope is placed in h-BN pipes:The hole for the h-BN rod centre drill Φ 5mm that size is Φ 10mm is made h-BN pipes on lathe,
The sample that platinum seals is filled in pipe, both ends take the h-BN pieces that Φ 5mm thickness is 2mm to seal, and complete high pressure assembling block.High pressure
Assemble block assembling mode:
1. a diameter of 12mm manhole is made at 32 × 32mm pyrophyllite block center;
2. one external diameter of set is 12mm inside the manhole of pyrophyllite block, internal diameter is 10mm graphite heater furnace;
It is to be entered with a diameter of 10mm pyrophillite plug up and down 3. putting the sample in h-BN pipes among graphite heater furnace
Row closure.
So far, high pressure assembling block is completed, and the size that its mesohigh assembling block is related to can be according to the sample in h-BN pipes
The size of product specifically determines;In the assembling block, pyrophillite and h-BN make transmission medium, and graphite furnace makees heating furnace, and thermocouple is made
Temperature regulating device.The advantages of high pressure of the present invention assembling block is:1. use thermocouple temperature control, the temperature that heating system is fed back by thermocouple
Degree regulation heating power, so as to change temperature, this method can realize the immediately monitoring to temperature, suitable for temperature survey essence
Degree requires high experiment;2. pyrophillite has good pressure transmission, machining property, heat insulation as one-level transmission medium
Property and insulating properties, h-BN are a kind of low sheraing materials, as two level transmission medium, make the pressure ratio in cavity more uniform, and its
Good airproof performance;3. graphite furnace is high as heating furnace, temperature homogeneity.
Assembling block is put into the big press of cubic apparatus and carries out high-temperature high-voltage reaction, sets pressure as 0.5GPa, design temperature
For 500 DEG C, reaction time 30h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, opened using diamond cutting knife
Platinum pipe, by sample natural air drying, dolomite monocrystalline is selected under the microscope.
Claims (6)
1. a kind of method for growing dolomite monocrystalline at high temperature under high pressure, it includes:
Step 1, using analytically pure magnesia, calcium carbonate powder and anhydrous oxalic acid ground and mixed uniformly it is used as initiation material;
Step 2, using tablet press machine mix powder is pressed into cylinder, then filled in cylindrical sample in platinum pipe, both ends
Sealed using welding gun;
Step 3, by platinum seal sample be placed in h-BN pipes, using h-BN as transmission medium;
Step 4, by mounted in the sample assembly of h-BN pipes in high-pressure synthesis assembles block and be placed on the big press of cubic apparatus carry out it is high
Warm reaction under high pressure, the temperature of high-temperature high-voltage reaction is 400 DEG C -700 DEG C, pressure 0.2-1GPa, and the reaction time is 12-30 small
When;
Step 5, reacted sample taken out, use diamond cutting knife to open platinum pipe, natural air drying sample, then micro-
Dolomite monocrystalline is selected under mirror.
A kind of 2. method for growing dolomite monocrystalline at high temperature under high pressure according to claim 1, it is characterised in that:Step
3 concrete operations are:One hole of h-BN rods centre drill is made h-BN pipes on lathe, the sample that platinum seals is filled in into pipe
In, both ends seal by h-BN pieces.
A kind of 3. method for growing dolomite monocrystalline at high temperature under high pressure according to claim 1, it is characterised in that:Step
The method mounted in the sample assembly of h-BN pipes in high-pressure synthesis assembles block is included described in 4:
Step 4.1, one piece of pyrophyllite block is chosen, a manhole is made at pyrophyllite block center;
Step 4.2, in one circular graphitic heating furnace of manhole inner sleeve;
Step 4.3, the sample for placing among graphite heater furnace the h-BN seals of tube;
Step 4.4, by circular graphitic heating furnace upper and lower ends with pyrophillite plug seal.
A kind of 4. method for growing dolomite monocrystalline at high temperature under high pressure according to claim 1 or 3, it is characterised in that:
Thermocouple is provided with high-pressure synthesis assembling block described in step 4.
A kind of 5. method for growing dolomite monocrystalline at high temperature under high pressure according to claim 1, it is characterised in that:Step
The 5 dolomite monocrystalline are single thing phases, free from admixture phase.
A kind of 6. method for growing dolomite monocrystalline at high temperature under high pressure according to claim 1, it is characterised in that:Step
The 5 dolomite monocrystalline are trigonal crystal structure, and space group is R-3c (no.167), lattice parameter Rhombus tabular, 60-100 μm of average-size, 200 μm of full-size is presented in crystal.
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CN114232068A (en) * | 2021-12-08 | 2022-03-25 | 中国科学院地球化学研究所 | Method for preparing magnalium garnet single crystal under high-temperature and high-pressure conditions |
CN114318489A (en) * | 2021-12-09 | 2022-04-12 | 中国科学院地球化学研究所 | Preparation method for preparing calcium aluminum garnet single crystal under high-temperature and high-pressure conditions |
CN114318491A (en) * | 2021-12-09 | 2022-04-12 | 中国科学院地球化学研究所 | Method for preparing wollastonite single crystal under high-temperature and high-pressure conditions |
CN114318489B (en) * | 2021-12-09 | 2023-02-14 | 中国科学院地球化学研究所 | Preparation method for preparing calcium aluminum garnet single crystal under high-temperature and high-pressure conditions |
CN114318491B (en) * | 2021-12-09 | 2023-02-28 | 中国科学院地球化学研究所 | Method for preparing wollastonite single crystal under high-temperature and high-pressure conditions |
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