CN107675255B - A method of growing siderite monocrystalline at high temperature under high pressure - Google Patents
A method of growing siderite monocrystalline at high temperature under high pressure Download PDFInfo
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- CN107675255B CN107675255B CN201710787694.1A CN201710787694A CN107675255B CN 107675255 B CN107675255 B CN 107675255B CN 201710787694 A CN201710787694 A CN 201710787694A CN 107675255 B CN107675255 B CN 107675255B
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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
- C30B29/16—Oxides
- C30B29/22—Complex oxides
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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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Abstract
The invention discloses a kind of methods for growing siderite monocrystalline at high temperature under high pressure, using analytically pure ferric oxide powder and anhydrous oxalic acid, stoichiometrically molar ratio 1:1.5 weighing ground and mixed is uniform for it, 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 pipe, carries out high-temperature high-voltage reaction for assembling in block in high-pressure synthesis mounted in the sample assembly of h-BN pipe and being placed on the big press of cubic apparatus；Sample after reaction is taken out, opens platinum pipe using diamond cutter, natural air drying selects siderite monocrystalline under the microscope, and crystal is presented diamond shape plate, and 50-100 μm of average-size, 200 μm of full-size.The present invention solves the technical problem of current siderite crystal growth difficulty, while having the characteristics that experimental implementation is simple, experiment condition is easy to control.
Description
Technical field:
The present invention relates to mineral materials to synthesize field, more particularly to a kind of side for growing siderite monocrystalline at high temperature under high pressure
Method.
Background technique:
In recent years, greenhouse gases CO2Into atmospheric thermodynamics, the problem of leading to global warming, gets more and more people's extensive concerning, carbon
Hydrochlorate mineral as carbon storehouse maximum in earth's layers, its circulating effect in earth system global carbon system, institute
With the stability of the carbonate mineral in sedimentary rock and its existing morphological research are even more important.Magnesite is considered as one
Kind of the carbon being stabilized in Earth lays in form, studies have shown that the magnesite existing for lower mantle is often and siderite
(FeCO3) isomorph formation breunnerite.Although under high pressure, breunnerite can be kept with intrinsic trigonal crystal structure
Stable structure, but can cause the important physicals parameter such as its density, elasticity modulus that discrete change occurs with recurring structure phase transformation
Change, therefore, the phase of spin of breunnerite at high temperature under high pressure is under the research and foundation of lower mantle elasticity, seismic wave velocity
Earth mantle model has important value.
The end member phase important as breunnerite one, the siderite single crystal samples of free from admixture are to study the base of breunnerite
Plinth.Importantly, it reflects a kind of earth interior, there may be the carbonate mineral of perfect condition, outstanding other low spins
State delimit boundary for the maximum density and Bulk modulus of earth interior carbonate, and has been the low velocity of wave shape of Earth
State provides a kind of possible explanation.
Since siderite thermal stability is very poor, so that its crystal growth is extremely difficult, so that having no siderite monocrystalline so far
Growth and single crystal diffraction structured data report.Natural siderite sample generally all contains Ca2+、Mg2+、Mn2+Equal impurity,
Property research to siderite itself includes anisotropic elasticity modulus, seismic wave velocity, conductivity etc., and the influence of impurity is non-
Chang great influences bigger.Therefore, the method for exploring artificial synthesized high-purity siderite is the research necessary basis of siderite.
Existing patented technology, application number: 2016104708719, a method of it preparing siderite at high temperature under high pressure, makes
It uses analytically pure ferrous oxalate dihydrate as starting material, ferrous oxalate dihydrate powder is pressed into cylindrical body using tablet press machine, is made
It is wrapped up with silver foil and is made into sample, sodium chloride is ground into the powder of 200 mesh or more, be placed in baking oven at a temperature of 150 DEG C
Drying 2 hours, is made cylindrical samples for the sodium chloride powder after drying, and sample assembly in high-pressure synthesis assembling block and is put
It sets and carries out high-temperature high-voltage reaction in the big press of cubic apparatus, the sample after reaction is taken out, it is pure to get arriving to remove sample surfaces silver foil
Siderite.The siderite of this method preparation is powder crystal, cannot be used to the crystallographic properties of research material itself, and due to being made
Siderite product be powdered substance, hygroscopic, stability is poor.
Summary of the invention
The technical problem to be solved by the present invention is a kind of method for growing siderite monocrystalline at high temperature under high pressure is provided, with
The technical problem of current siderite crystal growth difficulty is solved, meanwhile, this method is simple with experimental implementation, experiment condition is easily-controllable
The features such as processed.
Technical solution of the present invention:
Step 1 uses analytically pure ferric oxide powder and anhydrous oxalic acid as starting material, stoichiometrically mole
It is more uniform than 1:1.5 ground and mixed；
Mix powder is pressed into cylinder using tablet press machine by step 2, then fills in cylindrical sample in platinum pipe,
Both ends are sealed using welding gun；
The sample that platinum seals is placed in h-BN pipe by step 3, using h-BN as transmission medium；
Step 4, by mounted in h-BN pipe sample assembly high-pressure synthesis assembling block in and be placed on the big press of cubic apparatus into
Row high-temperature high-voltage reaction, the temperature of high-temperature high-voltage reaction are 400 DEG C -1200 DEG C, pressure 1-4GPa, reaction time 12-40
A hour；
Step 5 takes out the sample after reaction, opens platinum pipe using diamond cutter, then natural air drying sample exists
Siderite monocrystalline is selected under microscope.
The concrete operations of step 3 are as follows: one hole of h-BN stick centre drill is made h-BN pipe on lathe, by platinum sealing
Sample is filled in pipe, and both ends are sealed by h-BN piece.
To include: mounted in method of the sample assembly of h-BN pipe in high-pressure synthesis assembling block described in step 4
Step 4.1 chooses one piece of pyrophyllite block, makes a circular through hole at pyrophyllite block center；
Step 4.2, in one circular graphitic heating furnace of circular through hole inner sleeve；
Step 4.3, the sample that the h-BN seal of tube is placed among graphite heater furnace；
Step 4.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug.
Thermocouple is provided in the assembling block of high-pressure synthesis described in step 4.
Siderite monocrystalline described in step 5 is single object phase, free from admixture phase.
Siderite monocrystalline described in step 5 is trigonal crystal structure, and space group is R-3c (no.167), lattice parameter Crystal presentation diamond shape plate, 50-100 μm of average-size, 200 μm of full-size.
Beneficial effects of the present invention:
The present invention combines geochemical knowledge background, i.e., in sedimentary rock under the reducing condition of certain temperature, pressure,
Bloodstone water and carbon dioxide there are in the environment of be slowly formed the principle of siderite, simulate siderite in laboratory conditions
Forming process, the chemical equation that this experiment is related to are as follows:
Fe2O3+H2C2O4- 2FeCO3+H2O
H2C2O4- H2O+CO2+CO
Wherein, excessive oxalic acid provides the CO atmosphere that siderite can be stabilized, and CO atmosphere can be di-iron trioxide
Powder and anhydrous oxalic acid redox reaction provide reduction atmosphere, the water and CO that excessive oxalic acid decomposes2For siderite list
The necessary condition of crystals growth.
Compared to natural siderite, because it contains Ca2+、Mg2+、Mn2+Equal impurity, existing report detect natural sparring
Mine degree of purity is extremely difficult to 90%, in addition, natural siderite absorbs water to form bloodstone due to containing a large amount of impurities easy weathering.
The present invention prepares the process of siderite monocrystalline, and laboratory environment is pure, and sample is in sealed environment, does not contact, obtains with impurity
The siderite monocrystalline arrived is pure substance, and not hygroscopic, chemical stability is good.
Compared to existing patented technology, application number: 2016104708719, a kind of side preparing siderite at high temperature under high pressure
Method, present invention has an advantage that first, raw material is ferrous oxalate dihydrate in existing patented technology, currently without business57The two of Fe
Water ferrous oxalate, raw material of the present invention can use commercially available57The Fe of Fe2O3As starting material, so as to further study
The isotope of carbonate57Fe fractionation effect；Second, the NaCl transmission medium used in existing patented technology, fusing point is low, for a long time
Crystallization is easy under high temperature and pressure influences its pressure transmission performance, and the present invention uses stability and the better h-BN conduct of pressure transmission performance
Transmission medium；The siderite of third, existing patented technology preparation is powder crystal, and prepared by the present invention is siderite monocrystalline, from material
Field, the property that monocrystalline is embodied be include crystallographic anisotropic essential attribute, compare powder crystal, monocrystalline can get
The information of more physics and chemistry.
To sum up, method of the invention has the advantages such as the simple, easily-controlled experimental conditions of operating process, the siderite of acquisition
Monocrystalline has the characteristics that purity is high, chemical stability be not good, hygroscopic, and this method is the anisotropic research of siderite monocrystalline
Important leverage is provided, solves the technical problem of current siderite crystal growth difficulty, single crystal size can satisfy diamond
Press the requirement of chamber Hi-pot test and single crystal diffraction etc..
Specific embodiment:
A method of growing siderite monocrystalline at high temperature under high pressure, it includes:
Step 1 uses analytically pure ferric oxide powder and anhydrous oxalic acid as starting material, stoichiometrically mole
It is more uniform than 1:1.5 ground and mixed；
Mix powder is pressed into Φ 5 × 3mm cylinder using tablet press machine by step 2, and cylindrical sample is then filled in Φ
5mm, thickness 0.1mm platinum pipe in, both ends are sealed using welding gun；
The sample that platinum seals is placed in h-BN pipe by step 3, using h-BN as transmission medium；
Step 4, by mounted in h-BN pipe sample assembly high-pressure synthesis assembling block in and be placed on the big press of cubic apparatus into
Row high-temperature high-voltage reaction, the temperature of high-temperature high-voltage reaction are 400 DEG C -1200 DEG C, pressure 1-4GPa, reaction time 12-40
A hour；
Step 5 takes out the sample after reaction, opens platinum pipe using diamond cutter, then natural air drying sample exists
Siderite monocrystalline is selected under microscope.
The concrete operations of step 3 are as follows: the hole for the h-BN stick centre drill Φ 5mm that size is Φ 10mm is made h- on lathe
BN pipe, the sample that platinum seals is filled in pipe, and both ends take Φ 5mm to seal with a thickness of the h-BN piece of 2mm.
To include: mounted in method of the sample assembly of h-BN pipe in high-pressure synthesis assembling block described in step 4
Step 4.1 chooses one piece of pyrophyllite block, makes a Φ 12mm circular through hole at pyrophyllite block center；
Step 4.2, in the circular graphitic heating furnace of one outer diameter Φ 12mm of circular through hole inner sleeve, internal diameter Φ 10mm；
Step 4.3, among graphite heater furnace place Φ 10mm the h-BN seal of tube sample；
Step 4.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug.
Thermocouple is provided in the assembling block of high-pressure synthesis described in step 4.
Siderite monocrystalline described in step 5 is single object phase, free from admixture phase.
Siderite monocrystalline described in step 5 is trigonal crystal structure, and space group is R-3c (no.167), lattice parameter Crystal presentation diamond shape plate, 50-100 μm of average-size, 200 μm of full-size.
Embodiment 1
Using analytically pure ferric oxide powder and anhydrous oxalic acid as starting material, by raw material with nonstoichiometric molar ratio
1:1.5 ground and mixed is uniform, is pressed at the end mixture (about 0.25g) cylindrical body (Φ 5mm × 3mm) using powder compressing machine, will
Cylindrical samples are filled in the platinum pipe of Φ 5mm, thickness 0.1mm, and both ends are sealed using welding gun.Using h-BN as transmission medium, by platinum
The sample of gold sealing is placed in h-BN pipe: the hole for the h-BN stick centre drill Φ 5mm that size is Φ 10mm being made h- on lathe
BN pipe, the sample that platinum seals is filled in pipe, and both ends take Φ 5mm to seal with a thickness of the h-BN piece of 2mm, completes high pressure assembling
Block.High pressure assembles block assembling mode:
1. the circular through hole that diameter is 12mm is made at the pyrophyllite block center of 32 × 32mm；
2. covering an outer diameter inside the circular through hole of pyrophyllite block is 12mm, internal diameter is the graphite heater furnace of 10mm；
3. the sample in h-BN pipe is put among graphite heater furnace, up and down for diameter be 10mm pyrophillite plug into
Row blocks.
So far, high pressure assembling block is completed, and the size that mesohigh assembling block is related to can be according to the sample in h-BN pipe
The sizes 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 assembling block of the present invention, is: 1. using thermocouple temperature control, the temperature that heating system is fed back by thermocouple
Degree adjusts heating power, to change temperature, the immediately monitoring to temperature is may be implemented in this method, is suitable for measuring essence to temperature
Spend demanding experiment；2. pyrophillite has good pressure transmission, machining property, heat insulation as level-one transmission medium
Property and insulating properties, h-BN are a kind of low sheraing materials, as second level transmission medium, keep the pressure in cavity relatively uniform, and its
Good airproof performance；3. graphite furnace, as heating furnace, temperature uniformity is high.
Assembling block is put into the big press of cubic apparatus and carries out high-temperature high-voltage reaction, sets pressure as 4GPa, set temperature is
1200 DEG C, reaction time 12h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, opens platinum using diamond cutter
Sample natural air drying is selected siderite monocrystalline by Jin Guan under the microscope.
Embodiment 2
Using analytically pure ferric oxide powder and anhydrous oxalic acid as starting material, by raw material with nonstoichiometric molar ratio
1:1.5 ground and mixed is uniform, is pressed at the end mixture (about 0.25g) cylindrical body (Φ 5mm × 3mm) using powder compressing machine, will
Cylindrical samples are filled in the platinum pipe of Φ 5mm, thickness 0.1mm, and both ends are sealed using welding gun.Using h-BN as transmission medium, by platinum
The sample of gold sealing is placed in h-BN pipe: the hole for the h-BN stick centre drill Φ 5mm that size is Φ 10mm being made h- on lathe
BN pipe, the sample that platinum seals is filled in pipe, and both ends take Φ 5mm to seal with a thickness of the h-BN piece of 2mm, completes high pressure assembling
Block.High pressure assembles block assembling mode:
1. the circular through hole that diameter is 12mm is made at the pyrophyllite block center of 32 × 32mm；
2. covering an outer diameter inside the circular through hole of pyrophyllite block is 12mm, internal diameter is the graphite heater furnace of 10mm；
3. the sample in h-BN pipe is put among graphite heater furnace, up and down for diameter be 10mm pyrophillite plug into
Row blocks.
So far, high pressure assembling block is completed, and the size that mesohigh assembling block is related to can be according to the sample in h-BN pipe
The sizes 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 assembling block of the present invention, is: 1. using thermocouple temperature control, the temperature that heating system is fed back by thermocouple
Degree adjusts heating power, to change temperature, the immediately monitoring to temperature is may be implemented in this method, is suitable for measuring essence to temperature
Spend demanding experiment；2. pyrophillite has good pressure transmission, machining property, heat insulation as level-one transmission medium
Property and insulating properties, h-BN are a kind of low sheraing materials, as second level transmission medium, keep the pressure in cavity relatively uniform, and its
Good airproof performance；3. graphite furnace, as heating furnace, temperature uniformity is high.
Assembling block is put into the big press of cubic apparatus and carries out high-temperature high-voltage reaction, sets pressure as 1GPa, set temperature is
400 DEG C, reaction time 40h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, opens platinum using diamond cutter
Sample natural air drying is selected siderite monocrystalline by Jin Guan under the microscope.
Embodiment 3
Using analytically pure ferric oxide powder and anhydrous oxalic acid as starting material, by raw material with nonstoichiometric molar ratio
1:1.5 ground and mixed is uniform, is pressed at the end mixture (about 0.25g) cylindrical body (Φ 5mm × 3mm) using powder compressing machine, will
Cylindrical samples are filled in the platinum pipe of Φ 5mm, thickness 0.1mm, and both ends are sealed using welding gun.Using h-BN as transmission medium, by platinum
The sample of gold sealing is placed in h-BN pipe: the hole for the h-BN stick centre drill Φ 5mm that size is Φ 10mm being made h- on lathe
BN pipe, the sample that platinum seals is filled in pipe, and both ends take Φ 5mm to seal with a thickness of the h-BN piece of 2mm, completes high pressure assembling
Block.High pressure assembles block assembling mode:
1. the circular through hole that diameter is 12mm is made at the pyrophyllite block center of 32 × 32mm；
2. covering an outer diameter inside the circular through hole of pyrophyllite block is 12mm, internal diameter is the graphite heater furnace of 10mm；
3. the sample in h-BN pipe is put among graphite heater furnace, up and down for diameter be 10mm pyrophillite plug into
Row blocks.
So far, high pressure assembling block is completed, and the size that mesohigh assembling block is related to can be according to the sample in h-BN pipe
The sizes 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 assembling block of the present invention, is: 1. using thermocouple temperature control, the temperature that heating system is fed back by thermocouple
Degree adjusts heating power, to change temperature, the immediately monitoring to temperature is may be implemented in this method, is suitable for measuring essence to temperature
Spend demanding experiment；2. pyrophillite has good pressure transmission, machining property, heat insulation as level-one transmission medium
Property and insulating properties, h-BN are a kind of low sheraing materials, as second level transmission medium, keep the pressure in cavity relatively uniform, and its
Good airproof performance；3. graphite furnace, as heating furnace, temperature uniformity is high.
Assembling block is put into the big press of cubic apparatus and carries out high-temperature high-voltage reaction, sets pressure as 3GPa, set temperature is
1000 DEG C, reaction time 30h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, opens platinum using diamond cutter
Sample natural air drying is selected siderite monocrystalline by Jin Guan under the microscope.
Claims (6)
1. a kind of method for growing siderite monocrystalline at high temperature under high pressure, it includes:
Step 1 uses analytically pure ferric oxide powder and anhydrous oxalic acid as starting material, stoichiometrically molar ratio 1:
1.5 ground and mixeds are uniform；
Mix powder is pressed into cylinder using tablet press machine by step 2, is then filled in cylindrical sample in platinum pipe, both ends
It is sealed using welding gun；
The sample that platinum seals is placed in h-BN pipe by step 3, using h-BN as transmission medium；
Step 4 will assemble in block in high-pressure synthesis mounted in the sample assembly of h-BN pipe and be placed on the big press progress height of cubic apparatus
Warm reaction under high pressure, the temperature of high-temperature high-voltage reaction are 400 DEG C -1200 DEG C, pressure 1-4GPa, and the reaction time is 12-40 small
When；
Step 5 takes out the sample after reaction, opens platinum pipe, natural air drying sample, then micro- using diamond cutter
Siderite monocrystalline is selected under mirror.
2. a kind of method for growing siderite monocrystalline at high temperature under high pressure according to claim 1, it is characterised in that: step
3 concrete operations are as follows: one hole of h-BN stick centre drill is made h-BN pipe on lathe, the sample that platinum seals is filled in into pipe
In, both ends are sealed by h-BN piece.
3. a kind of method for growing siderite monocrystalline at high temperature under high pressure according to claim 1, it is characterised in that: step
To include: mounted in method of the sample assembly of h-BN pipe in high-pressure synthesis assembling block described in 4
Step 4.1 chooses one piece of pyrophyllite block, makes a circular through hole at pyrophyllite block center；
Step 4.2, in one circular graphitic heating furnace of circular through hole inner sleeve；
Step 4.3, the sample that the h-BN seal of tube is placed among graphite heater furnace；
Step 4.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug.
4. a kind of method for growing siderite monocrystalline at high temperature under high pressure according to claim 1 or 3, it is characterised in that:
Thermocouple is provided in the assembling block of high-pressure synthesis described in step 4.
5. a kind of method for growing siderite monocrystalline at high temperature under high pressure according to claim 1, it is characterised in that: step
The 5 siderite monocrystalline are single object phase, free from admixture phase.
6. a kind of method for growing siderite monocrystalline at high temperature under high pressure according to claim 1, it is characterised in that: step
The 5 siderite monocrystalline are trigonal crystal structure, and space group is R-3c (no.167), lattice parameter Crystal presentation diamond shape plate, 50-100 μm of average-size, 200 μm of full-size.
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| CN106082350A (en) * | 2016-06-24 | 2016-11-09 | 中国科学院地球化学研究所 | A kind of method preparing siderite at high temperature under high pressure |
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