CN108793259A - A method of synthesizing nemalite at high temperature under high pressure - Google Patents
A method of synthesizing nemalite at high temperature under high pressure Download PDFInfo
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- CN108793259A CN108793259A CN201810622473.3A CN201810622473A CN108793259A CN 108793259 A CN108793259 A CN 108793259A CN 201810622473 A CN201810622473 A CN 201810622473A CN 108793259 A CN108793259 A CN 108793259A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
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Abstract
The invention discloses a kind of methods synthesizing nemalite at high temperature under high pressure, using analytically pure magnesium hydroxide, analytically pure iron powder Fe and analytically pure iron hydroxide with molar ratio 27：1：2 ground and mixeds are uniformly used as starting material；It is pressed into cylindrical sample using tablet press machine starting material, analytically pure iron powder is separately taken to be pressed into two pieces of iron plates, then cylindrical sample and iron plate are put into the sandwich structure of iron plate-cylindrical sample-iron plate in platinum snap fastener and are sealed, it will finally be sealed in pellet in a shotgun cartridge female thread that platinum snap fastener is fitted into, pellet in a shotgun cartridge female thread is placed in h-BN pipes, using h-BN as transmission medium；H-BN pipes are assembled in high-pressure synthesis assembling block and are placed on the big press of cubic apparatus into 600-700 DEG C of trip temperature, pressure 3GPa, reaction time 8h high-temperature high-voltage reaction are single object phase to get nemalite sample, free from admixture phase solves the problems, such as that current nemalite sample can not be artificial synthesized.
Description
Technical field
The present invention relates to geoscience high temperature and pressure research fields, and in particular to one kind synthesizing iron-bearing water at high temperature under high pressure
The method of magnesite.
Background technology
Shepardite is a kind of most common enhydrite of nature.It is the representative cryogenic in a kind of serpentinite or dolomite
Hydrothermal alteration mineral, mineral shape is in the form of sheets or fibrous agrregate.It is easy to be substituted by iron (or manganese) in shepardite mineral structure
Form iron content (or manganese) shepardite.Wherein, nemalite has extremely important researching value, iron content in field of earth sciences
The chemical formula of shepardite is (Mg0.9Fe0.1)(OH)2。
Experimental study shows traditional anhydrous mafite (such as olivine) of name in nature often to contain a small amount of structure
The form of water exists, i.e., the coordination oxygen of metallic element is substituted by hydroxyl in crystal structure, and the result of replacement makes the electricity of mineral
Conductance dramatically increases, and also has large effect to its elasticity and velocity of wave.And nemalite provides the rich hydroxyl of an extreme
Carrier provides a kind of possibility of hydroxyl replacement coordination oxygen, and therefore, it is the important forerunner for synthesizing other aqueous ferromagnesian minerals
Body.Importantly, recently about core-mantle boundary peromag iron (MgFe) O2Existing possibility and earth early stage core curtain
The discussion of differentiation redox environment has become the problem in science of the hottest point of field of earth sciences.Experiment shows Tie Heshui
High-temperature high-voltage reaction and the high temperature and pressure phase transformation reaction of FeOOH FeOOH can obtain peroxide of iron FeO2, but
Its process is difficult to be connected with subducting plate.Compare, nemalite as the common enhydrite of subduction zone more likely
Into Earth, its dehydration under superhigh-temperature and-pressure may directly obtain peromag iron, be peromag iron and plate
The contact that block dives provides definitely experimental basis.
However, the chemical stability due to ferrous hydroxide is very poor, conventional laboratory conditions be difficult control ferrous hydroxide and
The solid solution of magnesium hydroxide, it is extremely difficult that this so that the sample of nemalite synthesizes, and there has been no nemalite synthesis at present
Report.Due to the shortcoming of artificial synthesized nemalite sample technology, lack the sample of high-purity nemalite so that iron content
Experimental study of the shepardite under high-temperature and high-pressure conditions can not be carried out.
Invention content
The technical problem to be solved by the present invention is to：A kind of method synthesizing nemalite at high temperature under high pressure is provided, with
Solve the problems, such as that current nemalite sample can not be artificial synthesized.
The technical scheme is that：A method of it synthesizing nemalite at high temperature under high pressure, includes the following steps：
Step 1 uses analytically pure magnesium hydroxide Mg (OH)2, analytically pure iron powder Fe and analytically pure iron hydroxide Fe
(OH)3With molar ratio 27：1：2 ground and mixeds are uniformly used as starting material；
Mix powder in step 1 is pressed into Φ 5 × 2mm cylindrical samples by step 2 using tablet press machine, separately takes analysis
Pure iron powder is pressed into the iron plate of two pieces of 5 × 1mm of Φ, then by cylindrical sample and iron plate with iron plate-cylindrical sample-iron plate
Sandwich structure is put into Φ 5mm, thickness 0.1mm platinum snap fasteners and seals, and platinum snap fastener is finally packed into Φ 5.5mm, thickness
It is sealed in the pellet in a shotgun cartridge female thread of 0.2mm, pellet in a shotgun cartridge female thread is placed in h-BN pipes, using h-BN as transmission medium；
The h-BN pipes that sample is housed in step 2 are assembled in high-pressure synthesis assembling block and to be placed on cubic apparatus big by step 3
Press carries out high-temperature high-voltage reaction；
Step 4 takes out the pellet in a shotgun cartridge female thread in step 3, is sawed with diamond low speed and opens pellet in a shotgun cartridge female thread, takes out cylindrical sample
Product obtain nemalite sample.
The production method concrete operations of h-BN pipes described in step 2 are：In the h-BN sticks for being Φ 10mm by size on lathe
The hole that the heart bores Φ 6mm is made h-BN pipes, and sample is filled in pipe, and both ends take the h-BN pieces that Φ 6mm thickness is 2mm to seal.
The high-pressure synthesis that is assembled in h-BN pipes described in step 3 assembles method concrete operations in the block and includes：
Step 3.1 chooses one piece of pyrophyllite block, and a Φ 12mm circular through hole is made at pyrophyllite block center；
Step 3.2, in the circular graphitic heating furnace of one outer diameter Φ 12mm of circular through hole inner sleeve, internal diameter Φ 10mm；
Step 3.3, placed among graphite heater furnace Φ 10mm the h-BN seals of tube sample；
Step 3.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug.
The temperature of high-temperature high-voltage reaction described in step 3 is 600-700 DEG C, pressure 3GPa, reaction time 8h.
The nemalite sample obtained described in step 4 is single object phase, and free from admixture phase, nemalite is six sides knot
Structure, space group P-3m1, lattice parameter
Beneficial effects of the present invention：
The present invention obtains nemalite sample using high temperature and pressure solid phase reaction, and reaction is
1/3Fe+2/3Fe(OH)3—Fe(OH)2
0.1Fe(OH)2+0.9Mg(OH)2—(Mg0.9Fe0.1)(OH)2
It is designed using iron and platinum Shuangzi female thread, uses the oxygen fugacity in a large amount of iron control sample cavity, it is ensured that reacted
The chemical stability of ferrous hydroxide in journey.Wherein, the effect of outermost layer pellet in a shotgun cartridge female thread is that the oxygen blocked in external environment enters
Sample cavity；The effect of platinum snap fastener is isolation magnesium hydroxide and pellet in a shotgun cartridge female thread, since magnesium hydroxide belongs to highly basic, high temperature and pressure
Under the conditions of can corrode pellet in a shotgun cartridge female thread, you must use platinum isolation protection；The purpose of mono- iron plate of Ge Jia above and below in sample cavity
It is to provide necessary buffer using the oxygen fugacity in a large amount of iron simple substance control chamber body for ferrous hydroxide.
The method of high temperature and pressure has the advantages such as the simple, easily-controlled experimental conditions of operating process, the iron-bearing water magnesium of acquisition
Stone sample has the characteristics that purity height, better crystallinity degree, chemical stability are good, and this method provides weight for the research of nemalite
Ensure solve the technical barrier that current nemalite can not be artificial synthesized.
Specific implementation mode
It is further below in conjunction with specific embodiment to make present disclosure, technical solution and advantage be more clearly understood
Illustrate the present invention, these embodiments are merely to illustrate the present invention, and the present invention is not limited only to following embodiment.
Embodiment 1：
A method of it synthesizing nemalite at high temperature under high pressure, includes the following steps：
Step 1 uses analytically pure magnesium hydroxide Mg (OH)2, analytically pure iron powder Fe and analytically pure iron hydroxide Fe
(OH)3With molar ratio 27：1：2 ground and mixeds are uniformly used as starting material；
Mix powder in step 1 is pressed into Φ 5 × 2mm cylindrical samples by step 2 using tablet press machine, separately takes analysis
Pure iron powder is pressed into the iron plate of two pieces of 5 × 1mm of Φ, then by cylindrical sample and iron plate with iron plate-cylindrical sample-iron plate
Sandwich structure is put into Φ 5mm, thickness 0.1mm platinum snap fasteners and seals, and platinum snap fastener is finally packed into Φ 5.5mm, thickness
It is sealed in the pellet in a shotgun cartridge female thread of 0.2mm, pellet in a shotgun cartridge female thread is placed in h-BN pipes, using h-BN as transmission medium；
The h-BN pipes that sample is housed in step 2 are assembled in high-pressure synthesis assembling block and to be placed on cubic apparatus big by step 3
Press carries out high-temperature high-voltage reaction, and the temperature of high-temperature high-voltage reaction is 600 DEG C, pressure 3GPa, reaction time 8h；
Step 4 takes out the pellet in a shotgun cartridge female thread in step 3, is sawed with diamond low speed and opens pellet in a shotgun cartridge female thread, takes out cylindrical sample
Product obtain nemalite sample.
The production method concrete operations of h-BN pipes described in step 2 are：In the h-BN sticks for being Φ 10mm by size on lathe
The hole that the heart bores Φ 6mm is made h-BN pipes, and sample is filled in pipe, and both ends take the h-BN pieces that Φ 6mm thickness is 2mm to seal.
The high-pressure synthesis that is assembled in h-BN pipes described in step 3 assembles method concrete operations in the block and includes：
Step 3.1 chooses one piece of pyrophyllite block, and a Φ 12mm circular through hole is made at pyrophyllite block center；
Step 3.2, in the circular graphitic heating furnace of one outer diameter Φ 12mm of circular through hole inner sleeve, internal diameter Φ 10mm；
Step 3.3, placed among graphite heater furnace Φ 10mm the h-BN seals of tube sample；
Step 3.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug；
The advantages of high pressure of the present invention assembling block is：1. using thermocouple temperature control, the temperature that heating system is fed back by thermocouple
Degree adjusts heating power, and to change temperature, the immediately monitoring to temperature may be implemented in this method, is suitable for measuring essence to temperature
Degree requires high 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 two 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.
The nemalite sample obtained described in step 4 is single object phase, and free from admixture phase, nemalite is six sides knot
Structure, space group P-3m1, lattice parameter
Embodiment 2：
A method of it synthesizing nemalite at high temperature under high pressure, includes the following steps：
Step 1 uses analytically pure magnesium hydroxide Mg (OH)2, analytically pure iron powder Fe and analytically pure iron hydroxide Fe
(OH)3With molar ratio 27：1：2 ground and mixeds are uniformly used as starting material；
Mix powder in step 1 is pressed into Φ 5 × 2mm cylindrical samples by step 2 using tablet press machine, separately takes analysis
Pure iron powder is pressed into the iron plate of two pieces of 5 × 1mm of Φ, then by cylindrical sample and iron plate with iron plate-cylindrical sample-iron plate
Sandwich structure is put into Φ 5mm, thickness 0.1mm platinum snap fasteners and seals, and platinum snap fastener is finally packed into Φ 5.5mm, thickness
It is sealed in the pellet in a shotgun cartridge female thread of 0.2mm, pellet in a shotgun cartridge female thread is placed in h-BN pipes, using h-BN as transmission medium；
The h-BN pipes that sample is housed in step 2 are assembled in high-pressure synthesis assembling block and to be placed on cubic apparatus big by step 3
Press carries out high-temperature high-voltage reaction, and the temperature of high-temperature high-voltage reaction is 700 DEG C, pressure 3GPa, reaction time 8h；
Step 4 takes out the pellet in a shotgun cartridge female thread in step 3, is sawed with diamond low speed and opens pellet in a shotgun cartridge female thread, takes out cylindrical sample
Product obtain nemalite sample.
The production method concrete operations of h-BN pipes described in step 2 are：In the h-BN sticks for being Φ 10mm by size on lathe
The hole that the heart bores Φ 6mm is made h-BN pipes, and sample is filled in pipe, and both ends take the h-BN pieces that Φ 6mm thickness is 2mm to seal.
The high-pressure synthesis that is assembled in h-BN pipes described in step 3 assembles method concrete operations in the block and includes：
Step 3.1 chooses one piece of pyrophyllite block, and a Φ 12mm circular through hole is made at pyrophyllite block center；
Step 3.2, in the circular graphitic heating furnace of one outer diameter Φ 12mm of circular through hole inner sleeve, internal diameter Φ 10mm；
Step 3.3, placed among graphite heater furnace Φ 10mm the h-BN seals of tube sample；
Step 3.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug；
The advantages of high pressure of the present invention assembling block is：1. using thermocouple temperature control, the temperature that heating system is fed back by thermocouple
Degree adjusts heating power, and to change temperature, the immediately monitoring to temperature may be implemented in this method, is suitable for measuring essence to temperature
Degree requires high 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 two 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.
The nemalite sample obtained described in step 4 is single object phase, and free from admixture phase, nemalite is six sides knot
Structure, space group P-3m1, lattice parameter
Claims (5)
1. a kind of method synthesizing nemalite at high temperature under high pressure, which is characterized in that include the following steps：
Step 1 uses analytically pure magnesium hydroxide Mg (OH)2, analytically pure iron powder Fe and analytically pure iron hydroxide Fe (OH)3
With molar ratio 27：1：2 ground and mixeds are uniformly used as starting material；
Mix powder in step 1 is pressed into Φ 5 × 2mm cylindrical samples by step 2 using tablet press machine, is separately taken analytically pure
Iron powder is pressed into the iron plate of two pieces of 5 × 1mm of Φ, then by cylindrical sample and iron plate with Sanming City of iron plate-cylindrical sample-iron plate
It controls structure and is put into Φ 5mm, thickness 0.1mm platinum snap fasteners and seal, platinum snap fastener is finally packed into Φ 5.5mm, thickness 0.2mm
It is sealed in pellet in a shotgun cartridge female thread, pellet in a shotgun cartridge female thread is placed in h-BN pipes, using h-BN as transmission medium；
The h-BN pipes that sample is housed in step 2 are assembled in high-pressure synthesis assembling block and are placed on the big press of cubic apparatus by step 3
Carry out high-temperature high-voltage reaction；
Step 4 takes out the pellet in a shotgun cartridge female thread in step 3, cuts pellet in a shotgun cartridge female thread with diamond saw, takes out cylindrical sample and contained
Esisenbrucite sample.
2. a kind of method synthesizing nemalite at high temperature under high pressure described in accordance with the claim 1, which is characterized in that step
The production method concrete operations of the 2 h-BN pipes are：By the hole for the h-BN stick centre drill Φ 6mm that size is Φ 10mm on lathe
H-BN pipes are made, sample is filled in pipe, both ends take the h-BN pieces that Φ 6mm thickness is 2mm to seal.
3. a kind of method synthesizing nemalite at high temperature under high pressure described in accordance with the claim 1, which is characterized in that step
The high-pressure synthesis that is assembled in h-BN pipes described in 3 assembles method concrete operations in the block and includes：
Step 3.1 chooses one piece of pyrophyllite block, and a Φ 12mm circular through hole is made at pyrophyllite block center；
Step 3.2, in the circular graphitic heating furnace of one outer diameter Φ 12mm of circular through hole inner sleeve, internal diameter Φ 10mm；
Step 3.3, placed among graphite heater furnace Φ 10mm the h-BN seals of tube sample；
Step 3.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug.
4. a kind of method synthesizing nemalite at high temperature under high pressure described in accordance with the claim 1, which is characterized in that step
The temperature of 3 high-temperature high-voltage reactions is 600-700 DEG C, pressure 3GPa, reaction time 8h.
5. a kind of method synthesizing nemalite at high temperature under high pressure described in accordance with the claim 1, which is characterized in that step
The nemalite sample obtained described in 4 is single object phase, and free from admixture phase, nemalite is hexagonal structure, space group P-
3m1, lattice parameter
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111646513A (en) * | 2020-07-24 | 2020-09-11 | 中国科学院地球化学研究所 | Method for directly synthesizing manganese-doped zinc sulfide block through solid-phase reaction |
| CN111675540A (en) * | 2020-07-24 | 2020-09-18 | 中国科学院地球化学研究所 | Method for directly synthesizing high-purity bornite through solid-phase reaction |
| CN111825122A (en) * | 2020-07-24 | 2020-10-27 | 中国科学院地球化学研究所 | Method for directly synthesizing high-density magnesium sulfide iron block through solid-phase reaction |
| CN111829850A (en) * | 2020-07-24 | 2020-10-27 | 中国科学院地球化学研究所 | Method for directly synthesizing high-purity sulfur-arsenic-copper ore by solid-phase reaction |
| CN112851351A (en) * | 2020-08-29 | 2021-05-28 | 中国科学院地球化学研究所 | Method for directly synthesizing iron-doped zinc sulfide block through solid-phase reaction |
| CN113247957A (en) * | 2021-06-22 | 2021-08-13 | 贵州师范学院 | Method for synthesizing barium manganese carbonate-trigonosterite solid solution at high temperature and high pressure |
| CN113897665A (en) * | 2021-11-09 | 2022-01-07 | 中国科学院地球化学研究所 | Preparation method of high-titanium and high-water-content forsterite single crystal |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111646513A (en) * | 2020-07-24 | 2020-09-11 | 中国科学院地球化学研究所 | Method for directly synthesizing manganese-doped zinc sulfide block through solid-phase reaction |
| CN111675540A (en) * | 2020-07-24 | 2020-09-18 | 中国科学院地球化学研究所 | Method for directly synthesizing high-purity bornite through solid-phase reaction |
| CN111825122A (en) * | 2020-07-24 | 2020-10-27 | 中国科学院地球化学研究所 | Method for directly synthesizing high-density magnesium sulfide iron block through solid-phase reaction |
| CN111829850A (en) * | 2020-07-24 | 2020-10-27 | 中国科学院地球化学研究所 | Method for directly synthesizing high-purity sulfur-arsenic-copper ore by solid-phase reaction |
| CN111829850B (en) * | 2020-07-24 | 2021-04-23 | 中国科学院地球化学研究所 | Method for directly synthesizing high-purity sulfur-arsenic-copper ore by solid-phase reaction |
| CN111675540B (en) * | 2020-07-24 | 2021-05-14 | 中国科学院地球化学研究所 | Method for directly synthesizing high-purity bornite through solid-phase reaction |
| CN112851351A (en) * | 2020-08-29 | 2021-05-28 | 中国科学院地球化学研究所 | Method for directly synthesizing iron-doped zinc sulfide block through solid-phase reaction |
| CN113247957A (en) * | 2021-06-22 | 2021-08-13 | 贵州师范学院 | Method for synthesizing barium manganese carbonate-trigonosterite solid solution at high temperature and high pressure |
| CN113247957B (en) * | 2021-06-22 | 2022-08-02 | 贵州师范学院 | Method for synthesizing barium manganese carbonate-trigonosterite solid solution at high temperature and high pressure |
| CN113897665A (en) * | 2021-11-09 | 2022-01-07 | 中国科学院地球化学研究所 | Preparation method of high-titanium and high-water-content forsterite single crystal |
| CN113897665B (en) * | 2021-11-09 | 2022-07-26 | 中国科学院地球化学研究所 | Preparation method of high-titanium and high-water-content forsterite single crystal |
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