CN107778008A - A kind of method for preparing the iron FeP of a phosphatization one at high temperature under high pressure - Google Patents
A kind of method for preparing the iron FeP of a phosphatization one at high temperature under high pressure Download PDFInfo
- Publication number
- CN107778008A CN107778008A CN201711066561.1A CN201711066561A CN107778008A CN 107778008 A CN107778008 A CN 107778008A CN 201711066561 A CN201711066561 A CN 201711066561A CN 107778008 A CN107778008 A CN 107778008A
- Authority
- CN
- China
- Prior art keywords
- iron
- phosphatization
- boron nitride
- sample
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/5154—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on phosphides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/405—Iron group metals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Products (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of method for preparing the iron of a phosphatization one at high temperature under high pressure, it includes：Initiation material is used as using analytically pure iron nano powder and red phosphorus powder；By it according to mol ratio 1：1 is fully ground mixing in agate mortar using alcohol；The mixed-powder after grinding is pressed into cylindrical sample using tablet press machine；Boron nitride ceramics rod is processed into pipe, is placed in oven for drying；Cylindrical sample is put into boron nitride pipe, the big press of cubic apparatus will be integrally placed at after its upper-lower seal using boron nitride ceramics piece carries out high-temperature high-voltage reaction；Reacted sample is taken out, removes the boron nitride of sample exterior, you can obtains the pure iron bulk sample of a phosphatization one；Solve in the prior art, response variable is whard to control, etch quartz pipe, the reaction time is long, product purity is low, crystallinity is low, and product is that powder can not the technical problem such as post-production.
Description
Technical field
The invention belongs to functional material to synthesize field, more particularly to one kind prepares the iron FeP of a phosphatization one at high temperature under high pressure
Method.
Background technology
Industrially, the iron FeP of a phosphatization one is also known as iron phosphide, ferrophosphorus, is the accessory substance of phosphorous chemical industry, is widely used in smelting
Gold, smelt, chemical industry.Ultra-fine ferrophosphorus powder has the characteristic such as conduction, heavy antisepsis, the absorption of anti-marine organisms, environmental protection, be paint,
The new science and technology product of coating industry, particularly on zinc powder is substituted, there are environmental protection, protection welding worker health, price low, resistance to heavy
The advantage of corrosion.Epoxy zinc rich primer, electrically-conducting paint, filler etc. are widely used in, any paint is adapted to and does antirust, anti-corrosive
Pigment.It is the important original for researching and developing new type lithium ion battery meanwhile the iron of a phosphatization one can also be used as lithium ion battery negative material
Material and research object；The iron of one phosphatization one is also a kind of additive for having and improving evolving hydrogen reaction efficiency, is high-performance evolving hydrogen reaction
The object that Material Field is being furtherd investigate.
The ferrophosphorus powder for the technical grade that currently there are is mainly by the iron FeP of a phosphatization one, the iron Fe of a phosphatization two2P, a silicon
Change the mixture composition of an iron FeSi.Compare, the pure iron product of a phosphatization one can only be used for by the artificial synthesized acquisition in laboratory
Study the critical natures such as resistivity, the magnetic susceptibility of its single-phase.At present it has been reported that laboratory synthesis the iron of one phosphatization one side
Method is mainly based on quartz ampoule vacuum method：With iron and red phosphorus according to mol ratio 1：1 is enclosed in the quartz ampoule after vacuumizing, and heating is burnt
Burn to 1000 DEG C, obtain the iron of one phosphatization of final product one.Although quartz ampoule vacuum method can obtain the iron of a phosphatization one, but still deposit
In following shortcoming：Because red phosphorus is being heated to 400 DEG C or so the volatilizations that will distil under normal pressure, the red phosphorus amount that name matches is caused to be damaged
Lose so that the phosphorus content entirely reacted is difficult to control, and causes the iron sample composition of a phosphatization one of acquisition impure；In hot conditions
Under, the phosphorus steam of volatilization can react with quartz ampoule, corrode the quartz ampoule of sealing, may cause in very long sintering process
The failure of an experiment, and the product that this method obtains is powdered, can not carry out post-production to meet the detection of some performances, such as lead
Electrical property etc., and obtained product crystallinity is very poor, can not meet requirement of the spectrum tests such as Raman scattering to sample crystallinity.
Therefore, it is insufficient present in current synthetic method to improve must to explore the new iron synthetic method of a phosphatization one for we.
The content of the invention
The technical problem to be solved in the present invention is：A kind of method for preparing the iron FeP of a phosphatization one at high temperature under high pressure, with solution
Certainly prior art operation process complexity, Acceleration study ageing equipment, reaction time length, the iron product purity of a phosphatization one obtained
It is low, cleanliness factor is low, is powdered, the technical problem such as post-production difficulty.
The technical scheme is that：A kind of method for preparing the iron FeP of a phosphatization one at high temperature under high pressure, it includes：
Step 1：Initiation material is used as using analytically pure reduced iron powder and red phosphorus powder；
Step 2：By iron nano powder and red phosphorus massage that ratio 1：1 ratio mixes, and is placed in mortar, adds alcohol, so
Grinding is until liquid all volatilizees afterwards；
Step 3：The mixed-powder after grinding is placed into tabletting in circular die using tablet press machine, obtains cylindrical sample
Product；
Step 4：Boron nitride BN ceramic rods are processed into pipe, is placed in baking oven and dries；
Step 5：The sample of pre-molding in step 3 is put into the boron nitride pipe in step 4, uses boron nitride ceramics
Piece is by its upper-lower seal；
Step 6：Cylindrical samples obtained by step 5 are assembled in high-pressure synthesis assembling block and are placed on the big pressure of cubic apparatus
Machine carries out high-temperature high-voltage reaction；
Step 7：Reacted sample is taken out, removes the boron nitride cover of sample exterior, you can obtains a pure phosphatization
One iron bulk sample.
Specific preparation method described in step 5 is：Boron nitride ceramics rod is utilized into lathe process into length 10mm, external diameter
10mm, internal diameter 6mm pipe, as the sleeve pipe of parcel sample, then the cylindrical sample obtained by step 3 is put into wherein, made
With boron nitride ceramics piece by its upper-lower seal.
The method in high-pressure synthesis assembling block described in step 6 includes：
Step 6.1, one piece of pyrophyllite block is chosen, a manhole is made at pyrophyllite block center；
Step 6.2, in one cylindrical graphite heater furnace of manhole inner sleeve；
Step 6.3, the sample that placement is wrapped up with boron nitride tube among graphite heater furnace；
Step 6.4, by circular graphitic heating furnace upper and lower ends with pyrophillite plug seal.
Thermocouple is provided with described high-pressure synthesis assembling block.
The temperature of high-temperature high-voltage reaction described in step 6 is 800 DEG C~1200 DEG C, pressure 1-3GPa, reaction time 1-5
Individual hour.
The pure iron of a phosphatization one described in step 7 is single thing phase, free from admixture phase, is hexagonal structure, space group Pnma
(no.62), lattice parameterIt is a kind of typical case with good metallic luster
Alloy material.
The beneficial effects of the invention are as follows：
Using analysis pure iron nano powder and red phosphorus powder as initiation material, at high temperature under high pressure, using solid reaction process
The iron sample of a phosphatization one is obtained, its principle is：
Fe+P-FeP
1st, the iron of a phosphatization one prepared by the present invention is the very high single-phase sample of purity, due to high temperature and pressure experiment sample quilt
Highdensity boron nitride ceramics is wrapped up, and is to be carried out in closed cavity, avoiding problems the volatilization loss of red phosphorus so that
Reaction can be reacted in strict accordance with name proportioning, obtain the pure iron of a phosphatization one.Meanwhile high-temperature and high-pressure conditions accelerate point
The solid phase reaction speed of son diffusion so that reaction can be completed within a hour, greatly increase combined coefficient.Solve often
The volatile quantity for being pressed into red phosphorus in method is difficult control so that the name proportioning loss of red phosphorus in solid phase reaction, causes one obtained
The problem of iron sample purity of phosphatization one is relatively low.
2nd, the iron of a phosphatization one prepared by the present invention is high-density sintered bulk sample, and fine and close bulk sample, which can be processed, to be beaten
The geometry needed for resistivity measurement is worn into, is provided safeguard for the research of resistivity.Compare, the one of atmospheric synthesis method sintering
The shaping of the iron of phosphatization one is poor, has substantial amounts of space in sample, causes the difficulty of resistivity measurement.
3rd, the iron of a phosphatization one prepared by the present invention is the good sample of crystallinity.Because high pressure can improve the decomposition of material
Temperature so that the reaction temperature of the HTHP synthesis iron of one phosphatization one wants high more compared to normal pressure-sintered, therefore, higher reaction
Temperature not only completes HTHP solid phase reaction, while also completes the recrystallization reaction of sample so that the iron sample of a phosphatization one
The crystallization degree of product is significantly increased.The iron sample of a phosphatization one of big crystal grain provides guarantor for spectrum tests such as Raman scatterings
Barrier.Compare, because reaction temperature is very low, the iron crystallinity of a phosphatization one of atmospheric synthesis method sintering is very poor, can not meet Raman
The requirements of the spectrum test to sample crystallinity such as scattering.
To sum up, instant invention overcomes the phosphorus content that quartz ampoule vacuum method entirely reacts is difficult to control, phosphorus steam can corrode stone
The problem of Ying Guan, reaction time length, reactor product are powdered, are not easy post-production, and product impurity is more, crystallinity is low.This
The preparation method of invention has that operating process is simple, fast period time is short, cost is low, is not easy to damage the advantages such as experimental facilities, obtains
The iron of a phosphatization one obtained has the characteristics that purity height, bulk can be processed, and this method is the research of the single thing phase of the iron of a phosphatization one
Important leverage is provided, in addition, the consumptive material that the present invention is required, if graphite, boron nitride ceramics are than quartz ampoule price in the prior art
It is low, save cost.
Brief description of the drawings
Fig. 1 is the XRD of the iron of a phosphatization one prepared by the embodiment of the present invention 3；
Fig. 2 is the BSE figures of the iron of a phosphatization one prepared by the embodiment of the present invention 3；
Fig. 3 is the Raman figure of the iron of a phosphatization one prepared by the embodiment of the present invention 3.
Embodiment
Below in conjunction with the accompanying drawings and invention is described further specific embodiment：
Case study on implementation 1
Using analytically pure iron nano powder (Fe) and red phosphorus powder (P) as initiation material, by it according to mol ratio 1：1 in agate
Be fully ground mixing using alcohol in Nao mortars, take iron phosphorus mixed-powder about 0.30g using powder compressing machine will be pressed into φ 6mm ×
6mm cylinders, boron nitride pottery rod is processed into length 10mm, external diameter 10mm, internal diameter 6mm boron nitride ceramics pipe, is placed in baking oven
In dried 2 hours at a temperature of 150 DEG C, then powder cylinders sample is placed in boron nitride ceramics pipe, uses 2mm boron nitride up and down
Potsherd seals, and completes high pressure assembling block.High pressure assembles block assembling mode：
1. 32mm × 32mm × 32mm one a diameter of 12mm of pyrophillite cubic block centre drill manhole；
2. one external diameter of set is 12mm inside the manhole of pyrophyllite block, internal diameter is 10mm graphite bush heating furnace；
It is with a diameter of up and down 3. putting the boron nitride cylinder of interior iron content phosphorus mixed-powder among graphite bush heating furnace
10mm pyrophillite plug is blocked.
So far, high pressure assembling block is completed, and the size that its mesohigh assembling block is related to can be according to boron nitride cylindrical samples
Size come specifically determine；In the assembling block, pyrophillite and boron nitride make transmission medium, and graphite bush makees heating furnace, thermocouple
Make temperature regulating device.The advantages of high pressure of the present invention assembling block is：1. using thermocouple temperature control, heating system is fed back by thermocouple
Temperature adjustment heating power, so as to change temperature, this method can realize the immediately monitoring to temperature, suitable for temperature survey
The high experiment of required precision；2. pyrophillite has good pressure transmission, machining property, heat-resisting guarantor as one-level transmission medium
Warm nature and insulating properties, boron nitride are a kind of strong ceramic materials of processability, as two level transmission medium, make the pressure in cavity equal
It is even, good airproof performance, and boron nitride is sufficiently stable, will not pollute destruction product quality, is that the phosphatization one of completion one is iron standby most suitable
Encapsulant；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, design temperature is 800 DEG C, and pressure is
1GPa, reaction time 5h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, removes the boron nitride of sample surfaces, i.e.,
It can obtain the pure iron sample of a phosphatization one.The result of X-ray diffraction electron probing analysis shows, passes through preparation method system of the present invention
It is standby go out the iron of a phosphatization one be single thing phase, free from admixture phase.
Case study on implementation 2
Using analytically pure iron nano powder (Fe) and red phosphorus powder (P) as initiation material, by it according to mol ratio 1：1 in agate
Be fully ground mixing using alcohol in Nao mortars, take iron phosphorus mixed-powder about 0.30g using powder compressing machine will be pressed into φ 6mm ×
6mm cylinders, boron nitride pottery rod is processed into length 10mm, external diameter 10mm, internal diameter 6mm boron nitride ceramics pipe, is placed in baking oven
In dried 2 hours at a temperature of 150 DEG C, then powder cylinders sample is placed in boron nitride ceramics pipe, uses 2mm boron nitride up and down
Potsherd seals, and completes high pressure assembling block.High pressure assembles block assembling mode：
1. 32mm × 32mm × 32mm one a diameter of 12mm of pyrophillite cubic block centre drill manhole；
2. one external diameter of set is 12mm inside the manhole of pyrophyllite block, internal diameter is 10mm graphite bush heating furnace；
It is with a diameter of up and down 3. putting the boron nitride cylinder of interior iron content phosphorus mixed-powder among graphite bush heating furnace
10mm pyrophillite plug is blocked.
So far, high pressure assembling block is completed, and the size that its mesohigh assembling block is related to can be according to boron nitride cylindrical samples
Size come specifically determine；In the assembling block, pyrophillite and boron nitride make transmission medium, and graphite bush makees heating furnace, thermocouple
Make temperature regulating device.The advantages of high pressure of the present invention assembling block is：1. using thermocouple temperature control, heating system is fed back by thermocouple
Temperature adjustment heating power, so as to change temperature, this method can realize the immediately monitoring to temperature, suitable for temperature survey
The high experiment of required precision；2. pyrophillite has good pressure transmission, machining property, heat-resisting guarantor as one-level transmission medium
Warm nature and insulating properties, boron nitride are a kind of strong ceramic materials of processability, as two level transmission medium, make the pressure in cavity equal
It is even, good airproof performance, and boron nitride is sufficiently stable, will not pollute destruction product quality, is that the phosphatization one of completion one is iron standby most suitable
Encapsulant；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, design temperature is 1200 DEG C, and pressure is
3GPa, reaction time 1h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, removes the boron nitride of sample surfaces, i.e.,
It can obtain the pure iron sample of a phosphatization one.The result of X-ray diffraction electron probing analysis shows, passes through preparation method system of the present invention
It is standby go out the iron of a phosphatization one be single thing phase, free from admixture phase.
Case study on implementation 3
Using analytically pure iron nano powder (Fe) and red phosphorus powder (P) as initiation material, by it according to mol ratio 1：1 in agate
Be fully ground mixing using alcohol in Nao mortars, take iron phosphorus mixed-powder about 0.30g using powder compressing machine will be pressed into φ 6mm ×
6mm cylinders, boron nitride pottery rod is processed into length 10mm, external diameter 10mm, internal diameter 6mm boron nitride ceramics pipe, is placed in baking oven
In dried 2 hours at a temperature of 150 DEG C, then powder cylinders sample is placed in boron nitride ceramics pipe, uses 2mm boron nitride up and down
Potsherd seals, and completes high pressure assembling block.High pressure assembles block assembling mode：
1. 32mm × 32mm × 32mm one a diameter of 12mm of pyrophillite cubic block centre drill manhole；
2. one external diameter of set is 12mm inside the manhole of pyrophyllite block, internal diameter is 10mm graphite bush heating furnace；
It is with a diameter of up and down 3. putting the boron nitride cylinder of interior iron content phosphorus mixed-powder among graphite bush heating furnace
10mm pyrophillite plug is blocked.
So far, high pressure assembling block is completed, and the size that its mesohigh assembling block is related to can be according to boron nitride cylindrical samples
Size come specifically determine；In the assembling block, pyrophillite and boron nitride make transmission medium, and graphite bush makees heating furnace, thermocouple
Make temperature regulating device.The advantages of high pressure of the present invention assembling block is：1. using thermocouple temperature control, heating system is fed back by thermocouple
Temperature adjustment heating power, so as to change temperature, this method can realize the immediately monitoring to temperature, suitable for temperature survey
The high experiment of required precision；2. pyrophillite has good pressure transmission, machining property, heat-resisting guarantor as one-level transmission medium
Warm nature and insulating properties, boron nitride are a kind of strong ceramic materials of processability, as two level transmission medium, make the pressure in cavity equal
It is even, good airproof performance, and boron nitride is sufficiently stable, will not pollute destruction product quality, is that the phosphatization one of completion one is iron standby most suitable
Encapsulant；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, design temperature is 1100 DEG C, and pressure is
2GPa, reaction time 4h.After the completion of high-temperature high-voltage reaction, obtained sample is taken out, removes the boron nitride of sample surfaces, i.e.,
It can obtain the pure iron sample of a phosphatization one.The result of X-ray diffraction electron probing analysis shows, passes through preparation method system of the present invention
It is standby go out the iron of a phosphatization one be single thing phase, free from admixture phase.BSE images show the phosphatization one that preparation method of the present invention is prepared
Iron is crystal structure, and crystallite dimension is big, and completes the test of Raman collection of illustrative plates.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (6)
1. a kind of method for preparing the iron FeP of a phosphatization one at high temperature under high pressure, it includes：
Step 1：Initiation material is used as using analytically pure reduced iron powder and red phosphorus powder；
Step 2：By iron nano powder and red phosphorus massage that ratio 1：1 ratio mixes, and is placed in mortar, adds alcohol, Ran Houyan
Mill is until liquid all volatilizees；
Step 3：The mixed-powder after grinding is placed into tabletting in circular die using tablet press machine, obtains cylindrical sample；
Step 4：Boron nitride BN ceramic rods are processed into pipe, is placed in baking oven and dries；
Step 5：The sample of pre-molding in step 3 is put into the boron nitride pipe in step 4, will using boron nitride ceramics piece
Its upper-lower seal；
Step 6：Cylindrical samples obtained by step 5 are assembled in high-pressure synthesis assembling block and are placed on the big press of cubic apparatus
Row high-temperature high-voltage reaction；
Step 7：Reacted sample is taken out, removes the boron nitride cover of sample exterior, you can obtains the pure iron of a phosphatization one
Bulk sample.
A kind of 2. method for preparing the iron FeP of a phosphatization one at high temperature under high pressure according to claim 1, it is characterised in that：
Specific preparation method described in step 5 is：Boron nitride ceramics rod is utilized into lathe process into length 10mm, external diameter 10mm, internal diameter
6mm pipe, as the sleeve pipe of parcel sample, then the cylindrical sample obtained by step 3 is put into wherein, made pottery using boron nitride
Ceramics is by its upper-lower seal.
A kind of 3. method for preparing the iron FeP of a phosphatization one at high temperature under high pressure according to claim 1, it is characterised in that：
The method in high-pressure synthesis assembling block described in step 6 includes：
Step 6.1, one piece of pyrophyllite block is chosen, a manhole is made at pyrophyllite block center；
Step 6.2, in one cylindrical graphite heater furnace of manhole inner sleeve；
Step 6.3, the sample that placement is wrapped up with boron nitride tube among graphite heater furnace；
Step 6.4, by circular graphitic heating furnace upper and lower ends with pyrophillite plug seal.
A kind of 4. method for preparing the iron FeP of a phosphatization one at high temperature under high pressure according to claim 1, it is characterised in that：
Thermocouple is provided with described high-pressure synthesis assembling block.
A kind of 5. method for preparing the iron FeP of a phosphatization one at high temperature under high pressure according to claim 1, it is characterised in that：
The temperature of high-temperature high-voltage reaction described in step 6 is 800 DEG C~1200 DEG C, pressure 1-3GPa, and the reaction time is 1-5 hour.
A kind of 6. method for preparing the iron FeP of a phosphatization one at high temperature under high pressure according to claim 1, it is characterised in that：
The pure iron of a phosphatization one described in step 7 is single thing phase, free from admixture phase, is hexagonal structure, and space group is Pnma (no.62), brilliant
Lattice parameterIt is a kind of typical alloy material with good metallic luster.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711066561.1A CN107778008B (en) | 2017-11-02 | 2017-11-02 | Method for preparing iron phosphide FeP at high temperature and high pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711066561.1A CN107778008B (en) | 2017-11-02 | 2017-11-02 | Method for preparing iron phosphide FeP at high temperature and high pressure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107778008A true CN107778008A (en) | 2018-03-09 |
| CN107778008B CN107778008B (en) | 2020-03-24 |
Family
ID=61432340
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711066561.1A Active CN107778008B (en) | 2017-11-02 | 2017-11-02 | Method for preparing iron phosphide FeP at high temperature and high pressure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107778008B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110002419A (en) * | 2019-04-18 | 2019-07-12 | 王东升 | A kind of preparation method of high-tap density ferric phosphate |
| CN112250082A (en) * | 2020-10-26 | 2021-01-22 | 燕山大学 | Transition metal compound and preparation method thereof |
| CN112403395A (en) * | 2020-11-27 | 2021-02-26 | 南方科技大学 | Preparation method of metal phosphide |
| CN114843478A (en) * | 2022-05-23 | 2022-08-02 | 广东技术师范大学 | Nano FeP for lithium ion battery 2 Preparation method of/C/CNTs composite material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659403A (en) * | 2009-09-18 | 2010-03-03 | 中国海洋大学 | Hydro-thermal synthesis process of phosphide |
| CN106115791A (en) * | 2016-06-24 | 2016-11-16 | 中国科学院地球化学研究所 | A kind of method of the side of preparation at high temperature under high pressure magnesioferrite |
| CN108352230A (en) * | 2015-10-30 | 2018-07-31 | 巴斯夫欧洲公司 | Include the magneto-caloric material of manganese, iron, silicon, phosphorus and nitrogen |
-
2017
- 2017-11-02 CN CN201711066561.1A patent/CN107778008B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659403A (en) * | 2009-09-18 | 2010-03-03 | 中国海洋大学 | Hydro-thermal synthesis process of phosphide |
| CN108352230A (en) * | 2015-10-30 | 2018-07-31 | 巴斯夫欧洲公司 | Include the magneto-caloric material of manganese, iron, silicon, phosphorus and nitrogen |
| CN106115791A (en) * | 2016-06-24 | 2016-11-16 | 中国科学院地球化学研究所 | A kind of method of the side of preparation at high temperature under high pressure magnesioferrite |
Non-Patent Citations (1)
| Title |
|---|
| TINGTING GU1 ET AL: "Probing nonequivalent sites in iron phosphide Fe2P and its mechanism of phase transition", 《EUR. PHYS. J. B》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110002419A (en) * | 2019-04-18 | 2019-07-12 | 王东升 | A kind of preparation method of high-tap density ferric phosphate |
| CN110002419B (en) * | 2019-04-18 | 2021-07-02 | 王东升 | Preparation method of high-tap-density iron phosphate |
| CN112250082A (en) * | 2020-10-26 | 2021-01-22 | 燕山大学 | Transition metal compound and preparation method thereof |
| CN112403395A (en) * | 2020-11-27 | 2021-02-26 | 南方科技大学 | Preparation method of metal phosphide |
| CN114843478A (en) * | 2022-05-23 | 2022-08-02 | 广东技术师范大学 | Nano FeP for lithium ion battery 2 Preparation method of/C/CNTs composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107778008B (en) | 2020-03-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107778008A (en) | A kind of method for preparing the iron FeP of a phosphatization one at high temperature under high pressure | |
| Zhang et al. | Field assisted sintering of dense Al-substituted cubic phase Li7La3Zr2O12 solid electrolytes | |
| CN102931335B (en) | A kind of Graphene is combined thermoelectric material of cobalt stibide based skutterudite and preparation method thereof | |
| CN107814572A (en) | A kind of method for preparing a phosphatization three-iron Fe3P at high temperature under high pressure | |
| Noudem et al. | Granular and lamellar thermoelectric oxides consolidated by spark plasma sintering | |
| CN107651959A (en) | One kind prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method | |
| Zybala et al. | Anisotropy analysis of thermoelectric properties of Bi2Te2. 9Se0. 1 prepared by SPS method | |
| CN102942366B (en) | Preparation method of Al-Mg-B ceramic material | |
| CN109399580B (en) | Rapid preparation of CuFeSe2Method (2) | |
| Liu et al. | Synthesis of Li7La3Zr2O12 solid electrolyte by solid phase sintering method | |
| CN107123729A (en) | A kind of nanometer silicon carbide/P-type silicon germanium alloy base thermoelectrical composite material and preparation method thereof | |
| CN101358313B (en) | Method for improving Bi-S binary system thermoelectric material performance | |
| CN101338386B (en) | Method for preparing TiNi Sn based thermoelectric compounds | |
| CN101407340A (en) | Iron arsenic compound high temperature superconductor crystal and preparation thereof | |
| CN105568023A (en) | Preparation method for Al6Mn quasicrystal | |
| CN111446357A (en) | Preparation of Cu2Method for Se thermoelectric material | |
| CN112582527B (en) | Preparation method of graphite-doped GeS2 thermoelectric material | |
| CN109455678B (en) | FeTe is prepared fast to ordinary pressure2Method (2) | |
| CN109604605B (en) | Rapid preparation of CoSb by solid-phase reaction method3Method (2) | |
| JP2001335367A (en) | Lanthanum sulfide or cerium sulfide sintered compact and manufacturing method therefor | |
| CN109686989B (en) | Preparation method of solid fuel cell cathode material | |
| Bao et al. | Synthesis, thermionic emission and magnetic properties of (NdxGd1–x) B6 | |
| CN110357620A (en) | A kind of preparation method of high intensity indium doping calcium zirconate ceramics | |
| CN113699587B (en) | Preparation method of P-type polycrystalline zirconium pentatelluride block thermoelectric material | |
| CN109628784B (en) | Method for preparing FeSb2 by high-temperature solid-phase reaction method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |