CN107651959A - One kind prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method - Google Patents
One kind prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method Download PDFInfo
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- CN107651959A CN107651959A CN201711066574.9A CN201711066574A CN107651959A CN 107651959 A CN107651959 A CN 107651959A CN 201711066574 A CN201711066574 A CN 201711066574A CN 107651959 A CN107651959 A CN 107651959A
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Abstract
The invention discloses a kind of method for preparing the iron of a phosphatization two 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 2：1 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 two；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, product is that powder or little particle can not the technical problems such as post-production.
Description
Technical field
The invention belongs to functional material to synthesize field, more particularly to one kind prepares the iron Fe of a phosphatization two at high temperature under high pressure2P
Method.
Background technology
Industrially, the iron Fe of a phosphatization two2P is also known as Iron hemiphosphide, is the accessory substance of phosphorous chemical industry, be widely used in it is metallurgical,
Smelt, chemical industry.Ultra-fine ferrophosphorus powder has the characteristics such as conduction, heavy antisepsis, the absorption of anti-marine organisms, environmental protection, is paint, coating
The new science and technology product of industry, particularly on zinc powder is substituted, there is environmental protection, protection welding worker is healthy, price is low, resistance to heavy corrosion
Advantage.Epoxy zinc rich primer, electrically-conducting paint, filler etc. are widely used in, any paint is adapted to and does antirust, anti-corrosive pigment.
Meanwhile the iron of a phosphatization two is a kind of important multifunctional material, it is extensively concerned in the application of catalysis, magnetic etc. etc..It is early
The experiment of phase just has found that the iron of a phosphatization two is the functional material for having magnetic refrigeration effect.The iron of one phosphatization two has cheap be produced into
This, excellent performance, research and application to it can provide abundant experimental data for magnetic Refrigeration Technique.
The iron part of a phosphatization two that currently there are comes from industrial production, but dephasign therein, such as a phosphatization
One iron, a phosphatization three-iron, the iron of a silication one etc. are more, and purification unmanageable to the single-phase pure iron finished product of a phosphatization two.Mesh
The preceding method for preparing the iron of a phosphatization two mainly has pipe furnace heating, hydrothermal synthesis method and TPR- hydrogen atmosphere Program heating reductions
The phosphate using iron in method, and the A patents of publication No. CN 102442652 as presoma potassium borohydride be reducing agent,
The iron of a phosphatization two is prepared under argon gas protection.The main advantage and disadvantage of these methods are as follows：
Using pipe furnace heating, heating calcination can obtain the iron of one phosphatization of final product two to 1000 DEG C.Tube furnace method
The iron of a phosphatization two is prepared to have the following disadvantages：The starting material red phosphorus of reaction will distil being heated to 400 DEG C or so, and generation phosphorus steams
Vapour, so the phosphorus content entirely reacted is unmanageable, it is necessary to a large amount of excessive elemental phosphorous；In addition, under hot conditions, phosphorus steam meeting
Reacted with quartz ampoule, corrosion heating pipe furnace.
The iron of a phosphatization two prepared by hydrothermal synthesis method is poor as catalytic materials catalytic performance, and the hydro-thermal method time is grown, the cycle
It is long.
TPR- hydrogen atmosphere Program heating reduction methods use transition metal phosphate as presoma, have low cost,
The advantages of security performance is high, obtained product is purer, is widely used, but the temperature of this method and reaction time need strict control
System, heating-up time are longer.
It is reducing agent using the phosphate of iron as presoma potassium borohydride, the iron of a phosphatization two is prepared under argon gas protection,
Although can also obtain the purer iron particle sample of a phosphatization two, complex manufacturing is, it is necessary to which argon gas is protected, during vacuum drying
Between it is oversize, generally require more than 12 hours, the production cycle length, obtained product particle is small, is not easy post-production.
The content of the invention
The technical problem to be solved in the present invention is：One kind prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method, with
Solves prior art operation process complexity, Acceleration study ageing equipment, reaction time length, the iron product purity of a phosphatization two obtained
It is low, crystallinity is low, is the technical problem such as powdered or little particle, post-production difficulty.
The technical scheme is that：One kind prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method, 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 2：1 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
Two iron bulk samples.
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 two described in step 7 is single thing phase, free from admixture phase, is hexagonal structure, space group P-62m
(no.189), lattice parameterIt is a kind of typical alloy material with good metallic luster
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 two is obtained, its principle is：
2Fe+P-Fe2P
1st, the iron of a phosphatization two 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 two.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 two is relatively low.
2nd, the iron of a phosphatization two 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 two is poor, has substantial amounts of space, the standby iron of a phosphatization two of publication No. CN102442652A patent systems in sample
Particle is small, is not easy post-production, causes the difficulty of resistivity measurement.
3rd, the iron of a phosphatization two 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 two 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 two
The crystallization degree of product is significantly increased.The iron sample of a phosphatization two 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 two 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, the phosphorus content entirely reacted instant invention overcomes pipe furnace heating is difficult to control, and phosphorus steam can corrode heating
The problem of pipe furnace；The iron of a phosphatization two for overcoming hydrothermal synthesis method preparation makees that catalytic performance is poor, and hydro-thermal method time length is asked
Topic；Overcoming TPR- hydrogen atmosphere Program heating reduction method temperature and reaction time needs strictly to control, and the heating-up time is longer
The problem of；The method production cycle length in publication No. CN 102442652A patents is overcome, obtained product particle is small, is not easy
The problem of post-production.The preparation method of the present 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, the iron of a phosphatization two of acquisition have the characteristics that purity height, bulk can be processed, and this method is a phosphatization two
The research of the single thing phase of iron provides important leverage.In addition, the consumptive material that the present invention is required, if graphite, boron nitride ceramics are than existing
Quartz ampoule price is low in technology, has saved cost.
Brief description of the drawings
Fig. 1 is the XRD of the iron of a phosphatization two prepared by the embodiment of the present invention 3；
Fig. 2 is the BSE figures of the iron of a phosphatization two prepared by the embodiment of the present invention 3；
Fig. 3 is the Raman figure of the iron of a phosphatization two 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 2：1 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 two 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 two.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 two 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 2：1 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 two 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 two.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 two 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 2：1 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 two 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 1000 DEG C, and pressure is
2GPa, reaction time 3h.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 two.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 two be single thing phase, free from admixture phase.BSE images show the phosphatization two 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. one kind prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method, 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 2：1 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 two
Bulk sample.
2. one kind according to claim 1 prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method, 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.
3. one kind according to claim 1 prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method, 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.
4. one kind according to claim 1 prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method, it is characterised in that：
Thermocouple is provided with described high-pressure synthesis assembling block.
5. one kind according to claim 1 prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method, 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.
6. one kind according to claim 1 prepares the iron Fe of a phosphatization two at high temperature under high pressure2P method, it is characterised in that：
The pure iron of a phosphatization two described in step 7 is single thing phase, free from admixture phase, is hexagonal structure, and space group is P-62m (no.189),
Lattice parameterIt is a kind of typical alloy material with good metallic luster.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711066574.9A CN107651959B (en) | 2017-11-02 | 2017-11-02 | preparation of iron phosphide Fe under high temperature and high pressure2Method of P |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711066574.9A CN107651959B (en) | 2017-11-02 | 2017-11-02 | preparation of iron phosphide Fe under high temperature and high pressure2Method of P |
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| CN107651959A true CN107651959A (en) | 2018-02-02 |
| CN107651959B CN107651959B (en) | 2020-01-31 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112064114A (en) * | 2020-09-15 | 2020-12-11 | 燕山大学 | Layered metal phosphide GePxMethod for producing single crystal |
| CN112250082A (en) * | 2020-10-26 | 2021-01-22 | 燕山大学 | Transition metal compound and preparation method thereof |
| CN115233096A (en) * | 2022-07-13 | 2022-10-25 | 首钢集团有限公司 | Cold-rolled steel and preparation method thereof |
| US11732370B2 (en) | 2020-07-23 | 2023-08-22 | Shaanxi University Of Science & Technology | Core-shell FE2P@c-FE3C electrocatalyst and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1571188A2 (en) * | 2004-02-17 | 2005-09-07 | Kabushiki Kaisha Kobe Seiko Sho | Resin coated metal plate having excellent formability, weldability and corrosion resistance, and worked articles using the resin coated metal plate and method for manufacturing same |
| 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 CN201711066574.9A patent/CN107651959B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1571188A2 (en) * | 2004-02-17 | 2005-09-07 | Kabushiki Kaisha Kobe Seiko Sho | Resin coated metal plate having excellent formability, weldability and corrosion resistance, and worked articles using the resin coated metal plate and method for manufacturing same |
| 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11732370B2 (en) | 2020-07-23 | 2023-08-22 | Shaanxi University Of Science & Technology | Core-shell FE2P@c-FE3C electrocatalyst and preparation method and application thereof |
| CN112064114A (en) * | 2020-09-15 | 2020-12-11 | 燕山大学 | Layered metal phosphide GePxMethod for producing single crystal |
| CN112250082A (en) * | 2020-10-26 | 2021-01-22 | 燕山大学 | Transition metal compound and preparation method thereof |
| CN115233096A (en) * | 2022-07-13 | 2022-10-25 | 首钢集团有限公司 | Cold-rolled steel and preparation method thereof |
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