CN107778008B - Method for preparing iron phosphide FeP at high temperature and high pressure - Google Patents
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Abstract
The invention discloses a method for preparing iron phosphide under high temperature and high pressure, which comprises the following steps: analytically pure iron nano powder and red phosphorus powder are used as starting materials; the method comprises the following steps of (1): 1, fully grinding and mixing the materials in an agate mortar by using alcohol; pressing the ground mixed powder into a cylindrical sample by using a tablet press; processing the boron nitride ceramic rod into a round tube, and placing the round tube in an oven for drying; putting a cylindrical sample into a boron nitride circular tube, sealing the upper part and the lower part of the cylindrical sample by using a boron nitride ceramic plate, and putting the whole body into a cubic apparatus press for high-temperature high-pressure reaction; taking out the reacted sample, and removing boron nitride outside the sample to obtain a pure iron phosphide blocky sample; the method solves the technical problems that in the prior art, reaction variables are not easy to control, a quartz tube is corroded, the reaction time is long, the product purity is low, the crystallinity is low, the product is powder, and the later-stage processing cannot be carried out.
Description
Technical Field
The invention belongs to the field of functional material synthesis, and particularly relates to a method for preparing iron phosphide FeP at high temperature and high pressure.
Background
In industry, iron-phosphide FeP is also called iron phosphide and ferrophosphorus, is a byproduct of phosphorus chemical industry, and is widely applied to metallurgy, smelting and chemical industry. The superfine ferrophosphorus powder has the characteristics of electric conduction, heavy corrosion resistance, marine organism adsorption resistance, environmental protection and the like, is a new technological product in the paint and coating industry, and particularly has the advantages of environmental protection, protection of the health of electric welders, low price and heavy corrosion resistance when replacing zinc powder. Has been widely used in epoxy zinc-rich primer, conductive coating, filler and the like, and is suitable for any paint coating to be used as an antirust and anticorrosive pigment. Meanwhile, the iron phosphide can also be used as a lithium ion battery cathode material, and is an important raw material and a research object for researching and developing a novel lithium ion battery; the iron phosphide is also an additive for improving the efficiency of the hydrogen evolution reaction, and is an object of intensive research in the field of high-performance hydrogen evolution reaction materials.
The industrial grade ferrophosphorus powder existing in the current market mainly comprises FeP and Fe2P, FeSi monosilicide. Compared withPure iron monophosphates products can only be obtained by laboratory synthesis and are used for studying important properties of single phase, such as resistivity, magnetic susceptibility and the like. The laboratory synthesis of iron phosphide reported at present mainly comprises a quartz tube vacuum method: using iron and red phosphorus according to a molar ratio of 1: 1, sealing the mixture in a vacuumized quartz tube, heating and burning the mixture to 1000 ℃ to obtain a final product, namely iron phosphide. Although the quartz tube vacuum method enables to obtain iron mono phosphide, the following drawbacks still remain: because red phosphorus is sublimated and volatilized when being heated to about 400 ℃ under normal pressure, the loss of red phosphorus amount of nominal proportion is caused, the phosphorus content of the whole reaction is difficult to control, and the obtained iron-phosphide sample is impure; under the condition of high temperature, the volatilized phosphorus steam can react with the quartz tube to corrode the sealed quartz tube, experiment failure can be caused in a long sintering process, the product obtained by the method is powdery, later-stage processing cannot be performed to meet detection of some properties such as conductivity and the like, the crystallinity of the obtained product is poor, and the requirement of spectrum tests such as Raman scattering and the like on the crystallinity of a sample cannot be met. Therefore, we have to search for new synthetic methods of monophosphorous-iron to improve the deficiencies of the current synthetic methods.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: a method for preparing FeP under high temperature and high pressure aims to solve the technical problems that the operation process is complex, the aging of experimental equipment is accelerated, the reaction time is long, the obtained FeP product has low purity and low cleanliness, is powdery, is difficult to process at a later stage and the like in the prior art.
The technical scheme of the invention is as follows: a process for preparing an iron-phosphide, FeP, at elevated temperature and pressure comprising:
step 1: analytically pure reduced iron powder and red phosphorus powder are used as starting materials;
step 2: mixing iron nano powder and red phosphorus powder according to a molar ratio of 1: 1, mixing, putting into a mortar, adding alcohol, and grinding until the liquid is completely volatilized;
and step 3: placing the ground mixed powder into a circular mold by using a tablet press for tabletting to obtain a cylindrical sample;
and 4, step 4: processing a boron nitride BN ceramic rod into a round tube, and drying in an oven;
and 5: putting the sample pre-pressed and molded in the step 3 into the boron nitride round tube in the step 4, and sealing the upper part and the lower part of the sample by using a boron nitride ceramic plate;
step 6: assembling the cylindrical sample prepared in the step 5 in a high-pressure synthesis assembly block and placing the cylindrical sample in a cubic apparatus large press for high-temperature high-pressure reaction;
and 7: and taking out the reacted sample, and removing the boron nitride sleeve outside the sample to obtain the pure iron phosphide blocky sample.
The specific preparation method in the step 5 comprises the following steps: and (3) machining the boron nitride ceramic rod into a circular tube with the length of 10mm, the outer diameter of 10mm and the inner diameter of 6mm by using a lathe, wherein the circular tube is used as a sleeve for wrapping the sample, then putting the cylindrical sample obtained in the step (3) into the circular tube, and sealing the upper part and the lower part of the circular tube by using a boron nitride ceramic plate.
The method for synthesizing the assembly block by high pressure in the step 6 comprises the following steps:
6.1, selecting a pyrophyllite block, and drilling a circular through hole in the center of the pyrophyllite block;
6.2, sleeving a cylindrical graphite heating furnace in the circular through hole;
6.3, placing a sample wrapped by a boron nitride tube in the middle of a graphite heating furnace;
and 6.4, sealing the upper end and the lower end of the circular graphite heating furnace by pyrophyllite plugs.
And a thermocouple is arranged in the high-pressure synthesis assembly block.
And 6, the temperature of the high-temperature high-pressure reaction is 800-1200 ℃, the pressure is 1-3GPa, and the reaction time is 1-5 hours.
The pure mono-iron phosphide in step 7 is a single phase, free of impurity phase, hexagonal in structure, space group Pnma (No.62), lattice parameter
Has good metallic luster, and is a typicalAnd (3) a type of alloy material.
The invention has the beneficial effects that:
analytically pure iron nano powder and red phosphorus powder are used as starting raw materials, and a solid-phase reaction method is adopted to obtain a phosphorized-iron sample under high temperature and high pressure, and the principle is as follows:
Fe+P－FeP
1. the iron monophosphosphate prepared by the invention is a single-phase sample with high purity, and the high-temperature and high-pressure experimental sample is wrapped by the high-density boron nitride ceramic and is carried out in a closed cavity, so that the volatilization loss of red phosphorus is avoided, the reaction can be strictly carried out according to the nominal proportion, and the pure iron monophosphosphate is obtained. Meanwhile, the solid-phase reaction rate of molecular diffusion is accelerated under the conditions of high temperature and high pressure, so that the reaction can be completed within one hour, and the synthesis efficiency is greatly improved. Solves the problem that the purity of the obtained iron-phosphide sample is low because the volatilization amount of red phosphorus in the normal-pressure synthesis method is difficult to control and the nominal proportioning of the red phosphorus in the solid-phase reaction is lost.
2. The iron phosphide prepared by the invention is a high-density sintered block sample, and the compact block sample can be processed and polished into a geometric shape required by resistivity test, so that the resistivity research is guaranteed. In contrast, the atmospheric pressure synthesis method sinters the mono-iron phosphide poorly formed and had a large number of voids in the sample, resulting in difficulty in resistivity testing.
3. The phosphorized monoiron prepared by the invention is a sample with good crystallinity. Because the high pressure can improve the decomposition temperature of the material, the reaction temperature for synthesizing the iron phosphide at high temperature and high pressure is much higher than that of normal pressure sintering, so that the higher reaction temperature not only completes the high-temperature and high-pressure solid-phase reaction, but also completes the recrystallization reaction of the sample, and the crystallization degree of the iron phosphide sample is greatly improved. The phosphorization-iron sample with large grains provides guarantee for Raman scattering and other spectrum tests. Compared with the prior art, the method has the advantages that the reaction temperature is low, the crystallinity of the iron phosphide sintered by the normal-pressure synthesis method is poor, and the requirements of spectrum tests such as Raman scattering and the like on the crystallinity of the sample cannot be met.
In conclusion, the invention overcomes the problems that the phosphorus content of the whole reaction of the vacuum method of the quartz tube is difficult to control, the phosphorus steam can corrode the quartz tube, the reaction time is long, the reaction product is powdery, the post processing is difficult, the product has more impurities and the crystallinity is low. The preparation method has the advantages of simple operation process, short time and period, low cost, difficulty in damaging experimental equipment and the like, the obtained iron mono-phosphide has the characteristics of high purity, the block can be processed and the like, the method provides important guarantee for the research of the single phase of the iron mono-phosphide, and in addition, the consumable materials required by the preparation method, such as graphite and boron nitride ceramics, are lower in price than the quartz tube in the prior art, and the cost is saved.
Drawings
FIG. 1 is an XRD pattern of a monophosphorous monoiron prepared in example 3 of the present invention;
FIG. 2 is a BSE graph of an iron phosphide prepared in example 3 of the present invention;
FIG. 3 is a Raman spectrum of iron monophosphates prepared in example 3 of the present invention.
Detailed Description
The invention will be further described with reference to the following drawings and specific embodiments:
example 1
Analytically pure iron nano powder (Fe) and red phosphorus powder (P) were used as starting materials, which were mixed in a molar ratio of 1: 1, fully grinding and mixing the mixture in an agate mortar by using alcohol, taking 0.30g of iron-phosphorus mixed powder, pressing the iron-phosphorus mixed powder into a cylinder with the diameter of 6mm multiplied by 6mm by using a powder tablet press, processing a boron nitride ceramic rod into a boron nitride ceramic tube with the length of 10mm, the outer diameter of 10mm and the inner diameter of 6mm, drying the boron nitride ceramic tube in an oven at the temperature of 150 ℃ for 2 hours, putting the powder cylinder body into the boron nitride ceramic tube, and sealing the upper part and the lower part by using a 2mm boron nitride ceramic plate to finish the high-pressure assembly block. Assembling a high-pressure assembling block:
① 32 a circular through hole with the diameter of 12mm is drilled in the center of a pyrophyllite cube with the diameter of 32mm x 32 mm;
② graphite sleeve heating furnace with outer diameter of 12mm and inner diameter of 10mm is sleeved in the circular through hole of the pyrophyllite block;
③ A boron nitride cylinder containing iron-phosphorus mixed powder is placed in the middle of the graphite sleeve heating furnace, and the upper part and the lower part are plugged by pyrophyllite plugs with the diameter of 10 mm.
The invention has the advantages that ① uses a thermocouple to control temperature, a heating system adjusts heating power through the temperature fed back by the thermocouple so as to change the temperature, the method can realize instant monitoring of the temperature and is suitable for experiments with high temperature measurement precision, ② pyrophyllite is used as a primary pressure transmission medium and has good pressure transmission, machinability, heat resistance and heat preservation and insulativity, boron nitride is a ceramic material with strong processability and is used as a secondary pressure transmission medium to ensure that the pressure in a cavity is uniform, the sealing performance is good, the boron nitride is stable, the quality of sealing materials of products cannot be polluted and damaged, and the most suitable preparation of iron phosphide is completed, and ③ graphite furnace is used as a heating furnace and has high temperature uniformity.
And (3) putting the assembly block into a cubic apparatus press for high-temperature high-pressure reaction, wherein the set temperature is 800 ℃, the pressure is 1GPa, and the reaction time is 5 h. And after the high-temperature high-pressure reaction is finished, taking out the obtained sample, and removing boron nitride on the surface of the sample to obtain the pure iron monophosphosphate sample. The result of X-ray diffraction electron probe analysis shows that the iron phosphide prepared by the preparation method is a single phase and has no impurity phase.
Example 2
Analytically pure iron nano powder (Fe) and red phosphorus powder (P) were used as starting materials, which were mixed in a molar ratio of 1: 1, fully grinding and mixing the mixture in an agate mortar by using alcohol, taking 0.30g of iron-phosphorus mixed powder, pressing the iron-phosphorus mixed powder into a cylinder with the diameter of 6mm multiplied by 6mm by using a powder tablet press, processing a boron nitride ceramic rod into a boron nitride ceramic tube with the length of 10mm, the outer diameter of 10mm and the inner diameter of 6mm, drying the boron nitride ceramic tube in an oven at the temperature of 150 ℃ for 2 hours, putting the powder cylinder body into the boron nitride ceramic tube, and sealing the upper part and the lower part by using a 2mm boron nitride ceramic plate to finish the high-pressure assembly block. Assembling a high-pressure assembling block:
① 32 a circular through hole with the diameter of 12mm is drilled in the center of a pyrophyllite cube with the diameter of 32mm x 32 mm;
② graphite sleeve heating furnace with outer diameter of 12mm and inner diameter of 10mm is sleeved in the circular through hole of the pyrophyllite block;
③ A boron nitride cylinder containing iron-phosphorus mixed powder is placed in the middle of the graphite sleeve heating furnace, and the upper part and the lower part are plugged by pyrophyllite plugs with the diameter of 10 mm.
The invention has the advantages that ① uses a thermocouple to control temperature, a heating system adjusts heating power through the temperature fed back by the thermocouple so as to change the temperature, the method can realize instant monitoring of the temperature and is suitable for experiments with high temperature measurement precision, ② pyrophyllite is used as a primary pressure transmission medium and has good pressure transmission, machinability, heat resistance and heat preservation and insulativity, boron nitride is a ceramic material with strong processability and is used as a secondary pressure transmission medium to ensure that the pressure in a cavity is uniform, the sealing performance is good, the boron nitride is stable, the quality of sealing materials of products cannot be polluted and damaged, and the most suitable preparation of iron phosphide is completed, and ③ graphite furnace is used as a heating furnace and has high temperature uniformity.
And (3) putting the assembly block into a cubic apparatus press for high-temperature high-pressure reaction, wherein the set temperature is 1200 ℃, the pressure is 3GPa, and the reaction time is 1 h. And after the high-temperature high-pressure reaction is finished, taking out the obtained sample, and removing boron nitride on the surface of the sample to obtain the pure iron monophosphosphate sample. The result of X-ray diffraction electron probe analysis shows that the iron phosphide prepared by the preparation method is a single phase and has no impurity phase.
Embodiment 3
Analytically pure iron nano powder (Fe) and red phosphorus powder (P) were used as starting materials, which were mixed in a molar ratio of 1: 1, fully grinding and mixing the mixture in an agate mortar by using alcohol, taking 0.30g of iron-phosphorus mixed powder, pressing the iron-phosphorus mixed powder into a cylinder with the diameter of 6mm multiplied by 6mm by using a powder tablet press, processing a boron nitride ceramic rod into a boron nitride ceramic tube with the length of 10mm, the outer diameter of 10mm and the inner diameter of 6mm, drying the boron nitride ceramic tube in an oven at the temperature of 150 ℃ for 2 hours, putting the powder cylinder body into the boron nitride ceramic tube, and sealing the upper part and the lower part by using a 2mm boron nitride ceramic plate to finish the high-pressure assembly block. Assembling a high-pressure assembling block:
① 32 a circular through hole with the diameter of 12mm is drilled in the center of a pyrophyllite cube with the diameter of 32mm x 32 mm;
② graphite sleeve heating furnace with outer diameter of 12mm and inner diameter of 10mm is sleeved in the circular through hole of the pyrophyllite block;
③ A boron nitride cylinder containing iron-phosphorus mixed powder is placed in the middle of the graphite sleeve heating furnace, and the upper part and the lower part are plugged by pyrophyllite plugs with the diameter of 10 mm.
The invention has the advantages that ① uses a thermocouple to control temperature, a heating system adjusts heating power through the temperature fed back by the thermocouple so as to change the temperature, the method can realize instant monitoring of the temperature and is suitable for experiments with high temperature measurement precision, ② pyrophyllite is used as a primary pressure transmission medium and has good pressure transmission, machinability, heat resistance and heat preservation and insulativity, boron nitride is a ceramic material with strong processability and is used as a secondary pressure transmission medium to ensure that the pressure in a cavity is uniform, the sealing performance is good, the boron nitride is stable, the quality of sealing materials of products cannot be polluted and damaged, and the most suitable preparation of iron phosphide is completed, and ③ graphite furnace is used as a heating furnace and has high temperature uniformity.
And (3) putting the assembly block into a cubic apparatus press for high-temperature high-pressure reaction, wherein the set temperature is 1100 ℃, the pressure is 2GPa, and the reaction time is 4 h. And after the high-temperature high-pressure reaction is finished, taking out the obtained sample, and removing boron nitride on the surface of the sample to obtain the pure iron monophosphosphate sample. The result of X-ray diffraction electron probe analysis shows that the iron phosphide prepared by the preparation method is a single phase and has no impurity phase. BSE images show that the iron phosphide prepared by the preparation method is of a crystal structure and large in grain size, and Raman spectrum tests are completed.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (4)
1. A process for preparing an iron-phosphide, FeP, at elevated temperature and pressure comprising:
step 1: analytically pure reduced iron powder and red phosphorus powder are used as starting materials;
step 2: mixing iron nano powder and red phosphorus powder according to a molar ratio of 1: 1, mixing, putting into a mortar, adding alcohol, and grinding until the liquid is completely volatilized;
and step 3: placing the ground mixed powder into a circular mold by using a tablet press for tabletting to obtain a cylindrical sample;
and 4, step 4: processing a boron nitride BN ceramic rod into a round tube, and drying in an oven;
and 5: putting the sample pre-pressed and molded in the step 3 into the boron nitride round tube in the step 4, and sealing the upper part and the lower part of the sample by using a boron nitride ceramic plate;
step 6: assembling the cylindrical sample prepared in the step 5 in a high-pressure synthesis assembly block and placing the cylindrical sample in a cubic apparatus large press for high-temperature high-pressure reaction;
the method for synthesizing the assembly block by high pressure in the step 6 comprises the following steps:
6.1, selecting a pyrophyllite block, and drilling a circular through hole in the center of the pyrophyllite block;
6.2, sleeving a cylindrical graphite heating furnace in the circular through hole;
6.3, placing a sample wrapped by a boron nitride tube in the middle of a graphite heating furnace;
step 6.4, sealing the upper end and the lower end of the round graphite heating furnace by pyrophyllite plugs;
6, the temperature of the high-temperature high-pressure reaction is 800-1200 ℃, the pressure is 1-3GPa, and the reaction time is 1-5 hours;
and 7: and taking out the reacted sample, and removing the boron nitride sleeve outside the sample to obtain the pure iron phosphide blocky sample.
2. The method of claim 1 for preparing an iron phosphide FeP under high temperature and high pressure, wherein: the specific preparation method in the step 5 comprises the following steps: and (3) machining the boron nitride ceramic rod into a circular tube with the length of 10mm, the outer diameter of 10mm and the inner diameter of 6mm by using a lathe, wherein the circular tube is used as a sleeve for wrapping the sample, then putting the cylindrical sample obtained in the step (3) into the circular tube, and sealing the upper part and the lower part of the circular tube by using a boron nitride ceramic plate.
3. The method of claim 1 for preparing an iron phosphide FeP under high temperature and high pressure, wherein: and a thermocouple is arranged in the high-pressure synthesis assembly block.
4. The method for preparing mono-iron phosphide FeP at high temperature and high pressure as claimed in claim 1, wherein the pure mono-iron phosphide in step 7 is a single phase, free of impurity phase, has a hexagonal structure, has a space group of Pnma (No.62), has a lattice parameter of a = 5.18 Å, b = 3.09 Å and c = 5.78 Å, has good metallic luster, and is a typical alloy material.
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| CN110002419B (en) * | 2019-04-18 | 2021-07-02 | 王东升 | Preparation method of high-tap-density iron phosphate |
| CN112250082B (en) * | 2020-10-26 | 2022-03-22 | 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 |
| CN114843478B (en) * | 2022-05-23 | 2023-05-23 | 广东技术师范大学 | Nanometer FeP for lithium ion battery 2 Preparation method of/C/CNTs composite material |
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| 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 |
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| 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 |
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