CN115818589A - Method for synthesizing two-dimensional transition metal nitride material with room-temperature ferromagnetism through regulating and controlling flow velocity of reaction gas - Google Patents
Method for synthesizing two-dimensional transition metal nitride material with room-temperature ferromagnetism through regulating and controlling flow velocity of reaction gas Download PDFInfo
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- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 13
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- 238000000137 annealing Methods 0.000 claims description 10
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
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- 150000003839 salts Chemical class 0.000 claims description 7
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
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- 238000005406 washing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
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- 238000004108 freeze drying Methods 0.000 claims description 3
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention discloses a method for synthesizing a two-dimensional transition metal nitride material with room-temperature ferromagnetism by regulating and controlling the flow rate of reaction gas. The method flexibly controls the final product by changing the experimental parameters, and has wider applicability and stronger controllability. The preparation process can realize the synthesis of the two-dimensional layered transition metal nitride without high temperature and high pressure, and has simple operation and low cost. The obtained product has room temperature ferromagnetism, meets the requirements of practical application better, has the advantages of stable structure, uniform appearance and the like, and solves the problems that the phase change temperature of the magnetic material is low, the magnetic material cannot be applied to conventional conditions, and a sample is unstable.
Description
Technical Field
The invention belongs to the technical field of room temperature ferromagnetic materials, and particularly relates to a method for synthesizing a two-dimensional transition metal nitride material with room temperature ferromagnetism by regulating and controlling the flow rate of reaction gas.
Background
With the rapid development of artificial intelligence and the Internet of things, the information amount is increased explosivelyWith the advent of the big data age, the conventional semiconductor integrated circuit gradually approaches the critical point of quantum confinement effect in the process. There is a need to find a new way to solve the dilemma faced by the current information storage. In the spintronics, the giant magnetoresistance effect, the tunneling magnetoresistance effect and the spin-orbit torque effect reveal that the movement of electrons can be regulated and controlled by controlling the spin magnetization direction, so that the information storage with high speed, low power consumption and nonvolatility is realized. Spintronics devices have shown a very broad prospect of development, from the first MRAM to the later STT-MRAM, to today's SOT-MRAM. The development of spintronics devices has not been isolated from the study of two-dimensional magnetic materials. Two very representative two-dimensional magnetic materials CrI from 2017 3 (Curie temperature 61K), cr 2 Ge 2 Te 6 (Curie temperature 68K) since this discovery, an increasing variety of materials have been investigated, including: transition metal phosphorus sulfur compounds, transition metal oxyhalide compounds, and the like. However, most of these materials have ferromagnetism at low temperature, the curie temperature is difficult to reach the room temperature, and simultaneously, the materials are easy to oxidize in the air environment, and cannot meet the requirements of practical application of the spintronics device. Therefore, the development of ferromagnetic materials with simple preparation, stable structure and Curie temperature reaching room temperature is a very important research direction.
Transition Metal Nitrides (TMNs) are a very abundant material, have numerous members and stable structure, and are widely applied to the fields of energy conversion, energy storage and the like. At present, the most widely applied synthesis mode for 2D TMNs is to use high pressure to prevent N atoms from diffusing out of metal lattices at high temperature, but the method has harsh conditions and huge consumption, has great danger under the conditions of high temperature and high pressure, has single product, and cannot flexibly regulate and control the final product by changing experimental parameters. In addition, (NH) may be used 4 ) 6 H 2 W 12 O 40 ·x H 2 The mixture of O and KCl obtains similar specific products through annealing, and the scheme also cannot realize the regulation of the product structure.
The existing sample synthesis method can only obtain a specific product, and can not realize the preparation of similar compounds containing different atomic percentages through simple regulation, namely, the problems of poor applicability, low sample synthesis efficiency, harsh reaction conditions and the like exist. In addition, most of the existing two-dimensional magnetic materials have ferromagnetism at low temperature, and few of the existing two-dimensional magnetic materials have intrinsic room temperature ferromagnetism, which severely limits the wide application of the materials.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses a method for synthesizing a two-dimensional room-temperature ferromagnetic material by regulating and controlling the flow rate of reaction gas. Meanwhile, the obtained products have room-temperature ferromagnetism, so that a new member is added to room-temperature ferromagnetic materials, and a new idea is provided for sample synthesis. The problems that the phase change temperature of the magnetic material is low, the magnetic material cannot be applied to conventional conditions, and a sample is unstable are solved.
In order to realize the purpose, the invention adopts the technical scheme that:
a method for synthesizing a two-dimensional transition metal nitride material with room-temperature ferromagnetism by regulating and controlling the flow rate of reaction gas comprises the following steps:
uniformly mixing transition metal oxide and oxysalt containing transition metal by ball milling to obtain mixed powder; the molecular formula of the transition metal oxide is AO 3 The oxygen-containing salt containing a transition metal has the formula B 2 AO 4 (ii) a Wherein: a is Mo or W, B is Na, K or Li; the oxygen-containing salt containing transition metal is used as fluxing agent to catalyze the reaction of transition metal oxide, and can be removed by ultrasonic water washing after the subsequent annealing is finished.
Flatly spreading the mixed powder in a square boat, then placing the square boat in the central position of a quartz tube furnace, heating to 650-800 ℃ at a certain speed, introducing reaction gas containing ammonia gas into the quartz tube furnace at different gas flow rates, and annealing for 5-8h; preferably, the flow rate of the reaction gas is 10sccm to 75sccm.
And dispersing the obtained powder in water after annealing treatment, performing ultrasonic washing, separating insoluble substances, and freeze-drying to obtain the two-dimensional transition metal nitride material with room-temperature ferromagnetism.
In one embodiment, the transition metal refers to Mo, and correspondingly, the transition metal oxide is MoO 3 The oxysalt of the transition metal is Na 2 MoO 4 ·2H 2 O、K 2 MoO 4 ·2H 2 O or Li 2 MoO 4 ·2H 2 O。
In another embodiment, the transition metal is W, and correspondingly, the transition metal oxide is WO 3 The oxygen-containing salt of the transition metal is Na 2 WO 4 ·2H 2 O、K 2 WO 4 ·2H 2 O or Li 2 WO 4 ·2H 2 O。
The invention adopts the following chemical reaction principle:
the transition metal oxide used in the present invention is MoO 3 Or WO 3 W and Mo belong to the same main group (VIB group) elements and have similar chemical characteristics, so that W and Mo can be used as the raw materials of the invention. With MoO 3 The reaction principle is illustrated as follows: moO 3 Is reduced to MoO in reaction gas containing ammonia gas 2 The metal oxide is melted to generate [ MoO ] under the catalysis of oxygen-containing salt 6 ]Octahedron, at high temperature [ MoO ] 6 ]Octahedron is first reacted with NH 3 Reaction to [ MoN x ]Octahedron, then assembled into a two-dimensional layered structure of MoN x I.e., a transition metal nitride. In the above reaction, changing the flow rate of the reactant gas will change the reactant and NH in the gas 3 The contact and reaction area of (A) and the amount of N contained in the product to be produced are different, that is, when the flow rate is high (75 sccm), it is considered that insufficient amination is caused and an oligonitrogen compound is produced. Through research, when the volume content of ammonia in the reaction gas is 5%, and the gas flow rate is 75sccm, the product is Mo 2 N; when the gas flow rate is 10sccm, the product is Mo 5 N 6 (ii) a The gas flow rate is 10sccm-75sBetween ccm, a mixed phase of the two materials is obtained.
Compared with the prior art, the invention has the following beneficial effects:
the method provided by the invention utilizes the same synthesis process, the preparation of the transition metal nitride containing different atomic percentages can be realized only by regulating and controlling the flow rate of the reaction gas, and the products have two-dimensional layered micro-morphology and room-temperature ferromagnetism. The method flexibly controls the final product by changing the experimental parameters, and has wider applicability and stronger controllability. The preparation process can realize the synthesis of the two-dimensional layered transition metal nitride without high temperature and high pressure, and has simple operation and low cost. The obtained product has room-temperature ferromagnetism, meets the requirements of practical application, and has the advantages of stable structure, uniform appearance and the like.
Drawings
Figure 1 is an XRD of the products prepared in example 1 and example 2.
FIG. 2 shows the magnetic properties at 300K of the products prepared in example 1 and example 2.
FIG. 3 shows Mo prepared in example 1 2 TEM image of N.
FIG. 4 shows Mo prepared in example 2 5 N 6 SEM image of (d).
Detailed Description
The present invention will be further described with reference to the following examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
In addition, the preparation processes in the following examples are conventional means in the prior art unless otherwise specified, and therefore, detailed descriptions thereof are omitted; the raw materials used in the following embodiments are all commercially available products.
Example 1
(1) Mixing the components in a molar ratio of 1:1 MoO 3 With Na 2 MoO 4 ·2H 2 Uniformly mixing the O by ball milling, and then grinding to reduce the particle size of the O to obtain mixed powder;
(2) Taking the mixed powder in the step 1 and tilingIn the ark, the ark was then placed in the center of the quartz tube furnace, and the temperature was raised to 650 ℃ at a rate of 1 ℃/min, thereby 5% of NH was contained 3 Annealing for 7h at a gas flow rate of 75sccm in an Ar atmosphere;
(3) Ultrasonically washing the annealed powder in deionized water, centrifuging, and finally freeze-drying to obtain a final product Mo 2 N；
Example 2
Different from example 1 in the content of 5% NH in the step (2) of example 2 3 The gas flow rate of Ar atmosphere was 10sccm, and the other processes were the same as in example 1, and Mo was prepared as a product 5 N 6 。
Structural characterization and Performance testing
XRD examination of the products prepared in examples 1 and 2 showed that the diffraction peaks corresponding to two pure phase nitrides of Mo at 75sccm were observed at two different gas flow rates, as shown in FIG. 1, and that XRD examination of the products in FIG. 1 showed that 2 N, mo at 10sccm 5 N 6 . The XRD standard cards are respectively PDF #25-1366 (Mo) 2 N)、PDF#51-1326(Mo 5 N 6 )。
The magnetic properties were tested at 300K for the products prepared in example 1 and example 2, and the results are shown in figure 2. Fig. 2 is a graph showing the magnetic properties tested at 300K for the products prepared in example 1 and example 2, and the right graph is a partial enlargement (low field portion) of the left graph. The hysteresis phenomenon is obviously observed from the M-H curve in the graph, and at the temperature of 300K, the coercive field of more than 100Oe can be still maintained by the two products, namely, the two products have room temperature ferromagnetism.
FIG. 3 shows Mo product of example 1 2 TEM image of N, FIG. 4 is Mo product prepared in example 2 5 N 6 SEM image of (d). As can be seen from FIGS. 3 and 4, the two products are two-dimensional lamellar nanosheets, and are ultrathin in thickness and smooth in surface.
Example 3
Different from example 1 in that, in example 3, in step (2), 5% NH 3 The gas flow rate of Ar atmosphere of (1) was 50sccm, and the obtained product was Mo 2 N and Mo 5 N 6 Mixed phases of (1).
Example 4
In contrast to example 1, WO was used for step (1) in example 4 3 Replacement of MoO 3 And with Na 2 WO 4 ·2H 2 Substitution of O for Na 2 MoO 4 ·2H 2 O; the temperature of the quartz tube furnace in the step (2) is 750 ℃, other processes are the same as those in the example 1, and the prepared product is W 2 N。
It should be noted that, in other embodiments, the object of the present invention can be achieved when the experimental process satisfies the following conditions:
the temperature of the quartz tube furnace is preferably 650 to 800 ℃, and can be 650 ℃, 700 ℃, 750 ℃, 800 ℃ or the like; the time for the annealing treatment is preferably 5 to 8 hours, and specifically, 5 hours, 6 hours, 7 hours, or 8 hours. The volume ratio of ammonia gas in the reaction gas is preferably 5% to 10%, and specifically may be 5%, 7%, 8%, 10%, or the like. The above process parameters can be properly selected by those skilled in the art according to actual needs, and all of them can achieve the purpose of the present invention.
It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (7)
1. A method for synthesizing a two-dimensional transition metal nitride material with room-temperature ferromagnetism by regulating and controlling the flow rate of reaction gas is characterized by comprising the following steps: the method comprises the following steps:
uniformly mixing transition metal oxide and oxysalt containing transition metal by ball milling to obtain mixed powder; the molecular formula of the transition metal oxide is AO 3 The molecular formula of the oxygen-containing salt containing transition metal is B 2 AO 4 (ii) a Wherein: a is Mo or W, B is Na, K or Li;
placing the mixed powder in an environment of 650-800 ℃ for annealing treatment, and simultaneously introducing reaction gas containing ammonia gas;
and dispersing the obtained powder in water after annealing treatment, performing ultrasonic washing, separating insoluble substances, and freeze-drying to obtain the two-dimensional transition metal nitride material with room-temperature ferromagnetism.
2. The method for synthesizing a two-dimensional transition metal nitride material having room-temperature ferromagnetism through flow rate control of reaction gas according to claim 1, wherein: the transition metal oxide is MoO 3 The oxygen-containing salt containing transition metal is Na 2 MoO 4 ·2H 2 O、K 2 MoO 4 ·2H 2 O or Li 2 MoO 4 ·2H 2 O。
3. The method for synthesizing a two-dimensional transition metal nitride material having room temperature ferromagnetism through flow rate control of reaction gas according to claim 1, wherein: the transition metal oxide is WO 3 The oxygen-containing salt containing transition metal is Na 2 WO 4 ·2H 2 O、K 2 WO 4 ·2H 2 O or Li 2 WO 4 ·2H 2 O。
4. The method for synthesizing a two-dimensional transition metal nitride material having room-temperature ferromagnetism through flow rate control of reaction gas according to claim 1, wherein: the reaction gas comprises ammonia gas and protective gas, and the flow rate of the reaction gas is 10sccm-75sccm.
5. The method for synthesizing a two-dimensional transition metal nitride material having room-temperature ferromagnetism through flow rate control of reaction gas according to claim 4, wherein: the protective gas is an inert gas.
6. The method for synthesizing a two-dimensional transition metal nitride material having room-temperature ferromagnetism through flow rate control of reaction gas according to claim 1, wherein: the time of the annealing treatment is 5-8h.
7. The method for synthesizing a two-dimensional transition metal nitride material having room-temperature ferromagnetism through flow rate control of reaction gas according to claim 1, wherein: the annealing treatment adopts a quartz tube furnace as equipment.
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