CN113387335B - Series of multilayer high-entropy structural compounds and preparation method thereof - Google Patents
Series of multilayer high-entropy structural compounds and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a series of multilayer high-entropy structural compounds and a preparation method thereof. The multilayer high-entropy structural compound is a series of transition metal layered compounds, and the molecular formula is expressed as (HEM) B ) x (HEM A )X 2 HEM is a high entropy metalA combination of elements consisting of four or more metal elements, HEM A 、HEM B Are two groups of high entropy elements respectively, x is HEM B The intercalation amount of the high-entropy metal elements is x, x is more than 0 and less than or equal to 1, and x is one or the combination of more of S, se and Te elements. The invention is in MX 2 HEM (high-entropy metal element combination) with M-position of laminated structure A On the basis of replacement, a layer of high-entropy metal atom HEM is introduced between layers B And the intercalation amount can be regulated and controlled to obtain a series of compounds with multilayer high-entropy structures, and the series of materials have great potential in the application fields of energy conversion, energy storage and the like. The multilayer high-entropy structural design concept provides a new idea for people to explore new high-entropy compounds.
Description
Technical Field
The invention relates to an inorganic non-metallic material, in particular to a series of multilayer high-entropy structural compounds and a preparation method thereof.
Background
With the heat of research on high-entropy alloys, high-entropy compounds have also entered the vigorous development stage in recent years, and high-entropy materials have already covered the fields of oxides, carbides, silicides, chalcogenides, and the like. The high-entropy layered compound, such as a high-entropy oxide, has excellent performance in the energy storage field of lithium ion batteries, super capacitors and the like due to the chemical stability of a high-entropy structure and the crystallographic characteristics of the layered structure. Recently, high entropy layered chalcogenides have also been reported and found to have good performance in catalytic reduction.
At present, the layered high-entropy material is still a single-layer high-entropy structure in the aspect of structure design, and the high-entropy structure layer is mainly at the position of the metal layer of the layered structure unit. However, compounds having a multi-layer high-entropy structure have not been reported yet.
Disclosure of Invention
The invention aims to provide a method for synthesizing a series of multilayer high-entropy structural compounds (HEM) by using a solid phase intercalation method B ) x (HEM A )X 2 The parent molecular formula of (HEM) A )X 2 The intercalated parent body has a high-entropy structure, namely a high-entropy metal element HEM B By high temperature solid phase sintering, in this case of high entropy compounds (HEM) A )X 2 A layer of high-entropy metal atoms is introduced between layers.
In order to achieve the purpose, the invention adopts the following technical scheme:
multilayer high entropy structured compound, the molecular formula of which is expressed as (HEM) B ) x (HEM A )X 2 Wherein the HEM is a high-entropy metal element combination and consists of four or more metal elements, and the HEM is A 、HEM B Are respectively two groups of high-entropy metal element combinations, x is HEM B Intercalation amount of high-entropy metal elements.
Further, HEM A Is the combination of any four or more than four metal elements of Ti, zr, hf, V, nb, ta, cr, mo, W, re, os, rh, ir, au, pd and Pt, the element proportion can be equal ratio or unequal ratio, and the total element amount is 1.
X is one or the combination of more of S, se and Te elements.
HEM B Is the combination of four or more than four metal elements which can be intercalated in the periodic table of the elements, the proportion of the elements is equal ratio, the total amount of the elements is x, x is more than 0 and less than or equal to 1.
Further, HEM B Is the combination of four or more metal elements in Fe, co, cr, ni, mn, V, cu, ag and Zn.
For example: (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.25 Cr 0.25 V 0.25 Ta 0.25 )Se 2 。
The preparation method of the series of multilayer high-entropy structural compounds comprises the following steps:
1) Weighing HEM according to atomic number percentage A Uniformly mixing the powder and the X element powder according to the proportion of 1;
2) Putting the uniformly mixed powder into a vacuum quartz tube, vacuumizing the quartz tube, sealing, sintering in a high-temperature furnace at 800-1300 ℃, preserving heat for 20-36h, quickly taking the quartz tube out of the furnace, putting the quartz tube into a substance such as water or ice water mixture for quenching treatment, taking the quenched product out of the vacuum quartz tube, and grinding to obtain the single-layer high-entropy structural compound (HEM) A )X 2 ；
3) Mixing HEM B Powder and (HEM) above A )X 2 Uniformly mixing the materials in a mortar to obtain powder, then loading the powder into a quartz tube, carrying out secondary calcination in high-temperature furnace equipment after vacuum sealing, firstly raising the temperature to 500-1200 ℃, keeping the temperature for 1-15 days, then quickly taking out the quartz tube from the high-temperature furnace equipment, putting the quartz tube into a substance such as water or ice-water mixture for quenching treatment, taking out the quenched product from the vacuum quartz tube, and grinding to obtain the multilayer high-entropy structural compound (HEM) B ) x (HEM A )X 2 。
Further, in the step 2), the temperature of the high-temperature furnace is increased to 800-1300 ℃ from 200 minutes to 8 hours.
In the step 3), the temperature is firstly raised to 800 ℃ during the secondary calcination, and the temperature is kept for more than 72 hours.
In step 3), HEM B The raw material is a mechanical mixture of any four or more than four metal simple substance powders or alloyed high-entropy alloy powder.
The invention synthesizes a series of multilayer high-entropy structural compounds (HEM) for the first time B ) x (HEM A )X 2 In this context, at MX 2 HEM (high-entropy metal element combination) with M position of laminated structure A On the basis of replacement, a layer of high-entropy metal atom HEM is introduced between layers B We refer to herein as multi-layer high entropy. It is worth mentioning thatThe invention can regulate and control the intercalation amount to obtain a series of multilayer high-entropy structural compounds, and the series of materials have great potential in the application fields of energy conversion, energy storage and the like.
Drawings
FIG. 1 is (HEM) B ) x (HEM A )X 2 A crystal structure diagram;
FIG. 2 shows (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.25 V 0.25 Ta 0.25 Cr 0.25 )Se 2 The X-ray powder diffraction fine-trimming spectrogram of (1).
FIG. 3 shows (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.25 V 0.25 Ta 0.25 Cr 0.25 )Se 2 EDS spectrum of (3).
FIG. 4 shows (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 Zr 0.2 V 0.2 Nb 0.2 Ta 0.2 )Se 2 The X-ray powder diffraction fine-correction spectrogram.
FIG. 5 shows (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 Zr 0.2 V 0.2 Nb 0.2 Ta 0.2 )Se 2 EDS energy spectrum of (a).
FIG. 6 shows (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 V 0.2 Ta 0.4 Cr 0.2 )Se 2 The X-ray powder diffraction fine-correction spectrogram.
FIG. 7 shows (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 V 0.2 Ta 0.4 Cr 0.2 )Se 2 EDS energy spectrum of (a).
Detailed Description
Example 1
The preparation method of the multilayer high-entropy structural compound comprises the following steps:
(1) ti powder with the purity of 99 percent, cr powder with the purity of 99 percent, V powder with the purity of 99 percent, ta powder with the purity of 99 percent and Se powder with the purity of 99 percent are adopted, the total amount of Ti, V, ta and Cr elements is 1, the Ti, V, ta and Cr elements and the Se powder are weighed according to the proportion of 1:2, and the Ti powder, the Cr powder, the V powder, the Ta powder and the Cr elements and the Se powder are carefully ground in a mortar; then pouring the uniformly mixed sample into a quartz tube, vacuumizing and sealing; sintering the sample: heating to 1100 deg.C from room temperature for 200min, maintaining for 1440 min, taking out quartz tube, quenching in ice-water mixture, taking out product, and grinding to obtain high purity (Ti) 0.25 V 0.25 Ta 0.25 Cr 0.25 )Se 2 And (3) powder.
(2) Adopting FeCoCrNiMn and other high-entropy alloys with the purity of 99 percent to sinter the products (Ti) in the step (1) 0.25 V 0.25 Ta 0.25 Cr 0.25 )Se 2 Carefully grinding in a mortar according to a molar ratio of 0.2:1 to mix the components uniformly, putting the ground mixture into a quartz tube, vacuumizing, sealing, and finally burning: heating to 800 deg.C from room temperature in 200min, maintaining for 4320 min, quenching at 800 deg.C in water, opening the quartz tube, taking out, and grinding to obtain high-purity multilayer high-entropy compound (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.25 V 0.25 Ta 0.25 Cr 0.25 )Se 2 And (3) phase powder.
(3) Taking the chemical formula as (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.25 V 0.25 Ta 0.25 Cr 0.25 )Se 2 The sample of (1) is obtained by X-ray powder diffractometer and its X-ray diffraction spectrum is shown in FIG. 2, and its space group is obtained by crystal structure refinement
Still retains the TiSe 2 Has a symmetrical crystal structure, a phase is a pure phase, and unit cell parameters are
The obtained refinement parameter is R p ＝6.72％，R wp The reliability of the crystal structure is confirmed by 8.70%, and as shown in fig. 3, an EDS energy spectrum of the sample can be observed, the types and proportions of elements contained therein can be observed, and further, the successful preparation of the sample is confirmed.
In summary, high purity (Fe) can be prepared by the method of example 1 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.25 V 0.25 Ta 0.25 Cr 0.25 )Se 2 And (4) phase(s).
Example 2
The preparation method of the multilayer high-entropy structural compound comprises the following steps:
(1) ti powder with the purity of 99%, cr powder with the purity of 99%, V powder with the purity of 99%, nb powder with the purity of 99%, ta powder with the purity of 99%, se powder with the purity of 99%, and Ti, V, nb, cr and Ta elements are weighed according to equal ratio, each element accounts for 0.2, the total amount is 1, and the elements and the Se powder are weighed according to the ratio of 1:2, and are carefully ground in a mortar; then pouring the uniformly mixed sample into a quartz tube, vacuumizing and sealing; and (3) sintering the sample: heating to 1100 deg.C from room temperature for 200min, holding for 1440 min, taking out quartz tube at 1100 deg.C, quenching in ice-water mixture, taking out product, and grinding to obtain high-purity (Ti) 0.2 Zr 0.2 V 0.2 Nb 0.2 Ta 0.2 )Se 2 And (3) powder.
(2) Fe powder with the purity of 99 percent, co powder with the purity of 99 percent, cr powder with the purity of 99 percent, ni powder with the purity of 99 percent and Mn powder with the purity of 99 percent are weighed according to the proportion of 1: 1, are carefully ground in a mortar, and are sintered with the product (Ti) in the step (1) 0.2 Zr 0.2 V 0.2 Nb 0.2 Ta 0.2 )Se 2 According to a molar ratio of 0.2:1 in a mortarCarefully grinding to mix them evenly, putting the ground mixture into a quartz tube, vacuumizing and sealing, and then carrying out final firing: heating to 800 deg.C from room temperature in 200min, maintaining for 4320 min, quenching in water at 800 deg.C, opening vacuum quartz tube, taking out product, and grinding to obtain high-purity multilayer high-entropy compound (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 Zr 0.2 V 0.2 Nb 0.2 Ta 0.2 )Se 2 And (3) phase powder.
(3) Taking the chemical formula as (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 Zr 0.2 V 0.2 Nb 0.2 Ta 0.2 )Se 2 The sample of (1) is obtained by X-ray powder diffractometer and X-ray diffraction spectrogram is collected, as shown in figure 4, object image identification is carried out by the diffraction spectrogram and multiphase refinement is carried out, the obtained phase is pure phase, and the space group is
Refined to obtain a crystal cell with parameters of
The fine modification parameter is R p ＝11.0％，R wp And =15.8%, which illustrates the reliability of the analyzed crystal structure, and as shown in fig. 5, which is an EDS energy spectrum of the sample, the types and proportions of the elements contained therein can be observed, thereby further confirming the successful preparation of the sample.
In summary, high purity (Fe) can be prepared by the method as described in example 2 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 Zr 0.2 V 0.2 Nb 0.2 Ta 0.2 )Se 2 。
Example 3
The preparation method of the multilayer high-entropy structural compound comprises the following steps:
(1) adopts Ti powder with the purity of 99 percent, cr powder with the purity of 99 percent and pureV powder with the degree of 99%, ta powder with the purity of 99%, se powder with the purity of 99%, ti, V, cr and Ta elements are weighed according to the ratio of 1:2, and the total amount of 1 and Se powder are weighed according to the ratio of 1:2, and are carefully ground in a mortar; then pouring the uniformly mixed sample into a quartz tube, vacuumizing and sealing; sintering the sample: heating to 1100 deg.C from room temperature for 200min, holding for 1440 min, taking out quartz tube at 1100 deg.C, quenching in ice-water mixture, taking out product, and grinding to obtain high-purity (Ti) 0.2 Cr 0.2 V 0.2 Ta 0.4 )Se 2 And (3) powder.
(2) Adopting FeCoCrNiMn and other high-entropy alloys with the purity of 99 percent to sinter the products (Ti) in the step (1) 0.2 Cr 0.2 V 0.2 Ta 0.4 )Se 2 Carefully grinding in a mortar according to the molar ratio of 0.2:1 to uniformly mix, putting the ground mixture into a quartz tube, vacuumizing and sealing, and then carrying out final firing: heating to 800 deg.C from room temperature within 200min, maintaining for 4320 min, quenching in water at 800 deg.C, opening vacuum quartz tube, taking out product, and grinding to obtain high-purity multilayer high-entropy structural compound (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 V 0.2 Ta 0.4 Cr 0.2 )Se 2 And (3) phase powder.
(3) The chemical formula is (Fe) 0.2 Co 0.2 Cr 0.2 Ni 0.2 Mn 0.2 ) 0.2 (Ti 0.2 V 0.2 Ta 0.4 Cr 0.2 )Se 2 The sample of (1) is obtained by X-ray powder diffractometer and X-ray diffraction spectrogram is collected, as shown in FIG. 6, object image identification is carried out by the diffraction spectrogram and multiphase refinement is carried out, the obtained phase is pure phase, and the space group is
Refined to obtain the crystal cell parameter of
The fine modification parameter is R p ＝7.18％，R wp And =9.34%, which shows the reliability of the resolved crystal structure, and as the EDS energy spectrum of the sample in fig. 7, the types and proportions of the elements contained therein can be observed, further confirming the successful preparation of the sample.
It should be noted that the above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above examples. It is to be understood that other modifications and variations, which may be directly derived or suggested to one skilled in the art without departing from the basic concept of the invention, are to be considered as included within the scope of the invention.
Claims (5)
1. The preparation method of the multilayer high-entropy structural compound is characterized in that the molecular formula of the multilayer high-entropy structural compound is expressed as (HEM) B ) x (HEM A )X 2 ，HEM A 、HEM B Are respectively two groups of high entropy elements, HEM B Is the combination of any four or more than four metal elements of Fe, co, cr, ni, mn, V, cu, ag and Zn, the element proportion is equal ratio, HEM B The total amount of the elements in (1) is x,0<x≤1，
HEM A Is the combination of any four or more than four metal elements of Ti, zr, hf, V, nb, ta, cr, mo, W, re, os, rh, ir, au, pd and Pt, the element proportion is equal ratio or unequal ratio, and the total element amount is 1;
x is one or the combination of more of S, se and Te elements;
the preparation method comprises the following steps:
1) Mixing HEM A Uniformly mixing the powder and the X element powder according to the proportion of 1;
2) Putting the uniformly mixed powder into a vacuum quartz tube, vacuumizing the quartz tube, sealing, sintering in a high-temperature furnace at 800-1300 ℃, preserving heat for 20-36h, taking out the quartz tube from the furnace, and quenching to obtain the single-layer high-entropy structural compound (HEM) A )X 2 ；
3) Mixing HEM B Powder and (HEM) above A )X 2 Uniformly mixing in a mortar to obtain powder, then loading the powder into a quartz tube, carrying out secondary calcination in high-temperature furnace equipment after vacuum sealing, raising the temperature to 500-1200 ℃, keeping the temperature for 1-15 days, taking out the quartz tube from the high-temperature furnace equipment, and quenching to obtain the multilayer high-entropy structural compound (HEM) B ) x (HEM A )X 2 。
2. A process for preparing a multilayer compound with a high entropy structure according to claim 1, wherein in step 2), the time for heating the furnace to 800-1300 ℃ is 200min-8h.
3. A method for the preparation of a multilayer high entropy structured compound according to claim 1, characterized in that the quenching treatment in step 2) and step 3) is a treatment in which the quartz tube is placed in water or an ice water mixture.
4. Method for the preparation of a multilayer compound with a high entropy structure according to claim 1, characterized in that in step 3), HEM B The raw material is a mechanical mixture of any four or more than four metal simple substance powders or alloyed high-entropy alloy powder.
5. A process for the preparation of a compound with a multilayer high entropy structure according to claim 1, characterized in that in step 3), the temperature is raised to 800 ℃ during the second calcination and is kept for more than 72 h.
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