CN116040640B - Method for synthesizing MAB phase ceramic powder - Google Patents
Method for synthesizing MAB phase ceramic powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 81
- 239000000919 ceramic Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 49
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 238000000498 ball milling Methods 0.000 claims description 24
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 35
- 238000002360 preparation method Methods 0.000 abstract description 12
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 11
- 239000011572 manganese Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000004880 explosion Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000001272 pressureless sintering Methods 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000002490 spark plasma sintering Methods 0.000 description 3
- 229910016459 AlB2 Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
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- 238000004321 preservation Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910016756 Mn3 Si Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/14—Compounds containing boron and nitrogen, phosphorus, sulfur, selenium or tellurium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/76—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by a space-group or by other symmetry indications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
A method for synthesizing MAB phase ceramic powder relates to a method for synthesizing ceramic powder. The preparation method aims to solve the problems of low efficiency, high energy consumption, complex process and high cost of the existing preparation method of the MAB phase powder material. The method comprises the following steps: weighing M element powder, A element powder and boron powder as raw materials according to the general formula of MAB phase ceramic, and uniformly mixing the raw materials to obtain raw material powder; the raw material powder is filled into a graphite boat, the graphite boat is placed into a closed pressure container, inert gas is introduced, finally, the raw material powder is ignited to cause self-propagating reaction to occur, loose MAB phase ceramic is obtained, and after cooling, the powder is crushed, sieved and dried in sequence. In combination with the analysis, the invention adopts the excellent performance of self-propagating high-temperature synthetic MAB phase material, has the outstanding advantages of simple production process, short time, low energy consumption, low cost and the like, and has wide application prospect.
Description
Technical Field
The invention belongs to the field of ceramic material preparation, and particularly relates to a method for synthesizing MAB phase ceramic powder.
Background
Ternary transition metal borides (abbreviated as MAB phase, M is a transition group metal element, A is a main group element, and B is boron) have a layered structure similar to that of MAX phase materials, and are also considered to be a very promising class of ultra-high temperature ceramic materials (UHTCs). They have the characteristics of good electrical conductivity, thermal conductivity, processability, low thermal expansion coefficient, large compressive strength, high fracture toughness and the like. For example, the 111-type orthorhombic MAB phase MoAlB has been demonstrated to be stable in an inert atmosphere at temperatures up to 1400 ℃. Unlike the corresponding binary boride MoB, the double layer Al atoms in MoAlB are "sandwiched" between the MoB layers, which gives MoAlB excellent oxidation resistance at high temperatures (by forming a dense alumina layer on the surface). The 212 type MAB phases Fe 2AlB2 and Mn 2AlB2 are found to be promising magnetic refrigeration materials because their ferromagnetic-paramagnetic transition temperature (also known as Curie temperature Tc) is near room temperature and the raw materials are low in cost, which is a research hotspot in the current MAB phase field.
Although the MAB phase material has good application prospect and potential, the research on the MAB phase powder synthesis technology has great defects. At present, ternary lamellar compound MAB phase powder is mainly prepared by pressureless sintering, a thermal explosion method or block sintering, and then crushing and grinding. Kota and Li Shibo et al successfully prepared MAB phase single-phase bulk ceramics by hot pressing and spark plasma sintering processes in 2016 and 2019 respectively, and the preparation process has the defects of high preparation temperature (> 1200 ℃) and long reaction time (> 15 minutes); long-time continuous heating is required in the preparation process, and a large amount of electric energy is consumed; the process is complex and requires a vacuum environment or argon protection to prevent oxidation. The powder prepared by traditional pressureless sintering is prepared by synthesizing cold-pressed elemental powder or intermediate products through solid-state reaction and then carrying out subsequent crushing and grinding, and the reaction time is long; the process flow is complex and the production efficiency is low; high cost and high power consumption. The thermal explosion method can only be used for small-batch preparation, and has the advantages of higher cost and higher electric energy consumption. These disadvantages greatly limit the popularization and application of ceramic powder materials, and are difficult to industrialize and industrialize.
Disclosure of Invention
The invention provides a method for synthesizing MAB phase ceramic powder, which aims to solve the problems of low efficiency, high energy consumption, complex process and high cost of the existing preparation method of MAB phase powder materials.
The method for synthesizing the MAB phase ceramic powder comprises the following steps:
Weighing M element powder, A element powder and boron powder as raw materials according to the general formula of MAB phase ceramic, and uniformly mixing the raw materials to obtain raw material powder; filling raw material powder into a graphite boat, putting the graphite boat into a closed pressure container, introducing inert gas, and adjusting the gas pressure in the closed pressure container to 0.01-5 MPa; finally, ignition is carried out to lead the raw material powder to have self-propagating reaction, thus obtaining loose MAB phase ceramic, and the preparation method is completed after cooling, grinding, sieving and drying in sequence.
ThesynthesizedMABphaseceramicpowderconsistsofapolycrystallineMABphase,isinanorthorhombic,tetragonal,hexagonalandothercrystalsystem,hasaspacegroupofCmcm,Cmmm,PM2,I4/mcm,P63/mmcandthelike,andisformedbyalternatelyarrangingandcombiningA-AorM-AweakbondsandM-BorB-Bstrongbondsinacrystalstructure,sothattheshearingdamageoftheMABphaseiseasytooccurinanAlayer,therebyenablingcrystalgrainstobeeasytogeneratekinkingandspalling,andmacroscopicallyenhancingthefracturetoughnessoftheMABphase.
The principle and beneficial effects of the invention are as follows:
1. the invention can prepare the low-cost and high-purity MAB phase ceramic powder by taking the low-cost elemental element powder and the boron powder as raw materials, does not need long-time heat preservation, has short synthesis time, can save a large amount of energy sources, reduces energy consumption, has high production efficiency and has low process cost, and the main process is completed within a few minutes. The invention has simple process equipment, small occupied area and convenient maintenance.
2. Compared with the MAB phase powder synthesized by pressureless sintering, thermal explosion method, hot-pressed sintering and spark plasma sintering, the invention has the main advantages that the method adopts the mature self-propagating high-temperature synthesis technology in the aspect of ternary ceramic synthesis, only needs extremely short reaction time, and greatly improves the production efficiency. The proper granularity of the raw materials can effectively improve the adiabatic temperature of the product, so that the possibility of the product in a self-propagating mode is improved to a certain extent, and the purity of the product is improved; and the powder material with high purity can be synthesized in a self-propagating mode without heat input, which is beneficial to practical engineering application.
3. The MAB phase material prepared by the method has the excellent performances of a metal material and a ceramic material, the preparation method has universality, and the raw material source is wide, so that the method has potential application prospects in the fields of high-temperature resistant and radiation resistant devices, magnetic refrigeration candidate materials and the like.
In combination with the analysis, the invention adopts the excellent performance of the MAB phase material synthesized at high temperature by self-propagating, has the outstanding advantages of simple production process, short time, low energy consumption, low cost and the like, and has wide application prospect.
Drawings
FIG. 1 is an XRD pattern of MAB phase material MoAlB in example 1;
FIG. 2 is an SEM image (30 μm) of MAB phase material MoAlB of example 1;
FIG. 3 is an SEM image (5 μm) of MAB phase material MoAlB of example 1;
FIG. 4 is an SEM image (10 μm) of MAB phase material MoAlB of example 1;
FIG. 5 is an XRD pattern for MAB phase material V 3PB4 in example 2;
FIG. 6 is an XRD pattern for MAB phase material Mn 5SiB2 in example 3;
FIG. 7 is an XRD pattern of the MAB phase material Nb 2 SB in example 4.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and also comprises any reasonable combination of the specific embodiments.
The first embodiment is as follows: the method for synthesizing MAB phase ceramic powder according to the present embodiment is carried out according to the following steps:
Weighing M element powder, A element powder and boron powder as raw materials according to the general formula of MAB phase ceramic, and uniformly mixing the raw materials to obtain raw material powder; filling raw material powder into a graphite boat, putting the graphite boat into a closed pressure container, introducing inert gas, and adjusting the gas pressure in the closed pressure container to 0.01-5 MPa; finally, ignition is carried out to lead the raw material powder to have self-propagating reaction, thus obtaining loose MAB phase ceramic, and the preparation method is completed after cooling, grinding, sieving and drying in sequence.
TheMABphaseceramicpowdersynthesizedbytheembodimentiscomposedofapolycrystallineMABphase,isinanorthorhombic,tetragonalandhexagonalcrystalsystem,hasaspacegroupofCmcm,Cmmm,PM2,I4/mcm,P63/mmcandthelike,andisformedbyalternatelyarrangingandcombiningA-AorM-AweakbondsandM-BorB-Bstrongbondsinacrystalstructure,sothattheshearingdamageoftheMABphaseiseasytooccurinanAlayer,therebyenablingcrystalgrainstobeeasytogeneratekinkingandspalling,andmacroscopicallyenhancingthefracturetoughnessoftheMABphase.
The principle and beneficial effects of the embodiment are as follows:
1. The method can prepare the low-cost and high-purity MAB phase ceramic powder by taking the low-cost elemental element powder and the boron powder as raw materials, does not need long-time heat preservation time, has short synthesis time, can save a large amount of energy sources, reduces energy consumption, has high production efficiency and has low process cost, and the main process is completed within a few minutes. In addition, the technical equipment of the embodiment is simple, the occupied area is small, and the maintenance is convenient.
2. Compared with the MAB phase powder synthesized by pressureless sintering, thermal explosion method, hot-pressed sintering and spark plasma sintering, the method has the main advantages that the method adopts the mature self-propagating high-temperature synthesis technology in the aspect of ternary ceramic synthesis, only needs extremely short reaction time, and greatly improves the production efficiency. The proper granularity of the raw materials can effectively improve the adiabatic temperature of the product, so that the possibility of the product in a self-propagating mode is improved to a certain extent, and the purity of the product is improved; and the powder material with high purity can be synthesized in a self-propagating mode without heat input, which is beneficial to practical engineering application.
3. The MAB phase material prepared by the embodiment has the excellent performances of a metal material and a ceramic material, the preparation method has universality, and the raw material source is wide, so that the MAB phase material has potential application prospects in the fields of high-temperature resistant and radiation-resistant devices, magnetic refrigeration candidate materials and the like.
In combination with the analysis, the method adopts the excellent performance of the MAB phase material synthesized at high temperature by self-propagating, has the outstanding advantages of simple production process, short time, low energy consumption, low cost and the like, and has wide application prospect.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the raw materials are mixed in a ball milling mode, ball milling balls are steel balls, a ball milling tank is a resin tank, and ball milling is carried out for 24-48 hours.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: the ignition adopts a single Ni-Cr alloy wire, and the ignition agent is titanium powder and carbon black or titanium powder and boron powder; the mol ratio of the titanium powder to the carbon black is 1:1, and the mol ratio of the titanium powder to the boron powder is 1:1; the amount of the ignition agent is 1-5g. The material can continuously spread and burn under the condition of no need of external heat source after ignition of the ignition agent until the reaction to obtain the product with the required composition and structure.
The specific embodiment IV is as follows: this embodiment differs from one of the first to third embodiments in that: the particle size of the M element powder, the A element powder and the boron powder is 500-50 mu M.
Fifth embodiment: this embodiment differs from one to four embodiments in that: the inert gas is Ar gas.
Specific embodiment six: this embodiment differs from one of the first to fifth embodiments in that: the general formula of the MAB phase ceramic is M xAyBz, x=1-5, y=1-3, and z=1-6.
Seventh embodiment: the sixth embodiment differs from the first embodiment in that: m is any one or more of Sc, Y, ti, zr, V, W, fe, ru, co, ni, cr, zr, nb, mo, hf, ta, mn.
Eighth embodiment: the sixth embodiment differs from the first embodiment in that: the A is any one or more of Al, ga, in, tl, si, ge, sn, pb, P, as, sb, bi, S, se, te.
Detailed description nine: the sixth embodiment differs from the first embodiment in that: and B is boron.
Detailed description ten: this embodiment differs from one of the embodiments one to nine in that: the MAB phase ceramic is MoAlB phase ceramic.
Example 1:
the MAB phase ceramic prepared in this example is MoAlB phase ceramic, and is 111-type orthorhombic system. The method for synthesizing MAB phase ceramic powder in this example is carried out according to the following steps:
Weighing molybdenum powder (99%, 1000 meshes), aluminum powder (99.99%, 300 meshes) and boron powder (99.95%, 2000 meshes) according to the general formula of MAB phase ceramic; uniformly mixing the raw materials to obtain raw material powder; the raw materials are mixed in a ball milling mode, ball milling balls are steel balls, a ball milling tank is a resin tank, and ball milling is carried out for 24 hours. Filling raw material powder into a graphite boat, putting the graphite boat into a closed pressure container, introducing Ar gas, and adjusting the gas pressure in the closed pressure container to 5MPa; finally, ignition is carried out to lead the raw material powder to carry out self-propagating reaction to obtain loose MAB phase ceramic, and the MAB phase ceramic is obtained after cooling, crushing, sieving with a 200-mesh sieve and drying are carried out in sequence; the ignition adopts a single Ni-Cr alloy wire, the ignition agent is titanium powder and carbon black, the molar ratio of the titanium powder to the carbon black is 1:1, and the consumption of the ignition agent is 2g.
FIG. 1 is an XRD pattern of MAB phase material MoAlB in example 1; in fig. 1, it can be seen that the obtained product is an orthorhombic MAB phase with 111 configuration and part of impurity phases MoB and Al 8Mo3, and the characteristic peaks of the synthesized MoAlB powder material and the characteristic peaks of the MoAlB crystal predicted by theory are well matched, which indicates that MoAlB powder is successfully prepared.
FIG. 2 is an SEM image (30 μm) of MAB phase material MoAlB of example 1; FIG. 3 is an SEM image (5 μm) of MAB phase material MoAlB of example 1; FIG. 4 is an SEM image (10 μm) of MAB phase material MoAlB of example 1; it can be seen in fig. 2-4 that the resultant MoAlB powder exhibited a distinct long-strip shape and was prone to agglomeration.
Example 2:
the MAB phase ceramic prepared in this example is V 3PB4 phase ceramic, which is a hexagonal system of 314 configuration. The method for synthesizing MAB phase ceramic powder in this example is carried out according to the following steps:
Weighing vanadium powder (99%, 200 mesh), red phosphorus powder (98.5%, 30 mesh) and boron powder (99.95%, 325 mesh) according to the general formula of MAB phase ceramic; uniformly mixing the raw materials to obtain raw material powder; the raw materials are mixed in a ball milling mode, ball milling balls are steel balls, a ball milling tank is a resin tank, and ball milling is carried out for 24 hours. Filling raw material powder into a graphite boat, putting the graphite boat into a closed pressure container, introducing Ar gas, and adjusting the gas pressure in the closed pressure container to 5MPa; finally, ignition is carried out to lead the raw material powder to carry out self-propagating reaction to obtain loose MAB phase ceramic, and the MAB phase ceramic is obtained after cooling, crushing, sieving with a 200-mesh sieve and drying are carried out in sequence; the ignition adopts a single Ni-Cr alloy wire, the ignition agent is titanium powder and boron powder, and the molar ratio of the titanium powder to the boron powder is 1:1; the amount of the ignition agent is 2g.
FIG. 5 is an XRD pattern for MAB phase material V 3PB4 in example 2; as can be seen in the XRD diagram, the obtained product is a hexagonal MAB phase with 314 configuration and part of impurity phase V 2B3, and the characteristic peaks of the synthesized V 3PB4 powder material and the characteristic peaks of the theoretical predicted V 3PB4 crystal are well matched, which shows that the V 3PB4 powder is successfully prepared.
Example 3:
the MAB phase ceramic prepared in the embodiment is Mn 5SiB2 phase ceramic and is a 512-configuration tetragonal crystal form. The method for synthesizing MAB phase ceramic powder in this example is carried out according to the following steps:
weighing manganese powder (99.5%, 300 mesh), silicon powder (99.99%, 2000 mesh) and boron powder (99.95%, 2000 mesh) according to the general formula of MAB phase ceramic; uniformly mixing the raw materials to obtain raw material powder; the raw materials are mixed in a ball milling mode, ball milling balls are steel balls, a ball milling tank is a resin tank, and ball milling is carried out for 24 hours. Filling raw material powder into a graphite boat, putting the graphite boat into a closed pressure container, introducing Ar gas, and adjusting the gas pressure in the closed pressure container to 5MPa; finally, ignition is carried out to lead the raw material powder to carry out self-propagating reaction to obtain loose MAB phase ceramic, and the MAB phase ceramic is obtained after cooling, crushing, sieving with a 200-mesh sieve and drying are carried out in sequence; the ignition adopts a single Ni-Cr alloy wire, the ignition agent is titanium powder and boron powder, and the molar ratio of the titanium powder to the boron powder is 1:1; the amount of the ignition agent is 2g.
FIG. 6 is an XRD pattern for MAB phase material Mn 5SiB2 in example 3; as can be seen in FIG. 6, the obtained product is a tetragonal MAB phase Mn 5SiB2 with 512 configuration and a part of impurity phase Mn 3B4、Mn3 Si, and the characteristic peaks of the synthesized Mn 5SiB2 powder material are well matched with the characteristic peaks of Mn 5SiB2 crystals predicted by theory, which indicates that Mn 5SiB2 powder is successfully prepared.
Example 4:
The MAB phase ceramic prepared in the embodiment is Nb 2 SB phase ceramic and is in a hexagonal crystal form with 211 configuration. The method for synthesizing MAB phase ceramic powder in this example is carried out according to the following steps:
Weighing niobium powder (99.9%, 200 mesh), sulfur powder (99.99%, 30 mesh) and boron powder (99.95%, 2000 mesh) according to the general formula of MAB phase ceramic; uniformly mixing the raw materials to obtain raw material powder; the raw materials are mixed in a ball milling mode, ball milling balls are steel balls, a ball milling tank is a resin tank, and ball milling is carried out for 24 hours. Filling raw material powder into a graphite boat, putting the graphite boat into a closed pressure container, introducing Ar gas, and adjusting the gas pressure in the closed pressure container to 5MPa; finally, ignition is carried out to lead the raw material powder to carry out self-propagating reaction to obtain loose MAB phase ceramic, and the MAB phase ceramic is obtained after cooling, crushing, sieving with a 200-mesh sieve and drying are carried out in sequence; the ignition adopts a single Ni-Cr alloy wire, the ignition agent is titanium powder and boron powder, and the molar ratio of the titanium powder to the boron powder is 1:1; the amount of the ignition agent is 2g.
FIG. 7 is an XRD pattern of the MAB phase material Nb 2 SB of example 4; fig. 7 shows that the obtained product is higher-purity hexagonal MAB phase Nb 2 SB with 211 configuration and partial impurity phases NbS and NbB, and the characteristic peaks of the synthesized Nb 2 SB powder material are well matched with the characteristic peaks of the theoretical predicted Nb 2 SB crystal, which shows that the Nb 2 SB powder is successfully prepared.
Claims (6)
1. A method of synthesizing a MAB phase ceramic powder, characterized by: the method for synthesizing the MAB phase ceramic powder comprises the following steps:
Weighing M element powder, A element powder and boron powder as raw materials according to the general formula of MAB phase ceramic, and uniformly mixing the raw materials to obtain raw material powder; filling raw material powder into a graphite boat, putting the graphite boat into a closed pressure container, introducing inert gas, and adjusting the gas pressure in the closed pressure container to 0.01-5 MPa; finally, ignition is carried out to lead the raw material powder to have self-propagating reaction to obtain loose MAB phase ceramic, and the MAB phase ceramic is obtained after cooling, grinding, sieving and drying are sequentially carried out;
The ignition adopts a single Ni-Cr alloy wire, and the ignition agent is titanium powder and carbon black or titanium powder and boron powder; the mol ratio of the titanium powder to the carbon black is 1:1, and the mol ratio of the titanium powder to the boron powder is 1:1; the consumption of the ignition agent is 1-5g;
m is any one or more of Sc, Y, ti, zr, V, W, fe, ru, co, ni, cr, zr, nb, mo, hf, ta, mn;
the A is any one or more of Al, ga, in, tl, si, ge, sn, pb, P, as, sb, bi, S, se, te;
And B is boron.
2. The method of synthesizing a MAB phase ceramic powder of claim 1 characterized in that: the raw materials are mixed in a ball milling mode, ball milling balls are steel balls, a ball milling tank is a resin tank, and ball milling is carried out for 24-48 hours.
3. The method of synthesizing a MAB phase ceramic powder of claim 1 characterized in that: the particle sizes of the M element powder, the A element powder and the boron powder are 500 nm-50 mu M.
4. The method of synthesizing a MAB phase ceramic powder of claim 1 characterized in that: the inert gas is Ar gas.
5. The method of synthesizing a MAB phase ceramic powder of claim 1 characterized in that: the general formula of the MAB phase ceramic is M xAyBz, x=1-5, y=1-3, and z=1-6.
6. The method of synthesizing a MAB phase ceramic powder of claim 1 characterized in that: the MAB phase ceramic is MoAlB phase ceramic.
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