CN106892663A - A kind of sheet powder metallurgy and preparation method thereof - Google Patents
A kind of sheet powder metallurgy and preparation method thereof Download PDFInfo
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- CN106892663A CN106892663A CN201710045432.8A CN201710045432A CN106892663A CN 106892663 A CN106892663 A CN 106892663A CN 201710045432 A CN201710045432 A CN 201710045432A CN 106892663 A CN106892663 A CN 106892663A
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- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 62
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000010276 construction Methods 0.000 claims abstract description 5
- 239000002159 nanocrystal Substances 0.000 claims abstract description 5
- 239000000919 ceramic Substances 0.000 claims description 28
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 claims description 15
- 239000010410 layer Substances 0.000 claims description 14
- 150000004767 nitrides Chemical class 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 241000446313 Lamella Species 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 5
- 229910052723 transition metal Inorganic materials 0.000 claims description 5
- 238000003475 lamination Methods 0.000 claims description 4
- 239000010955 niobium Substances 0.000 claims description 4
- 239000011241 protective layer Substances 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 2
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 3
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- -1 vanadium carbide nitride Chemical class 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/58007—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3839—Refractory metal carbides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
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Abstract
The invention discloses a kind of sheet powder metallurgy and preparation method thereof, the powder metallurgy is made up of multi-layer nano crystal grain, with laminated construction；Preparation process is as follows：（1）By XnAl C phase dusty materials corrode in being put into the hydrofluoric acid that mass concentration is 47%, corrode 20 40 hours under the conditions of 40 60 DEG C, obtain the carbide particle of sheet；（2）By step（1）In the carbide particle that obtains carry out cleaning until cleaning solution pH value is up to 7, be then dried；（3）By step（2）In the carbide particle that obtains be put into the nitrogen of flowing, isothermal holding 14 hours under the conditions of 900 1300 DEG C obtain target product after cooling；Powder metallurgy prepared by the present invention has lamellar structure, can introduce matrix material in piece lamellar spacing, plays a part of reinforcing and agrees with improving performance, preparation process is simple, low production cost.
Description
Technical field
The present invention relates to powder metallurgy and preparation method thereof, and in particular to a kind of lamellar structure of nanocrystalline composition
Powder metallurgy and preparation method thereof.
Background technology
There is magnesium-yttrium-transition metal nitride ceramics good heat endurance, high rigidity, high-modulus and good electricity can process
Property, it is widely available in the industry；Such as vanadium nitride as cubic boron nitride mould additive, niobium nitride as hard close
Golden additive, can greatly promote the service life of instrument；In addition, nitride electrode can be as the electrode material of ultracapacitor
Material, with extraordinary chemical stability；Commercial nitride particles are usually the full particle of irregular shape, in use
Strengthening and toughening is played a part of in mode disperse using mixing in the base, but effect is bad.
The content of the invention
The invention discloses it is a kind of by it is nanocrystalline constitute with laminar structured powder metallurgy and its preparation
Method.
The technical solution adopted by the present invention is：The powder metallurgy is made up of multi-layer nano crystal grain, with lamination
Structure, the laminated construction number of plies is 10-100 layers, between layers with piece lamellar spacing, residual adhesion and shape between layers
Into a powder metallurgy.Each lamella of the lamination is a nitride ceramics crystal grain for sheet, described
The lamellar spacing of layered nitride thing ceramic crystalline grain is 10-100nm.
Further, the nitride ceramics is magnesium-yttrium-transition metal nitride ceramics, specially in niobium nitride or vanadium nitride
One kind.
A kind of preparation method of sheet powder metallurgy, comprises the following steps：
(1) by Xn- Al-C phase dusty materials corrode in being put into the hydrofluoric acid that mass concentration is 47%, in 40-60 DEG C of condition
Lower corrosion 20-40 hours, obtains the carbide particle of sheet；
(2) carbide particle obtained in step (1) is carried out into cleaning up to cleaning solution pH value is up to 7, is then dried；
(3) carbide particle obtained in step (2) is put into the nitrogen of flowing, under the conditions of 900-1300 DEG C at insulation
Reason 1-4 hours, obtains target product after cooling.
Further, X is magnesium-yttrium-transition metal in the step (1), and n is 2.
Further, X is Nb or V, i.e. Nb in the step (1)2AlC or V2AlC, for prepare lamellar structure niobium nitride or
The raw material of vanadium nitride ceramic particle.
Further, dried 24 hours under the conditions of 20-60 DEG C in the step (2).
Further, it is described from step (2) to step (3) during carbide particle surface set protective layer, set
Protective layer can make not to be contaminated in material transfer process.
Further, the protective layer includes the graphite paper being arranged on carbide particle surface and is arranged on graphite paper
Graphite powder；Graphite-structure stabilization, it is not easy to react.
Further, the programming rate of nitrogen treatment is 1-30 DEG C/min, X in the step (3)n- Al-C phase ceramics are led
It is hot very well, under the limit ramp rate conditions of 30 DEG C/min also can uniformly transfer heat, therefore be adapted to industrialized production, can be significantly
The time-consuming and energy.
Further, oil bath heating is used in the step (1) in corrosion process, using oil bath heating temperature can be made steady
It is fixed, heat more uniform.
The beneficial effects of the invention are as follows：
(1) powder metallurgy of the invention has lamellar structure, can introduce matrix material in piece lamellar spacing, rises
Agree with the effect of improving performance to reinforcing；
(2) powder metallurgy lamella of the invention is made up of nanocrystalline, can prepare the nanometer of function admirable
Composite is used as electrode；
(3) preparation process of the present invention does not need special process meanses, and process is simple is prepared conveniently, is easy to industrial metaplasia
Produce.
Brief description of the drawings
Fig. 1 is the sheet vanadium carbide presoma scanning electron microscope (SEM) photograph in embodiment 1.
Fig. 2 is the sheet niobium carbide presoma scanning electron microscope (SEM) photograph in embodiment 3.
Fig. 3 is sheet vanadium nitride particles scanning electron microscope (SEM) photograph in embodiment 1.
Fig. 4 is sheet niobium nitride particulate scan electron microscope in embodiment 3.
Curve a is the X ray diffracting spectrum of vanadium nitride particles in embodiment 1 in Fig. 5, and curve b is niobium nitride in embodiment 3
The X ray diffracting spectrum of particle.
Specific embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Sheet vanadium nitride particles are prepared as steps described below
(1) by 2gV2AlC dusty materials corrode in being put into the hydrofluoric acid that 50ml mass concentrations are 47%, under the conditions of 60 DEG C
Corrode 20 hours in oil bath, obtain the carbide particle of sheet；
(2) carbide particle obtained in step (1) is cleaned up to cleaning solution pH value up to 7, Ran Hou with deionized water
Dried 24 hours under the conditions of 60 DEG C in vacuum drying chamber；
(3) carbide particle that will be obtained in step (2), is fitted into alumina crucible, and graphite paper is covered in particle surface,
Lid last layer graphite powder again；Crucible is put into stove and is processed 1 hour in the high-purity nitrogen (99.9%) of flowing；1300 DEG C of bars
Isothermal holding 1 hour under part, obtains target product after furnace cooling, heating rate is 1 DEG C/min.
The sheet vanadium nitride ceramic particle for obtaining, the thickness of lamella is 20 nanometers；Fig. 1 is the piece obtained in step (2)
The scanning electron microscope (SEM) photograph of shape vanadium carbide ceramic particle presoma, as can be seen from the figure the typical multi-layer sheet structure of presoma is follow-up heat
Treatment provides extraordinary template, it is ensured that prepare the nitride with same lamellar structure；Fig. 3 is the synusia for obtaining
Shape vanadium nitride ceramic particle, as can be seen from the figure its have uniqueness laminated construction, each lamella is by nanocrystal
Vanadium nitride particles are constituted；Table 1 is the elemental composition of the ceramic particle obtained through X-ray energy spectrum analysis, is found in vanadium nitride particles
In there is nitrogen, oxygen and carbon, also a small amount of aluminium element and micro fluorine element, this is probably due in processing procedure
There is small amounts aluminium to generate, and the nitride for being obtained is doped with a small amount of carbon, forms the compound of vanadium carbide nitride；In Fig. 5
Shown in curve a, all of diffraction maximum is all very sharp, illustrates that the crystallinity of crystal grain is very good, prepared sheet vanadium nitride
The defect of ceramic particle is little.
The X-ray energy spectrum constituent content analysis table of the vanadium nitride particles of table 1.
Embodiment 2
Sheet vanadium nitride particles are prepared as steps described below
(1) by 5gV2AlC dusty materials corrode in being put into the hydrofluoric acid that 100ml mass concentrations are 47%, in 40 DEG C of conditions
Corrode 20 hours in lower oil bath, obtain the carbide particle of sheet；
(2) carbide particle obtained in step (1) is cleaned up to cleaning solution pH value up to 7, Ran Hou with deionized water
Dried 24 hours under the conditions of 20 DEG C in vacuum drying chamber；
(3) carbide particle that will be obtained in step (2), is fitted into alumina crucible, and graphite paper is covered in particle surface,
Lid last layer graphite powder again；Crucible is put into stove and is processed 4 hours in the high-purity nitrogen (99.9%) of flowing；900 DEG C of bars
Isothermal holding 1 hour under part, obtains target product after furnace cooling, heating rate is 30 DEG C/min.
The sheet vanadium nitride ceramic particle for obtaining, the thickness of lamella is 14.8 nanometers.
Embodiment 3
Sheet niobium nitride particle is prepared as steps described below
(1) by 5gNb2AlC dusty materials corrode in being put into the hydrofluoric acid that 200ml mass concentrations are 47%, in 50 DEG C of conditions
Corrode 30 hours in lower oil bath, obtain the carbide particle of sheet；
(2) carbide particle obtained in step (1) is cleaned up to cleaning solution pH value up to 7, Ran Hou with deionized water
Dried 24 hours under the conditions of 40 DEG C in vacuum drying chamber；
(3) carbide particle that will be obtained in step (2), is fitted into alumina crucible, and graphite paper is covered in particle surface,
Lid last layer graphite powder again；Crucible is put into stove and is processed 3 hours in the high-purity nitrogen (99.9%) of flowing；1100 DEG C of bars
Isothermal holding 3 hours under part, obtain target product after furnace cooling, heating rate is 20 DEG C/min.
The sheet niobium nitride ceramic particle for obtaining, the thickness of lamella is 100 nanometers.
Fig. 2 is the scanning electron microscope (SEM) photograph of sheet niobium carbide ceramic particle presoma obtained in step (2), can from figure
Go out the typical multi-layer sheet structure of presoma for follow-up heat treatment provides extraordinary template, it is ensured that prepare with same print
The nitride of Rotating fields；Fig. 4 is the lamellar niobium nitride ceramic particle for obtaining, and as can be seen from the figure it has the lamination of uniqueness
Structure, each lamella is made up of the vanadium nitride particles of nanocrystal；Table 1 is the ceramics obtained through X-ray energy spectrum analysis
There is nitrogen, oxygen and carbon, also a small amount of aluminium element and micro fluorine in niobium nitride particle in the elemental composition of grain, discovery
Element, this be probably due to have in processing procedure small amounts aluminium generate, and the nitride for being obtained be doped with it is a small amount of
Carbon, forms the compound of vanadium carbide nitride；Shown in curve b in Fig. 5, all of diffraction maximum is all very sharp, illustrates the crystallization of crystal grain
Property is very good, and the defect of prepared sheet niobium nitride ceramic particle is little.
The X-ray energy spectrum constituent content analysis table of the niobium nitride particle of table 2.
Embodiment 4
Sheet vanadium nitride particles are prepared as steps described below
(1) by 2gNb2AlC dusty materials corrode in being put into the hydrofluoric acid that 30ml mass concentrations are 47%, in 40 DEG C of conditions
Corrode 40 hours in lower oil bath, obtain the carbide particle of sheet；
(2) carbide particle obtained in step (1) is cleaned up to cleaning solution pH value up to 7, Ran Hou with deionized water
Dried 24 hours under the conditions of 20 DEG C in vacuum drying chamber；
(3) carbide particle that will be obtained in step (2), is fitted into alumina crucible, and graphite paper is covered in particle surface,
Lid last layer graphite powder again；Crucible is put into stove and is processed 2 hours in the high-purity nitrogen (99.9%) of flowing；1000 DEG C of bars
Isothermal holding 2 hours under part, obtain target product after furnace cooling, heating rate is 10 DEG C/min.
The sheet niobium nitride ceramic particle for obtaining, the thickness of lamella is 88.4 nanometers.
The sheet vanadium nitride and niobium nitride ceramic particle prepared using the present invention, unique structure, with current commercial reality
Heart ceramic particle has obvious difference；For example：Nitrogenized using presoma in (J.Alloys Compd., 464,75-80 (2008))
Method prepares vanadium nitride nano particle, and crystallite dimension is about 50 nanometers, is the nano particle set reunited；(J.Alloys
Compd., 389,296-8 (2005)) in synthesize size for 10-20 nanometers of ceramic particle using hydro-thermal method, be nano particle
Aggregate；The present invention to corrode the sheet vanadium carbide and niobium carbide ceramic particle of preparation as presoma, by simple
After high-temperature ammonolysis PROCESS FOR TREATMENT, nitridation in situ obtains the brilliant flaky pottery particle for constituting of nitride nano；The sheet nitrogen of preparation
Changing vanadium and niobium nitride ceramic particle has special microstructure, can be as matrix enhancing phase and the electrode material of ultracapacitor
Material, structural manufacturing process is simple, low production cost.
Claims (10)
1. a kind of sheet powder metallurgy, it is characterised in that：The powder metallurgy is by multi-layer nano crystal grain group
Into with laminated construction, the laminated construction number of plies is 10-100 layers, between layers with piece lamellar spacing, between layers
Residual adhesion and form a powder metallurgy；Each lamella of the lamination is a nitride ceramics for sheet
Crystal grain, the lamellar spacing of the sheet nitride ceramics crystal grain is 10-100nm.
2. a kind of sheet powder metallurgy according to claim 1, it is characterised in that：The nitride ceramics is
One kind in magnesium-yttrium-transition metal nitride ceramics, specially vanadium nitride or niobium nitride.
3. a kind of preparation method of sheet powder metallurgy as claimed in claim 1, it is characterised in that including following
Step：
(1) by Xn- Al-C phase dusty materials corrode in being put into the hydrofluoric acid that mass concentration is 47%, corrode under the conditions of 40-60 DEG C
20-40 hours, obtain the carbide particle of sheet；
(2) carbide particle obtained in step (1) is carried out into cleaning up to cleaning solution pH value is up to 7, is then dried；
(3) carbide particle obtained in step (2) is put into the nitrogen of flowing, isothermal holding 1- under the conditions of 900-1300 DEG C
4 hours, target product is obtained after cooling.
4. a kind of preparation method of sheet powder metallurgy according to claim 3, it is characterised in that the step
Suddenly X is magnesium-yttrium-transition metal in (1), and n is 2.
5. a kind of preparation method of sheet powder metallurgy according to claim 3, it is characterised in that the step
Suddenly X is the one kind in Nb or V, i.e. Nb in (1)2AlC or V2AlC。
6. a kind of preparation method of sheet powder metallurgy according to claim 3, it is characterised in that the step
Suddenly dried 24 hours under the conditions of 20-60 DEG C in (2).
7. the preparation method of a kind of sheet powder metallurgy according to claim 3, it is characterised in that：It is described from
Step (2) sets protective layer to during step (3) on carbide particle surface.
8. the preparation method of a kind of sheet powder metallurgy according to claim 3, it is characterised in that：The guarantor
Sheath includes the graphite paper being arranged on carbide particle surface and the graphite powder being arranged on graphite paper.
9. the preparation method of a kind of sheet powder metallurgy according to claim 3, it is characterised in that：The step
Suddenly the programming rate of nitrogen treatment is 1-30 DEG C/min in (3).
10. the preparation method of a kind of sheet powder metallurgy according to claim 3, it is characterised in that：It is described
Oil bath heating is used in step (1) in corrosion process.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110615438A (en) * | 2018-10-10 | 2019-12-27 | 西南交通大学 | Ti3C2Method for preparing powder |
| CN113690444A (en) * | 2021-08-26 | 2021-11-23 | 大连理工大学 | Li based on MXene and transition metal oxynitride composite structure2S-based battery positive electrode material and synthesis method thereof |
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| JP3738784B2 (en) * | 1995-06-27 | 2006-01-25 | 石川島播磨重工業株式会社 | Method for producing interface control ceramics |
| CN106025200A (en) * | 2016-05-24 | 2016-10-12 | 浙江大学 | Preparation method and application of nitrogen-doped MXene battery anode material |
| CN106220180A (en) * | 2016-07-08 | 2016-12-14 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of two dimensional crystal MXene nano material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3738784B2 (en) * | 1995-06-27 | 2006-01-25 | 石川島播磨重工業株式会社 | Method for producing interface control ceramics |
| CN106025200A (en) * | 2016-05-24 | 2016-10-12 | 浙江大学 | Preparation method and application of nitrogen-doped MXene battery anode material |
| CN106220180A (en) * | 2016-07-08 | 2016-12-14 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of two dimensional crystal MXene nano material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110615438A (en) * | 2018-10-10 | 2019-12-27 | 西南交通大学 | Ti3C2Method for preparing powder |
| CN113690444A (en) * | 2021-08-26 | 2021-11-23 | 大连理工大学 | Li based on MXene and transition metal oxynitride composite structure2S-based battery positive electrode material and synthesis method thereof |
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