CN112079640B - MoSi 2 @ZrO 2 Preparation method of core-shell structure - Google Patents
MoSi 2 @ZrO 2 Preparation method of core-shell structure Download PDFInfo
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- 229910016006 MoSi Inorganic materials 0.000 title claims abstract description 31
- 239000011258 core-shell material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000000725 suspension Substances 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012670 alkaline solution Substances 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000002612 dispersion medium Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000009768 microwave sintering Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 239000002131 composite material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000607479 Yersinia pestis Species 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 239000002120 nanofilm Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 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 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
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- 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
- C04B35/58085—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 silicides
- C04B35/58092—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 silicides based on refractory metal silicides
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- 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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62818—Refractory metal oxides
- C04B35/62823—Zirconium or hafnium oxide
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Abstract
The invention discloses MoSi 2 @ZrO 2 The preparation method of the core-shell structure comprises the following steps of (1) MoSi 2 Adding the powder and SDS into a beaker, mechanically and ultrasonically stirring, and using water or alcohol as a dispersion medium; (2) After dispersing for a certain time, adding a zirconium source into the suspension, and dropwise adding an alkaline solution NH 3 ·H 2 O or NaOH until the PH value is between 7 and 14; continuously stirring for a certain time until the mixture is uniformly mixed; (3) Placing the prepared suspension into a reaction kettle, and curing for 12-48 h at 160-220 ℃; heating by using an oven, and keeping the temperature of the suspension after the suspension reaches a certain temperature through a certain heating rate; (4) After hydrothermal reaction synthesis, filtering, washing, drying and sieving to obtain powder; (5) Calcining the prepared powder in calcining equipment for 1-6 h, and keeping the temperature at 300-400 ℃; (6) Obtaining MoSi through the steps 2 @ZrO 2 Core-shell structure of synthetic ZrO 2 The volume fraction of the powder is 10-30 vol%. The invention adopts a hydrothermal method, has no pollution, reduces the requirement of equipment and is environment-friendly.
Description
Technical Field
The invention relates to the technical field of preparation of high-performance ceramic matrix composite powder, in particular to MoSi 2 @ZrO 2 A preparation method of a core-shell structure.
Background
MoSi 2 Has the advantages of higher melting point (2303K), high strength, good thermal conductivity and the like, and is a candidate material of the next generation high-temperature material. In particular, it is considered to be a promising high temperature coating for aerospace, nuclear industry, metallurgy and electronics. MoSi 2 The low-temperature brittleness (BDTT is between 900 and 1000 ℃), the high-temperature strength above 1300 ℃ is insufficient, and especially the creep resistance is lower. And MoSi at 400-600 deg.c 2 Accelerated oxidation occurs and eventually changes from a dense body to a powder, a phenomenon known as Pest. These disadvantages limit the MoSi 2 As an application for high temperature structures. Thus, room temperature toughening and high temperature reinforcement, and suppression of low temperature Pest is MoSi 2 There is a need for a key problem to be solved.
The hydrothermal method is to prepare ZrO 2 An important method for preparing powder features that the preparing process is completed at high temp. and pressure in one step without need of later crystallizing treatment, and the obtained powder has narrow granularity distribution and pure components.
The core-shell type nano-particle is a composite multinomial structure formed by using a particle formed by a micron to nano film as a core and coating a plurality of layers of uniform nano films on the surface of the particle, and the core and the shell are mutually connected through physical or chemical action. The chemical inertness of the cladding layer in the core-shell composite material can improve the stability of the nano particles, so that the core-shell structure material has more excellent physical and chemical properties than the single central particle, and has wide application prospect.
The MoSi is obtained by adopting mechanical stirring dispersion and hydrothermal synthesis 2 @ZrO 2 A core-shell structure. Coated with several layers of ZrO 2 With the object of preventing MoSi 2 Oxidation at low temperature (400-600 deg.C), and enhanced room temperature strength and fracture toughness. Is MoSi 2 The wide application of the base composite material lays a foundation.
Disclosure of Invention
The invention aims to solve the problems that: provides a MoSi 2 @ZrO 2 Preparation of core-shell structure from MoSi 2 As a matrix, by adding ZrOCl 2 ·8H 2 O in the hydrothermal synthesis process, zrO is synthesized 2 Further coating with MoSi 2 . Elimination of MoSi during sintering 2 ZrO produced by hydrothermal reaction under the harm of low-temperature oxidation 2 Thereby obtaining MoSi 2 @ZrO 2 A core-shell structure. This provides for further improvement of the mechanical properties of the composite material in the future.
The technical scheme provided by the invention for solving the problems is as follows: moSi 2 @ZrO 2 A method for preparing a core-shell structure, the method comprising the steps of,
(1) Certain proportion of MoSi 2 Adding the powder and SDS into a beaker, and mechanically and ultrasonically stirring, wherein water or alcohol is used as a dispersion medium;
(2) After dispersing for a certain time, adding a certain amount of zirconium source into the suspension, and dropwise adding an alkaline solution NH 3 ·H 2 O or NaOH until the PH value is between 7 and 14; continuously stirring for a certain time until the mixture is uniformly mixed;
(3) Placing the prepared suspension into a reaction kettle, and curing for 12-48 h at 160-220 ℃; heating by using an oven, and keeping the temperature of the suspension after the suspension reaches a certain temperature through a certain heating rate;
(4) After hydrothermal reaction synthesis, filtering, washing, drying and sieving to obtain powder;
(5) Calcining the prepared powder in calcining equipment for 1-6 h, and keeping the temperature at 300-400 ℃;
(6) Obtaining MoSi through the steps 2 @ZrO 2 Core-shell structure of synthetic ZrO 2 The volume fraction of the powder is 10-30 vol%.
Preferably, the dispersing time in the step (2) is 1 to 6 hours.
Preferably, the calcining equipment in the step (5) is an atmosphere tube furnace, a high-temperature vacuum furnace or a microwave sintering furnace.
Preferably, the temperature rise rate of the calcination in the step (5) is 5-20 ℃/min, the heat preservation time is 30-180 min, and the calcination atmosphere is vacuum, argon atmosphere or nitrogen atmosphere.
Compared with the prior art, the invention has the advantages that:
(1) Dispersing MoSi by adopting a mechanical stirring method 2 Powder, avoiding powder agglomeration and obtaining uniform suspension.
(2) And a hydrothermal method is adopted, so that the method is pollution-free, reduces the requirements of equipment and is environment-friendly.
(3) The preparation process is completed at one time under high temperature and high pressure, the later crystallization treatment is not needed, and the obtained powder has narrow particle size distribution and pure components.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 shows MoSi 2 @ZrO 2 XRD pattern of core-shell structure.
FIG. 2 shows the preparation of MoSi in example 1 2 @ZrO 2 TEM image of core-shell structure.
Detailed Description
The embodiments of the present invention will be described in detail with reference to the accompanying drawings and examples, so that how to implement the technical means for solving the technical problems and achieving the technical effects of the present invention can be fully understood and implemented.
Example 1
2.5g of MoSi after ball milling 2 Adding the powder and 1.6g/L SDS into a beaker containing 200ml distilled water, and carrying out mechanical ultrasonic stirring by using water as a dispersion medium; after 6h of dispersion, 1.5338g of zirconium source ZrOCl were added to the suspension 2 ·8H 2 O, calculated as 20% vol ZrO 2 . Alkaline solution NH is dripped 3 ·H 2 O to PH =9 or so. Stirring for 3h until uniform. Placing the prepared suspension into a reaction kettleHeating to 200 ℃ by using an oven, and curing for 24 hours at the curing temperature of 200 ℃. After the hydrothermal reaction synthesis, the composite powder is obtained by filtering with distilled water and alcohol, washing for three times respectively, drying, and sieving with a 200-mesh sieve. Calcining the prepared powder in an atmosphere tube furnace for 3 hours at the temperature of 380 ℃. Obtaining MoSi through the steps 2 @ZrO 2 A core-shell structure.
The foregoing is illustrative of the preferred embodiments of the present invention only and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary. All changes which come within the scope of the invention as defined by the independent claims are intended to be embraced therein.
Claims (3)
1. MoSi 2 @ZrO 2 The preparation method of the core-shell structure is characterized in that: the method comprises the following steps of (a) carrying out,
(1) Certain proportion of MoSi 2 Adding the powder and SDS into a beaker, mechanically and ultrasonically stirring, and using water or alcohol as a dispersion medium;
(2) After dispersing for a certain time, adding a certain amount of zirconium source ZrOCl into the suspension 2 ·8H 2 O, dropwise adding alkaline solution NH 3 ·H 2 O or NaOH until the pH value is between 7 and 14; continuously stirring for a certain time until the mixture is uniformly mixed;
(3) Placing the prepared suspension into a reaction kettle, and curing for 12-48 h at 160-220 ℃; heating by using an oven, and keeping the temperature of the suspension after the suspension reaches a certain temperature through a certain heating rate;
(4) After hydrothermal reaction synthesis, filtering, washing, drying and sieving to obtain powder;
(5) Calcining the prepared powder in calcining equipment for 1-6 h, and keeping the temperature at 300-400 ℃; the temperature rising rate of the calcination is 5-20 ℃/min, the heat preservation time is 30-180 min, and the calcination atmosphere is vacuum, argon atmosphere or nitrogen atmosphere;
(6) Obtaining MoSi through the steps 2 @ZrO 2 Core-shell structure of synthetic ZrO 2 Powder bodyThe integral percentage is 10-30 vol%.
2. MoSi according to claim 1 2 @ZrO 2 The preparation method of the core-shell structure is characterized by comprising the following steps: the dispersion time in the step (2) is 1-6 h.
3. MoSi according to claim 1 2 @ZrO 2 The preparation method of the core-shell structure is characterized in that: and (5) calcining equipment is an atmosphere tube furnace, a high-temperature vacuum furnace and a microwave sintering furnace.
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CN115321541B (en) * | 2022-07-27 | 2023-06-09 | 南昌航空大学 | MoSi (MoSi) 2 Material with@Nb core-shell structure and preparation method thereof |
CN115636691A (en) * | 2022-11-01 | 2023-01-24 | 陕西科技大学 | Spherical coating MoSi 2 @Y 2 O 3 Core-shell structure microcapsule powder and preparation method and application thereof |
CN115974561B (en) * | 2022-12-15 | 2024-01-16 | 内蒙古工业大学 | Mo-Si metal silicide/ZrC nano composite powder and preparation method thereof |
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