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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- CN112079640B CN112079640B CN202010702108.0A CN202010702108A CN112079640B CN 112079640 B CN112079640 B CN 112079640B CN 202010702108 A CN202010702108 A CN 202010702108A CN 112079640 B CN112079640 B CN 112079640B
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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
- C04B35/515—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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- 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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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- C04B35/62805—Oxide ceramics
- C04B35/62818—Refractory metal oxides
- C04B35/62823—Zirconium or hafnium oxide
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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