CN113185300A - Macro-particle-size-controllable ZrB2Method for preparing powder - Google Patents

Macro-particle-size-controllable ZrB2Method for preparing powder Download PDF

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CN113185300A
CN113185300A CN202110563705.4A CN202110563705A CN113185300A CN 113185300 A CN113185300 A CN 113185300A CN 202110563705 A CN202110563705 A CN 202110563705A CN 113185300 A CN113185300 A CN 113185300A
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powder
zrb
macro
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喇培清
许珂
占发琦
张华�
吴浩恺
朱敏
郑月红
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Lanzhou University of Technology
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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
    • C04B35/5805—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 borides
    • C04B35/58064—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 borides based on refractory borides
    • C04B35/58078—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 borides based on refractory borides based on zirconium or hafnium 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
    • C01B35/04—Metal borides
    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

Macro-particle-size-controllable ZrB2The preparation method of the powder comprises the following steps: weighing the reaction materials according to a preset proportion, and adding an inert diluent with a preset content to prepare an initial mixture; step (2) placing the initial mixture into a ball mill for uniform mixing, and then pressing the mixture into a cake-shaped blank with the diameter of 80 mm and the height of about 20-50 mm on a press machine; putting the cake-shaped blank into a reaction kettle, putting an ignition agent on the blank, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until the system generates a self-propagating reaction to obtain a black blocky initial product; crushing the primary product, leaching with hydrochloric acid solution and distilled water to reach the purification standard, and drying in a vacuum drying oven to obtain ZrB2And (3) powder.

Description

Macro quantityControllable-granularity ZrB2Method for preparing powder
Technical Field
The invention relates to a grain size controllable ZrB2A preparation technology of powder.
Background
Zirconium diboride is a material with great development prospect, and has high melting point (3245 ℃) and medium thermal conductivity coefficient (60 W.m)-1•K-1) Conductivity (107 s.m)-1) Higher hardness (23 GPa) and young's modulus (495 GPa), good wear resistance, and good corrosion resistance. Based on these excellent characteristics, ZrB2Materials used in rockets and supersonic aircraft, cutting tools, crucibles, high temperature heating elements and coating materials, and also in the fields of electrodes and microelectronics.
But ZrB2The applications of (a) are limited by sintering difficulties, mainly due to oxygen contamination and low self-diffusion coefficients resulting from strong chemical bonds in the resulting material inhibiting the diffusion degradation of the grains. By preparing nano ZrB with larger specific surface area and higher surface energy2This problem can be ameliorated.
ZrB2The main preparation method comprises the following steps: carbothermic processes, sol-gel processes, self-propagating high temperature synthesis processes, and mechanical alloying. The current situation of recent years of research, utilizing ZrO2And B4C is used as a raw material, and submicron ZrB2 powder with the minimum particle size of 245 nm is synthesized by a carbothermic method. Using ZrCl4And H3BO3ZrB2 powder with the average grain diameter less than 250 nm is prepared by a sol-gel method. Using ZrO2、B2O3And C as raw material, obtaining ZrB by mechanical alloying2The size of the calculated microcrystal of the powder is 67 nm, but the projection electron microscope image shows that the crystallite size is 0.5-1 mu m. Using ZrO2And amorphous B as raw material, adding NaCl as diluent, and salt-assisted combustion to synthesize ZrB with average particle size of 500 nm2And (3) powder. From recent research work, most of the ZrB prepared in the reports2The powder particles are all in submicron level, do not really reach nanometer level, and the particle size is not adjustableThe preparation is controlled and all prepared in trace amount. Therefore, a large-scale preparation method of high-quality ZrB with controllable granularity is needed2A preparation technology of powder.
Disclosure of Invention
The invention aims to provide the ZrB with controllable macro-particle size2A method for preparing powder.
The invention relates to a macro-particle size controllable ZrB2The preparation method of the powder comprises the following steps:
weighing the reaction materials according to a preset proportion, and adding an inert diluent with a preset content to prepare an initial mixture;
step (2) placing the initial mixture into a ball mill for uniform mixing, and then pressing the mixture into a cake-shaped blank with the diameter of 80 mm and the height of about 20-50 mm on a press machine;
putting the cake-shaped blank into a reaction kettle, putting an ignition agent on the blank, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until the system generates a self-propagating reaction to obtain a black blocky initial product;
crushing the primary product, leaching with hydrochloric acid solution and distilled water to reach the purification standard, and drying in a vacuum drying oven to obtain ZrB2And (3) powder.
The invention has the beneficial effects that: the energy consumption cost is low, an external heat source is not needed after the reaction is started, and the reaction is only needed to be heated to 280-350 ℃; the process flow is simple, the production equipment is simplified, and the operation is simple; high yield, short preparation period, and capability of preparing high-purity ZrB with controllable granularity in one macroscopic quantity (kilogram grade)2Powder, and the granularity of the product is fine and uniform; the average particle size of the product can be regulated and controlled to be reduced from 1-3 mu m to less than 100 nm by changing the content of the diluent.
Drawings
FIG. 1 shows ZrB prepared by the method2XRD pattern of powder, FIG. 2 is ZrB prepared by the invention2EPMA map of powder, FIG. 3 shows ZrB prepared by the present invention2SEM image of powder, FIG. 4 is ZrB prepared by the invention2Particle size distribution of powder (0 wt.% diluent), FIG. 5 is a diagram of ZrB prepared by the present invention2Powder (60 wt. -%)NaCl-KCl).
Detailed Description
The invention relates to a macro-particle size controllable ZrB2The preparation method of the powder comprises the following steps:
weighing the reaction materials according to a preset proportion, and adding an inert diluent with a preset content to prepare an initial mixture;
step (2) placing the initial mixture into a ball mill for uniform mixing, and then pressing the mixture into a cake-shaped blank with the diameter of 80 mm and the height of about 20-50 mm on a press machine;
putting the cake-shaped blank into a reaction kettle, putting an ignition agent on the blank, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until the system generates a self-propagating reaction to obtain a black blocky initial product;
crushing the primary product, leaching with hydrochloric acid solution and distilled water to reach the purification standard, and drying in a vacuum drying oven to obtain ZrB2And (3) powder.
The preparation method, the reaction materials in the step (1) and the mass ratio of the reaction materials are ZrO2：B2O3: mg = 123:70: 134; the inert diluent category comprises one of NaCl and KCl or a mixture thereof; the addition amount of the diluent accounts for 0-60 wt% of the total mass of the reaction materials.
According to the preparation method, the ball milling parameters in the step (2) are that the time is 8-15 h, the rotating speed is 150 r/min, and the ball-to-material ratio is 2: 1; the pressure of the press is 30-50 MPa.
According to the preparation method, the preheating temperature in the step (3) is 280-350 ℃; the protective atmosphere is argon, the gas washing pressure is 0.5 MPa, and the pressure maintaining pressure is 2-4 MPa.
The preparation method described above, wherein the hydrochloric acid solution in step (4) is 3 mol/L hydrochloric acid diluent and is in excess of 50 vol.%; the purification standard is as follows: in the pickling process, the color of the PH test paper tested by the pickling waste liquid twice is not changed; in the water washing process, the water washing waste liquid is titrated by a silver nitrate solution, so that no white precipitate is generated; drying at 70 deg.C for 12 h.
The above-mentioned preparation method, ZrB2The particle size of the powder is reduced from 1-3 μm to less than 100 nm, and the minimum average particle size is 115 nm.
The following are specific examples of the present invention, and the technical solutions of the present invention will be further described with reference to the examples, but the present invention is not limited to the examples.
Example 1:
the reactant material in this example was ZrO2（>99.5 wt.%，1 μm）、B2O3（>99.95 wt.%）、Mg（>99.5 wt.%, 325 mesh), selecting NaCl-KCl as a diluent, wherein the addition amount is 0 wt.%, the ball milling time is 8 h, the pressurizing pressure is 30 MPa, and the protective atmosphere pressure is 2 MPa, and the specific steps are as follows:
(1) firstly, respectively placing zirconium oxide, graphite and diluent in a drying oven for drying, adjusting the temperature to 50 ℃ for 24 hours, and then placing ZrO2：B2O3: mg = 123:70:134 batch, NaCl was added in an amount of 60 wt.% of the total mass of the reaction mass, the total mass of the initial mixture being 1 kg. Accurately weighing the reaction raw materials by using an electronic balance;
(2) mixing the initial mixture with QM-ISP4 planetary ball mill at 150 r/min for 8 hr, at a ball-to-material ratio of 2: 1;
(3) pressing the uniformly mixed reaction materials into a cake-shaped blank with the diameter of 80 mm and the height of about 20-50 mm in a die on a Y32-100t hydraulic press under the pressure of 30 MPa;
(4) putting the cake-shaped blank into a combustion synthesis reaction kettle, filling 0.5 MPa of argon, keeping for 10-20 min, discharging gas, and removing air in the kettle; when the temperature in the reaction kettle is heated to 170 ℃, discharging residual gas in the kettle, then filling argon until the pressure in the kettle is 2 Mpa, and when the temperature in the kettle is increased to 310 ℃, carrying out self-propagating reaction; after the sample is naturally cooled in the reaction kettle, taking out the black block sample, crushing and then carrying out subsequent purification;
(5) a50 vol.% excess of a 3 mol/L dilution of hydrochloric acid was made with 12 mol/L standard hydrochloric acid, and the product powder was immersed in it and placed in a magnetic stirrer for continuous stirring. Using pH test paper every 4 h or so in the acid washing processAnd testing the pH value of the solution to ensure that the solution keeps acidic, and adding a proper amount of hydrochloric acid diluent again if the solution is neutral or alkaline. And finishing the acid washing when the color of the pH test paper tested twice is not changed any more. Then repeatedly washing with distilled water to remove excessive salt, wherein the standard of washing is that the solution after the last washing is dripped into silver nitrate detection solution to avoid white precipitate, and Cl in the water washing solution is detected-To ensure that the salt is sufficiently removed. Finally, the isolated product was placed in a vacuum oven and dried at 70 ℃ for 12 h.
Example 2:
in the embodiment, NaCl-KCl is used as a diluent, the addition amount is 50 wt.%, the ball milling time is 8 h, the pressurizing pressure is 30 MPa, and the pressure of the protective atmosphere is 2 MPa, and the specific steps are the same as those in embodiment 1.
Example 3:
in the embodiment, NaCl-KCl is used as a diluent, the addition amount is 60 wt.%, the ball milling time is 8 h, the pressurizing pressure is 30 MPa, and the pressure of the protective atmosphere is 2 MPa, and the specific steps are the same as those in embodiment 1.
Example 4:
in the embodiment, NaCl is used as a diluent, the addition amount is 60 wt.%, the ball milling time is 8 h, the pressurizing pressure is 30 MPa, and the pressure of the protective atmosphere is 2 MPa, and the specific steps are the same as those in embodiment 1.
The sample prepared by the present invention is ZrB as shown in FIG. 12The phases, as shown in table 1, all had a purity of 99 wt.% or more. ZrB prepared by the invention as shown in FIG. 32The powder particles are fine and uniform. As shown in Table 2, ZrB can be controlled by changing the content of the diluent2The average particle diameter of the powder is reduced from 1-3 μm to 100 nm, and the median diameter D50 is reduced from 2 μm to 80 nm.
TABLE 1 elemental content of inventive samples
Figure DEST_PATH_IMAGE001
TABLE 2 particle size parameters of samples prepared according to the invention
Figure DEST_PATH_IMAGE002
。

Claims (6)

1. Macro-particle-size-controllable ZrB2The preparation method of the powder is characterized by comprising the following steps:
weighing the reaction materials according to a preset proportion, and adding an inert diluent with a preset content to prepare an initial mixture;
step (2) placing the initial mixture into a ball mill for uniform mixing, and then pressing the mixture into a cake-shaped blank with the diameter of 80 mm and the height of about 20-50 mm on a press machine;
putting the cake-shaped blank into a reaction kettle, putting an ignition agent on the blank, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until the system generates a self-propagating reaction to obtain a black blocky initial product;
crushing the primary product, leaching with hydrochloric acid solution and distilled water to reach the purification standard, and drying in a vacuum drying oven to obtain ZrB2And (3) powder.
2. Macro-grain controllable ZrB according to claim 12The preparation method of the powder is characterized in that the reaction materials in the step (1) and the mass ratio of the reaction materials are ZrO2：B2O3: mg = 123:70: 134; the inert diluent category comprises one of NaCl and KCl or a mixture thereof; the addition amount of the diluent accounts for 0-60 wt% of the total mass of the reaction materials.
3. Macro-grain controllable ZrB according to claim 12The preparation method of the powder is characterized in that the ball milling parameters in the step (2) are 8-15 h, the rotating speed is 150 r/min, and the ball-to-material ratio is 2: 1; the pressure of the press is 30-50 MPa.
4. Macro-grain controllable ZrB according to claim 12The preparation method of the powder is characterized in that the preheating temperature in the step (3) is 280-350 ℃; the protective atmosphere is argon, the gas washing pressure is 0.5 MPa, and the pressure maintaining pressure is2~4 MPa。
5. Macro-grain controllable ZrB according to claim 12The preparation method of the powder is characterized in that the hydrochloric acid solution in the step (4) is 3 mol/L hydrochloric acid diluent, and the excessive amount is 50 vol.%; the purification standard is as follows: in the pickling process, the color of the PH test paper tested by the pickling waste liquid twice is not changed; in the water washing process, the water washing waste liquid is titrated by a silver nitrate solution, so that no white precipitate is generated; drying at 70 deg.C for 12 h.
6. Macro-grain controllable ZrB according to claim 12The method for preparing the powder is characterized in that ZrB2The particle size of the powder is reduced from 1-3 μm to less than 100 nm, and the minimum average particle size is 115 nm.
CN202110563705.4A 2021-05-24 2021-05-24 Macro-particle-size-controllable ZrB2Method for preparing powder Pending CN113185300A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114790518A (en) * 2022-05-05 2022-07-26 兰州理工大学 Preparation method of metal vanadium

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