CN108585887A - A kind of TixZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology - Google Patents

A kind of TixZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology Download PDF

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CN108585887A
CN108585887A CN201810364420.6A CN201810364420A CN108585887A CN 108585887 A CN108585887 A CN 108585887A CN 201810364420 A CN201810364420 A CN 201810364420A CN 108585887 A CN108585887 A CN 108585887A
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powder
solid solution
production technology
ceramic raw
zro
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褚衍辉
刘达
周曦亚
敬思仪
叶贝琳
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South China University of Technology SCUT
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Abstract

The invention discloses a kind of TixZr1‑xB2Superhigh temperature solid solution ceramic raw powder's production technology, belongs to ultra-high temperature ceramic powder preparing technical field.The preparation method is by TiO2Powder, ZrO2Powder and amorphous boron powder are heat-treated 1 ~ 3 h under conditions of 1050 DEG C ~ 1150 DEG C after mixing with a certain amount of fused salt, pass through boron and TiO2、ZrO2Reaction generates Ti in fused salt environmentxZr1‑xB2Solid solution powder, the B then generated with deionized water and absolute ethyl alcohol infiltration the dissolving fused salt of heat and reaction2O3Obtain pure TixZr1‑xB2Solid solution powder.The method of the present invention is simple for process, production cost is low, and the powder constituents of synthesis are uniform, grain size is small and purity is high.In addition, can effectively control synthesis Ti by adjusting the amount of synthesis temperature and fused saltxZr1‑xB2The size of solid solution powder, these advantages make this method have the potentiality for developing into large-scale industrial production.

Description

A kind of TixZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology
Technical field
The present invention relates to ultra-high temperature ceramic powder preparing technical fields, and in particular to a kind of TixZr1-xB2Superhigh temperature solid solution The preparation method of ceramic powder.
Background technology
Superhigh temperature ceramic material mainly includes refractory boride, carbide, nitride and the phase of some magnesium-yttrium-transition metals The solid solution ceramic etc. answered, their fusing point is at 3000 DEG C or more.With single ceramic phase ratio, solid solution ceramic is because with more preferable The comprehensive performances such as physical chemistry and receive the concern of domestic and international researcher.Wherein, TixZr1-xB2Solid solution ceramic is because having Lower density（4.5~6.1 g/cm3）, high thermal conductivity and toughness, low coefficient of thermal expansion and good chemical stability It is received significant attention etc. a series of excellent performances.TixZr1-xB2The synthesis of solid solution powder is for TixZr1-xB2Solid solution The preparation and application of ceramics are most important, however, at present both at home and abroad for TixZr1-xB2The synthetic method of solid solution powder is reported It is less.
Document 1:“Peters J S, Cook B A, Harringa J L, et al. Erosion resistance of TiB2-ZrB2composites. Wear, 2009, 267(1-4):136 ~ 143. " describe a kind of utilization Ti, Zr gold Category powder, which is directly reacted with boron powder by high-energy ball milling, prepares TixZr1-xB2The method of solid solution powder.Due to this method synthesis Solid solution powder uneven components and diameter of particle is larger（Average grain diameter>1 μm）, meanwhile, the Ti of synthesisxZr1-xB2Solid solution powder In body the popularization of this method is seriously limited containing a large amount of impurity such as unreacted Ti, Zr and ball-milling medium, these disadvantages.
Invention content
In order to overcome the disadvantages mentioned above and deficiency of the prior art, the purpose of the present invention is to provide a kind of TixZr1-xB2Solid solution Body raw powder's production technology.This method is with ZrO2Powder, TiO2Powder, boron powder, KCl and NaCl are raw material, by using TiO2Powder, ZrO2Uniformly dispersed in fused salt of powder and boron powder successfully prepares the uniform Ti of ingredientxZr1-xB2Solid solution powder, this method It is simple for process, at low cost, efficient, the Ti of preparationxZr1-xB2Solid solution powder ingredient is uniform, grain size is small (average grain diameter be 50 ~ 200 nm）And purity is high, while also can be to the Ti of synthesis by adjusting preparation processxZr1-xB2Solid solution powder size is controlled System.
The purpose of the present invention is achieved through the following technical solutions.
A kind of TixZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology, includes the following steps：
（1）Take TiO2Powder, ZrO2Powder, boron powder, KCl, NaCl are placed in agate mortar and hand-ground, then by the mixed powder Transfer is as in corundum Noah's ark；
（2）Noah's ark is put into tube furnace, is kept the temperature again after heating, is then turned off power supply cooled to room temperature, in whole process It is passed through Ar gas shieldeds；
（3）Noah's ark is taken out and the mixture in Noah's ark is first washed with deionized, filter after dry, add absolute ethyl alcohol It is dried afterwards to get to Ti after magnetic agitation, filteringxZr1-xB2Superhigh temperature solid solution ceramic powder, wherein 0 x≤0.4 ＜.
Further, the step（1）In, ZrO2Powder and TiO2The total amount of powder is 3 with the molar ratio of boron powder:10, KCl and The gross mass of NaCl is ZrO2Powder, TiO2The molar ratio of 5 ~ 20 times of powder and boron powder gross mass, wherein KCl and NaCl are 1:1.
Further, step（1）In, the ZrO2The purity of powder is 99%, and grain size is 50 ~ 200 nm；The TiO2Powder Purity is 99%, and grain size is 50 ~ 200 nm；The purity of the boron powder be 99.9%, grain size be 0.7 ~ 0.9 μm, the KCl and NaCl reagent purities are that analysis is pure.
Further, step（1）In, the hand-ground time is 10 ~ 30min.
Further, step（2）In, tube furnace heating rate is 5 ~ 10 DEG C/min, and holding temperature is 1050 ~ 1150 DEG C, Soaking time is 1 ~ 3 h, and the flow for being passed through Ar gas is 100~300 sccm.
Further, step（3）In, the temperature of the deionized water is 80 ~ 100 DEG C, and the magnetic agitation time is 1 ~ 2 h, Drying box temperature is 40 ~ 80 DEG C, and drying time is 2 ~ 5 h.
Compared with prior art, the invention has the advantages that and advantageous effect：
（1）The method of the present invention is simple for process, production cost is low, the Ti of synthesisxZr1-xB2Solid solution powder ingredient is uniform, grain size is small And purity is high, is conducive to large-scale industrial production；
（2）The method of the present invention can effectively control synthesis by adjusting the content of fused salt, synthesis temperature and soaking time TixZr1-xB2The size of solid solution powder.
Description of the drawings
Fig. 1 is the Ti synthesized in embodiment 2xZr1-xB2The XRD spectrum of solid solution powder.
Fig. 2 is the Ti synthesized in embodiment 2xZr1-xB2The SEM photograph figure of solid solution powder.
Specific implementation mode
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment and attached drawing, but the guarantor of the present invention It protects range and embodiment is without being limited thereto.
In the specific embodiment of the invention, the TiO of use2Powder purity is 99%, and granularity is 50 ~ 200 nm；The ZrO of use2Powder Purity is 99%, and grain size is 50 ~ 200 nm；For the boron powder purity used for 99.9%, granularity is 0.7 ~ 0.9 μm；The KCl of use and NaCl reagent purities are that analysis is pure.
Embodiment 1
（1）The TiO of 0.13 g is weighed respectively2The ZrO of powder, 1.78g2Powder, the boron powder of 0.58 g, 17.03 g KCl and The NaCl of 13.91 g is placed in agate mortar and 20 min of hand-ground makes powder be uniformly mixed, and above-mentioned powder is transferred to just In beautiful Noah's ark；
（2）Noah's ark is put into tube furnace, vacuumize process is carried out to tube furnace, makes pressure vacuum gauge number after vacuumizing 10 min Value reaches -0.1 MPa, fidelity 10 min of sky, and observation vacuum meter indicates whether to change, such as unchanged, illustrates that system sealing is intact, This process was repeated three times.Ar gas is passed through to normal pressure, furnace temperature is risen to 1100 DEG C from room temperature with the heating rate of 8 DEG C/min later, Keep the temperature 2h；It is then turned off power supply cooled to room temperature, leads to Ar gas shieldeds in whole process, the flow of Ar gas is maintained at 200 sccm；
（3）Dry 3 h are filtered and are put into 60 DEG C of baking oven after obtained mixture is washed in 90 DEG C of deionized water, it is past Absolute ethyl alcohol and using being filtered after 1.5 h of magnetic stirrer is added in the powder obtained after drying, repeatedly the above process four It is secondary, the product after final filtration is placed in 60 DEG C of drying box dry 4 h and obtains target product.It synthesizes under this condition Ti0.1Zr0.9B2Solid solution powder is pure phase, and average grain diameter is about 100 nm.
Embodiment 2
（1）The TiO of 0.26 g is weighed respectively2The ZrO of powder, 1.60 g2Powder, the boron powder of 0.58 g, 6.56 g KCl and The NaCl of 5.35 g is placed in agate mortar and 10 min of hand-ground makes powder be uniformly mixed, and above-mentioned powder is transferred to corundum In Noah's ark；
（2）Noah's ark is put into tube furnace, vacuumize process is carried out to tube furnace, makes pressure vacuum gauge number after vacuumizing 10 min Value reaches -0.1 MPa, fidelity 10 min of sky, and observation vacuum meter indicates whether to change, such as unchanged, illustrates that system sealing is intact, This process was repeated three times.Ar gas is passed through to normal pressure, furnace temperature is risen to 1050 DEG C from room temperature with the heating rate of 5 DEG C/min later, Keep the temperature 1 h；It is then turned off power supply cooled to room temperature, leads to Ar gas shieldeds in whole process, the flow of Ar gas is maintained at 100 sccm；
（3）Dry 1 h is filtered and is put into 40 DEG C of baking oven after obtained mixture is washed in 80 DEG C of deionized water, it is past Absolute ethyl alcohol is added in the powder obtained after drying and using being filtered after 1 h of magnetic stirrer, the above process four times repeatedly, Product after final filtration is placed in 40 DEG C of drying box dry 2 h and obtains target product.
Fig. 1 is Ti prepared by this experiment embodiment0.2Zr0.8B2The XRD spectrum of solid solution powder, the collection of illustrative plates show prepared Ti0.2Zr0.8B2Solid solution powder is pure phase, does not contain other impurities phase.Fig. 2 is Ti prepared by this experiment embodiment0.2Zr0.8B2Gu The SEM photograph of solution powder, as shown in Figure 2, the Ti synthesized under this condition0.2Zr0.8B2Solid solution powder crystallite dimension is smaller, puts down Equal grain size is about 50 nm.
Embodiment 3
（1）The TiO of 0.51 g is weighed respectively2The ZrO of powder, 1.19 g2Powder, the boron powder of 0.58 g, 26.24 g KCl and The NaCl of 21.40 g is placed in agate mortar and 30 min of hand-ground makes powder be uniformly mixed, and above-mentioned powder is transferred to just In beautiful Noah's ark；
（2）The Noah's ark is put into tube furnace, vacuumize process is carried out to tube furnace, makes pressure vacuum gauge after vacuumizing 10 min Numerical value reaches -0.1 MPa, fidelity 10 min of sky, and observation vacuum meter indicates whether to change, such as unchanged, illustrates that system sealing is complete Good, this process was repeated three times.Ar gas is passed through to normal pressure, furnace temperature is risen to 1150 from room temperature with the heating rate of 10 DEG C/min later DEG C, keep the temperature 3 h；It is then turned off power supply cooled to room temperature, leads to Ar gas shieldeds in whole process, the flow of Ar gas is maintained at 300 sccm；
（3）Dry 5 h are filtered and are put into 80 DEG C of baking oven after obtained mixture is washed in 100 DEG C of deionized water, Absolute ethyl alcohol is added in the powder obtained after dry and using being filtered after 2 h of magnetic stirrer, repeatedly the above process four It is secondary, the product after final filtration is placed in 80 DEG C of drying box dry 5 h and obtains target product.It synthesizes under this condition Ti0.4Zr0.6B2Solid solution powder is pure phase, and average grain diameter is about 200 nm.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not limited by above-described embodiment System, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications, Equivalent substitute mode is should be, is included within the scope of the present invention.

Claims (6)

1. a kind of TixZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology, which is characterized in that include the following steps：
Take TiO2Powder, ZrO2Powder, boron powder, KCl, NaCl are placed in agate mortar and hand-ground, then shifts the mixed powder Into corundum Noah's ark；
Noah's ark is put into tube furnace, is kept the temperature again after heating, power supply cooled to room temperature is then turned off, is passed through in whole process Ar gas shieldeds；
Noah's ark is taken out and the mixture in Noah's ark is first washed with deionized, filter after dry, after adding absolute ethyl alcohol It is dried to get to Ti after magnetic agitation, filteringxZr1-xB2Superhigh temperature solid solution ceramic powder, wherein 0 x≤0.4 ＜.
2. a kind of Ti according to claim 1xZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology, feature exist In the step（1）In, ZrO2Powder and TiO2The total amount of powder is 3 with the molar ratio of boron powder:The gross mass of 10, KCl and NaCl is ZrO2Powder, TiO2The molar ratio of 5 ~ 20 times of powder and boron powder gross mass, wherein KCl and NaCl are 1:1.
3. a kind of Ti according to claim 1xZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology, feature exist In step（1）In, the ZrO2The purity of powder is 99%, and grain size is 50 ~ 200 nm；The TiO2The purity of powder is 99%, grain size For 50 ~ 200 nm；The purity of the boron powder is 99.9%, and grain size is 0.7 ~ 0.9 μm, KCl the and NaCl reagent purities are It analyzes pure.
4. a kind of Ti according to claim 1xZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology, feature exist In step（1）In, the hand-ground time is 10 ~ 30min.
5. a kind of Ti according to claim 1xZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology, feature exist In step（2）In, tube furnace heating rate is 5 ~ 10 DEG C/min, and holding temperature is 1050 ~ 1150 DEG C, and soaking time is 1 ~ 3 H, the flow for being passed through Ar gas are 100~300 sccm.
6. a kind of Ti according to claim 1xZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology, feature exist In step（3）In, the temperature of the deionized water is 80 ~ 100 DEG C, and the magnetic agitation time is 1 ~ 2 h, drying box temperature is 40 ~ 80 DEG C, drying time is 2 ~ 5 h.
CN201810364420.6A 2018-04-23 2018-04-23 A kind of TixZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology Pending CN108585887A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678523A (en) * 2019-01-16 2019-04-26 广东工业大学 A kind of high entropy ceramics and its preparation method and application with elevated temperature strength and hardness
CN109851367A (en) * 2019-03-11 2019-06-07 华南理工大学 A kind of rodlike (Zr, Hf, Ta, Nb) B2High entropy nanometer powder and preparation method thereof
CN110818432A (en) * 2019-11-19 2020-02-21 华南理工大学 Superfine high-entropy boride nano powder and preparation method thereof
CN114736024A (en) * 2022-03-03 2022-07-12 西安交通大学 Ultrahigh-temperature ceramic solid solution coated carbon microsphere composite powder with core-shell structure and preparation method thereof

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CN103950946A (en) * 2014-05-22 2014-07-30 安徽工业大学 Preparation method of nano niobium boride powder

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CN103950946A (en) * 2014-05-22 2014-07-30 安徽工业大学 Preparation method of nano niobium boride powder

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678523A (en) * 2019-01-16 2019-04-26 广东工业大学 A kind of high entropy ceramics and its preparation method and application with elevated temperature strength and hardness
CN109678523B (en) * 2019-01-16 2021-04-06 广东工业大学 High-entropy ceramic with high-temperature strength and hardness and preparation method and application thereof
CN109851367A (en) * 2019-03-11 2019-06-07 华南理工大学 A kind of rodlike (Zr, Hf, Ta, Nb) B2High entropy nanometer powder and preparation method thereof
CN109851367B (en) * 2019-03-11 2021-08-10 华南理工大学 A rod-like (Zr, Hf, Ta, Nb) B2High-entropy nano powder and preparation method thereof
CN110818432A (en) * 2019-11-19 2020-02-21 华南理工大学 Superfine high-entropy boride nano powder and preparation method thereof
CN110818432B (en) * 2019-11-19 2024-05-17 华南理工大学 Superfine high-entropy boride nano powder and preparation method thereof
CN114736024A (en) * 2022-03-03 2022-07-12 西安交通大学 Ultrahigh-temperature ceramic solid solution coated carbon microsphere composite powder with core-shell structure and preparation method thereof

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Application publication date: 20180928