CN110845234A - Spherical hollow ZrTiO4Ceramic powder and preparation method and application thereof - Google Patents
Spherical hollow ZrTiO4Ceramic powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramics, and particularly relates to spherical hollow ZrTiO4Ceramic powder and a preparation method and application thereof. The invention provides spherical hollow ZrTiO4The preparation method of the ceramic powder comprises the following steps: mixing zirconium boride, titanium boride, a dispersant, a binder and water, and carrying out ball milling to obtain slurry; carrying out centrifugal atomization treatment on the slurry to obtain agglomerated powder; sequentially carrying out binder removal and sintering treatment on the agglomerated powder to obtain sintered powder; carrying out plasma jet treatment on the sintering powder to obtain the spherical hollow ZrTiO4And (3) ceramic powder. The method directly obtains the spherical ZrTiO with the hollow structure without using various chemical reagents and templates4The ceramic powder ensures the high purity of the product.
Description
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to spherical hollow ZrTiO4Ceramic powder and a preparation method and application thereof.
Background
ZrTiO4The ceramic has high dielectric constant and low dielectric loss in the aspect of telecommunication, and is widely used for microwave communication dielectric resonators; in addition, the material is also used as functional ceramic (such as humidity sensor) due to its high fracture toughness, good wear resistance and low thermal conductivityCeramic materials) and are widely used in the fields of high-temperature pigments and functional catalysts. In addition, ZrTiO also belongs to the fields of catalysts, sensors, bioactive membrane materials and the like4Ceramics have raised requirements for large specific surface area, high chemical purity, and good compositional uniformity.
ZrTiO4Ceramics are usually prepared by ZrTiO4And preparing the ceramic powder. Currently, ZrTiO is prepared4The ZrO of the ceramic powder needs to be heated for a long time at the temperature of 1200-1600 ℃ or above2And TiO2Powder of ZrO2And TiO2Reacting to obtain; in order to obtain fine-grained high-quality ZrTiO4The ceramic powder can adopt sol-gel, coprecipitation, hydrolysis and other methods at a lower processing temperature, but the reaction route of the methods is complex, and a plurality of chemical reagents are used, so that the ZrTiO finally prepared4The chemical purity of the ceramic powder is not high; in addition, a template is generally required in the preparation process of the conventional hollow material, but pollution is easily caused in the subsequent calcining process, the chemical purity of the product is reduced, and the chemical purity of the hollow material is not ensured and improved.
Disclosure of Invention
In view of the above, the present invention provides a spherical hollow ZrTiO4Ceramic powder and preparation method thereof, and spherical hollow ZrTiO provided by the invention4The preparation method of the ceramic powder has simple process, no template is needed, and the prepared ZrTiO has high purity4The ceramic powder has high chemical purity and good hollow appearance; the invention also provides spherical hollow ZrTiO4Application of ceramic powder.
In order to achieve the purpose of the invention, the invention provides the following technical scheme:
the invention provides spherical hollow ZrTiO4The preparation method of the ceramic powder comprises the following steps:
mixing zirconium boride, titanium boride, a dispersant, a binder and water, and carrying out ball milling to obtain slurry;
carrying out centrifugal atomization treatment on the slurry to obtain agglomerated powder;
sequentially carrying out binder removal and sintering treatment on the agglomerated powder to obtain sintered powder;
carrying out plasma jet treatment on the sintering powder to obtain the spherical hollow ZrTiO4And (3) ceramic powder.
Preferably, the molar ratio of the zirconium boride to the titanium boride is 1: 1; the mass of the dispersing agent is 5-10% of the total mass of zirconium boride and titanium boride; the mass of the binder is 5-10% of the total mass of the zirconium boride and the titanium boride; the solid content of the slurry is 20-30%.
Preferably, the particle size of the zirconium boride is 1-5 μm; the particle size of the titanium boride is 3-5 mu m.
Preferably, the inlet temperature of the centrifugal atomization treatment is 200-300 ℃, and the outlet temperature is 100-150 ℃; the particle size of the agglomerated powder is 15-45 mu m.
Preferably, the degree of vacuum of the back bottom of the glue discharging and sintering treatment is 10-5～10-3Pa。
Preferably, the sintering treatment temperature is 1400-1500 ℃, and the time is 2-4 h.
Preferably, the plasma gun current in the plasma jet treatment is 600-700A, the argon flow is 20-40L/min, and the hydrogen flow is 10-12L/min.
The invention also provides the spherical hollow ZrTiO prepared by the preparation method of the technical scheme4And (3) ceramic powder.
Preferably, the spherical hollow ZrTiO4The grain size of the ceramic powder is 15-45 mu m.
The invention also provides the spherical hollow ZrTiO in the technical scheme4The application of the ceramic powder in the field of ceramics.
The invention provides spherical hollow ZrTiO4The preparation method of the ceramic powder comprises the following steps: mixing zirconium boride, titanium boride, a dispersant, a binder and water, and carrying out ball milling to obtain slurry; carrying out centrifugal atomization treatment on the slurry to obtain agglomerated powder; sequentially carrying out binder removal and sintering treatment on the agglomerated powder to obtain sintered powder; carrying out plasma jet treatment on the sintering powder to obtain the spherical hollow ZrTiO4And (3) ceramic powder. The invention uniformly mixes materials by ball milling, obtains quickly dried agglomerated powder with proper particle size by centrifugal atomization treatment, ensures that the agglomerated powder has certain structural strength by degumming and sintering treatment, is not broken in the powder feeding process, reduces the uniformity of powder components, improves the powder fluidity, is convenient to feed into the middle of plasma jet, and finally realizes the quick reaction and spheroidization of the preparation raw materials and the formation of a hollow structure by utilizing the characteristic of high-temperature and high-speed jet flow generated by plasma jet, and has quick preparation process, thus obtaining the spherical hollow ZrTiO4And (3) ceramic powder. The method directly obtains the spherical ZrTiO with the hollow structure without using various chemical reagents and templates4The ceramic powder ensures the high purity of the product.
The test result of the embodiment shows that the spherical hollow ZrTiO provided by the invention4The ceramic powder has a spherical and hollow structure, Dv (5) is 15.5 μm, Dv (95) is 43.7 μm, and the particle size is 15-45 μm.
Drawings
FIG. 1 shows a spherical hollow ZrTiO obtained in example 1 of the present invention4SEM picture of ceramic powder;
FIG. 2 shows spherical hollow ZrTiO obtained in example 1 of the present invention4A SEM image of the cross-sectional appearance of the ceramic powder;
FIG. 3 shows spherical hollow ZrTiO obtained in example 1 of the present invention4The particle size distribution of the ceramic powder.
Detailed Description
The invention provides spherical hollow ZrTiO4The preparation method of the ceramic powder comprises the following steps:
mixing zirconium boride, titanium boride, a dispersant, a binder and water, and carrying out ball milling to obtain slurry;
carrying out centrifugal atomization treatment on the slurry to obtain agglomerated powder;
sequentially carrying out binder removal and sintering treatment on the agglomerated powder to obtain sintered powder;
carrying out plasma jet treatment on the sintering powder to obtain the spherical hollow ZrTiO4And (3) ceramic powder.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
Zirconium boride, titanium boride, a dispersant, a binder and water are mixed and subjected to ball milling to obtain slurry.
In the present invention, the molar ratio of the zirconium boride to the titanium boride is preferably 1: 1. in the invention, the particle size of the zirconium boride is preferably 1-5 μm, and more preferably 2-4 μm; the particle size of the titanium boride is preferably 3 to 5 μm, and more preferably 3.5 to 4.5 μm. In the invention, the mass of the dispersant is preferably 5-10%, more preferably 6-9%, and still more preferably 7-8% of the total mass of zirconium boride and titanium boride. In the present invention, the dispersant is preferably gum arabic and/or citric acid. In the invention, the mass of the binder is preferably 5-10%, more preferably 6-9%, and still more preferably 7-8% of the total mass of the zirconium boride and the titanium boride. In the present invention, the binder is preferably polyethylene glycol (PEG) and/or Polyvinylpyrrolidone (PVG). In the invention, the solid content of the slurry is preferably 20-30%, more preferably 22-28%, and still more preferably 24-26%.
In the invention, the ball milling time is preferably 2-4 h, more preferably 2.5-3.5 h; the rotation speed of the ball mill is not particularly limited in the invention, and the rotation speed of the ball mill known to those skilled in the art can be adopted. The invention makes the materials mixed evenly by ball milling, and is beneficial to the function of the caking agent and the agglomeration of fine particles.
After the slurry is obtained, the slurry is subjected to centrifugal atomization treatment to obtain agglomerated powder.
In the invention, the inlet temperature of the centrifugal atomization treatment is preferably 200-300 ℃, more preferably 220-280 ℃, and further preferably 240-260 ℃; the outlet temperature is preferably 100-150 ℃, more preferably 110-140 ℃, and further preferably 120-130 ℃. In the present invention, the particle size of the agglomerated powder is preferably 15 to 45 μm, and more preferably 20 to 40 μm. In the present invention, the centrifugal atomizing device is preferably a spray drying device. The invention rapidly dries the slurry through centrifugal atomization treatment, and obtains agglomerated powder with the particle size range of 15-45 mu m under the action of the dispersing agent.
After the agglomerated powder is obtained, the agglomerated powder is sequentially subjected to binder removal and sintering treatment to obtain sintered powder.
In the invention, the degree of vacuum of the back bottom of the binder removal and sintering treatment is preferably 10-5～10-3Pa. The glue removing process is not particularly limited, and the glue removing process known to a person skilled in the art can be adopted, and specifically, the glue removing process is carried out for 2 hours at the temperature of 300 ℃. In the invention, the sintering treatment temperature is preferably 1400-1500 ℃, more preferably 1420-1480 ℃, and further preferably 1440-1460 ℃; the time is preferably 2 to 4 hours, and more preferably 2.5 to 3.5 hours. In the invention, the equipment for the glue discharging and sintering treatment is preferably a vacuum sintering furnace. The invention ensures that the agglomerated powder has certain structural strength through sintering treatment, is not broken in the powder feeding process, reduces the uniformity of powder components, can improve the powder fluidity and is convenient to be fed into the middle of plasma jet.
After the sintering powder is obtained, the invention carries out plasma jet treatment on the sintering powder to obtain the spherical hollow ZrTiO4And (3) ceramic powder.
In the invention, the plasma gun current in the plasma jet treatment is preferably 600-700A, more preferably 620-680A, and still more preferably 640-660A; the argon flow is preferably 20-40L/min, more preferably 23-37L/min, and still more preferably 25-35L/min; the hydrogen flow rate is preferably 10 to 12L/min, more preferably 10.5 to 11.5L/min. In the present invention, the apparatus for plasma spray treatment is preferably a plasma spray gun. In the present invention, the atmosphere of the plasma jet treatment is preferably an atmospheric atmosphere. The invention utilizes the high-temperature and high-speed jet flow characteristic generated by plasma jet to realize the rapid reaction and spheroidization of the preparation raw materials and form a hollow structure, the preparation process is rapid, and the spherical hollow ZrTiO is obtained4And (3) ceramic powder.
The invention also provides the spherical hollow ZrTiO prepared by the preparation method of the technical scheme4And (3) ceramic powder.
In the invention, the spherical hollow ZrTiO4The particle size of the ceramic powder is preferably 15-45 μm, and more preferably 20-40 μm. In the invention, the spherical hollow ZrTiO4The purity of the ceramic powder is preferably greater than 99.9%. In the invention, the spherical hollow ZrTiO4The wall thickness of the ceramic powder is preferably 6-10 μm, and more preferably 7-9 μm; the diameter of the hollow is preferably 33 μm or less.
The invention also provides the spherical hollow ZrTiO in the technical scheme4The application of the ceramic powder in the field of ceramics. In the invention, the application is preferably that the spherical hollow ZrTiO is adopted4Ceramic powder as ZrTiO4Preparing raw materials of the ceramic.
To further illustrate the present invention, the following examples are given to provide a spherical hollow ZrTiO4The ceramic powder and the preparation method and use thereof are described in detail, but they should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Carrying out mechanical ball milling on 123.8g of zirconium boride, 76.2g of titanium boride, 10g of dispersant gum arabic, 10g of binder PEG and deionized water for 2h to obtain slurry with the solid content of 20%;
pumping the obtained slurry into spray drying equipment, and controlling the inlet temperature to be 200 ℃ and the outlet temperature to be 100 ℃ under the high-speed centrifugal atomization of an atomizer to obtain agglomerated powder with the particle size range of 15-45 mu m;
putting the obtained agglomerated powder in a vacuum sintering furnace, and vacuumizing the back to 10 DEG-5Pa, firstly carrying out glue removal at the temperature of 300 ℃ for 2h, and then sintering at the temperature of 1400 ℃ for 2h to obtain sintering powder;
in the atmospheric environment, the obtained sintering powder is sent into high-temperature high-speed jet flow generated by a plasma spray gun, the current of the plasma spray gun is set to be 650A, the argon flow is set to be 30L/min, the hydrogen flow is set to be 10L/min, spheroidization is carried out, a hollow structure is formed, and the sintering powder is obtainedObtaining the spherical hollow ZrTiO4And (3) ceramic powder.
For the obtained spherical hollow ZrTiO4The ceramic powder was subjected to scanning electron microscope test, and the obtained SEM image is shown in FIG. 1. As shown in figure 1, the spherical hollow ZrTiO provided by the invention4The ceramic powder has a spherical shape.
For the obtained spherical hollow ZrTiO4The ceramic powder was subjected to scanning electron microscope test, and the obtained SEM image is shown in FIG. 2. As can be seen from figure 2, the spherical hollow ZrTiO provided by the invention4The ceramic powder has a hollow structure.
For the obtained spherical hollow ZrTiO4The particle size of the ceramic powder was counted, and the obtained particle size distribution map is shown in fig. 3. As can be seen from FIG. 3, the spherical hollow ZrTiO provided by the invention4The Dv (5) of the ceramic powder is 15.5 mu m, the Dv (95) is 43.7 mu m, the grain diameter is 15-45 mu m, and the grain diameter distribution is reasonable.
Spherical hollow ZrTiO obtained by adopting near-inductive coupling plasma-emission spectrum test (ICP)4The purity of the ceramic powder is measured, and the test result is that the spherical hollow ZrTiO4The purity of the ceramic powder is more than 99.9 percent.
Example 2
Carrying out mechanical ball milling on 185.7g of zirconium boride, 114.3g of titanium boride, 15g of dispersant citric acid, 15g of binder PVG and deionized water for 2h to obtain slurry with the solid content of 30%;
pumping the obtained slurry into spray drying equipment, and controlling the inlet temperature to be 200 ℃ and the outlet temperature to be 120 ℃ under the high-speed centrifugal atomization of an atomizer to obtain agglomerated powder with the particle size range of 15-45 mu m;
putting the obtained agglomerated powder in a vacuum sintering furnace, and vacuumizing the back to 10 DEG-5Pa, firstly carrying out glue removal at the temperature of 300 ℃ for 2h, and then sintering at the temperature of 1400 ℃ for 2h to obtain sintering powder;
in the atmospheric environment, the obtained sintering powder is sent into high-temperature high-speed jet flow generated by a plasma spray gun, the current of the plasma spray gun is set to be 700A, the argon flow is set to be 40L/min, the hydrogen flow is set to be 12L/min, spheroidization is carried out, a hollow structure is formed, and the spherical hollow ZrTiO is obtained4And (3) ceramic powder.
The obtained spherical hollow ZrTiO4Collecting and weighing ceramic powder to obtain spherical hollow ZrTiO4Dividing the quality of the ceramic powder by the preparation time to obtain the preparation speed; the spherical hollow ZrTiO4The preparation speed of the ceramic powder is 2.0kg/h, and the preparation speed is high.
Spherical hollow ZrTiO obtained by adopting near-inductive coupling plasma-emission spectrum test (ICP)4The purity of the ceramic powder is measured, and the test result is that the spherical hollow ZrTiO4The purity of the ceramic powder is more than 99.9 percent.
Example 3
Carrying out mechanical ball milling on 123.8g of zirconium boride, 76.2g of titanium boride, 10g of dispersant gum arabic, 10g of binder PVG and deionized water for 2h to obtain slurry with the solid content of 20%;
pumping the obtained slurry into spray drying equipment, and controlling the inlet temperature to be 200 ℃ and the outlet temperature to be 100 ℃ under the high-speed centrifugal atomization of an atomizer to obtain agglomerated powder with the particle size range of 15-45 mu m;
putting the obtained agglomerated powder in a vacuum sintering furnace, and vacuumizing the back to 10 DEG-5Pa, firstly carrying out glue removal at the temperature of 300 ℃ for 2h, and then sintering at the temperature of 1400 ℃ for 2h to obtain sintering powder;
in the atmospheric environment, the obtained sintering powder is sent into high-temperature high-speed jet flow generated by a plasma spray gun, the current of the plasma spray gun is set to be 680A, the argon flow is set to be 30L/min, the hydrogen flow is set to be 10L/min, spheroidization is carried out, a hollow structure is formed, and the spherical hollow ZrTiO is obtained4And (3) ceramic powder.
Spherical hollow ZrTiO obtained by adopting near-inductive coupling plasma-emission spectrum test (ICP)4The purity of the ceramic powder is measured, and the test result is that the spherical hollow ZrTiO4The purity of the ceramic powder is more than 99.9 percent.
As can be seen from the above examples, the spherical hollow ZrTiO provided by the invention4The purity of the ceramic powder is more than 99.9 percent, and the ceramic powder has extremely high purity; in addition, the preparation method provided by the invention does not need to use various chemical reagents or templates, and directly obtains the spherical ZrTiO with the hollow structure4The ceramic powder has high preparation speed and great industrial value.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. Spherical hollow ZrTiO4The preparation method of the ceramic powder is characterized by comprising the following steps:
mixing zirconium boride, titanium boride, a dispersant, a binder and water, and carrying out ball milling to obtain slurry;
carrying out centrifugal atomization treatment on the slurry to obtain agglomerated powder;
sequentially carrying out binder removal and sintering treatment on the agglomerated powder to obtain sintered powder;
carrying out plasma jet treatment on the sintering powder to obtain the spherical hollow ZrTiO4And (3) ceramic powder.
2. The method according to claim 1, wherein the molar ratio of the zirconium boride to the titanium boride is 1: 1; the mass of the dispersing agent is 5-10% of the total mass of zirconium boride and titanium boride; the mass of the binder is 5-10% of the total mass of the zirconium boride and the titanium boride; the solid content of the slurry is 20-30%.
3. The method according to claim 1, wherein the zirconium boride has a particle size of 1 to 5 μm; the particle size of the titanium boride is 3-5 mu m.
4. The preparation method according to claim 1, wherein the inlet temperature of the centrifugal atomization treatment is 200-300 ℃ and the outlet temperature is 100-150 ℃; the particle size of the agglomerated powder is 15-45 mu m.
5. The production method according to claim 1, wherein the degree of vacuum of the back surface of the de-gluing and sintering process is 10-5～10-3Pa。
6. The method according to claim 1, wherein the sintering treatment is carried out at 1400-1500 ℃ for 2-4 hours.
7. The method according to claim 1, wherein a plasma gun current in the plasma jet treatment is 600 to 700A, an argon gas flow rate is 20 to 40L/min, and a hydrogen gas flow rate is 10 to 12L/min.
8. Spherical hollow ZrTiO prepared by the preparation method of any one of claims 1 to 74And (3) ceramic powder.
9. Spherical hollow ZrTiO according to claim 84The ceramic powder is characterized in that the spherical hollow ZrTiO4The grain size of the ceramic powder is 15-45 mu m.
10. Spherical hollow ZrTiO according to claim 8 or 94The application of the ceramic powder in the field of ceramics.
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