CN115073181B - High-sintering-activity pure-phase MgAlON fine powder and preparation method and application thereof - Google Patents
High-sintering-activity pure-phase MgAlON fine powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to high-sintering-activity pure-phase MgAlON fine powder and a preparation method and application thereof, belonging to the technical field of ceramic powder preparation. A method for preparing pure-phase MgAlON fine powder with high sintering activity comprises mixing MgAl with water 2 O 4 、γ‑Al 2 O 3 Ball-milling and mixing 15-20 wt.%, 65-75 wt.% and 10-15 wt.% of AlN powder, and performing a two-step heating process on the obtained mixed powder in a normal-pressure nitrogen atmosphere to obtain pure-phase MgAlON powder, wherein the two-step heating process specifically comprises the following steps: keeping the temperature at 1500-1600 ℃ for 20-60 min, then continuing to heat to 1650-1750 ℃ and keeping the temperature for 40-120 min; and ball-milling the obtained pure-phase MgAlON powder to obtain pure-phase MgAlON fine powder with high sintering activity. The method uses nano MgAl 2 O 4 The powder is used as Mg source and is mixed with nano gamma-Al 2 O 3 And the MgAlON powder is synthesized by two-step heating normal-pressure high-temperature solid-phase reaction with the micron AlN powder, and the method is simple and easy to implement and convenient to operate.
Description
Technical Field
The invention relates to high-sintering-activity pure-phase MgAlON fine powder and a preparation method and application thereof, belonging to the technical field of ceramic powder preparation.
Background
The MgAlON transparent ceramic has high transmittance, wide wave-transmitting range, close infrared cut-off wavelength with sapphire, good high-temperature thermal stability and excellent high-temperature mechanical property, and the characteristics make the MgAlON transparent ceramic become a very potential window material, can be widely used in the fields of aerospace, ground armor, deep sea detection and the like, is an ideal material for protecting, observing and monitoring windows in advanced equipment, and can effectively improve the performance and reliability of the equipment.
The preparation of the MgAlON transparent ceramic generally takes MgAlON powder as a raw material, and high density is obtained through high-temperature sintering, so that the light transmission is realized. MgAlON powder is used as a key raw material for preparing transparent ceramics by sintering, and the current main synthesis method comprises three types: one is MgO and Al 2 O 3 A direct solid-phase reaction method using AlN powder as a raw material; secondly, carbon powder and Al 2 O 3 And a carbothermal reduction nitriding method using MgO powder as a raw material; and thirdly, an aluminothermic reduction nitridation method which takes Al powder, alN and MgO powder as raw materials. The solid-phase reaction method is widely concerned due to the fact that raw materials are easy to obtain, the use is convenient and safe, the process is simple, the component controllability is strong, and the purity of the synthesized powder is high, so that the method is an effective means for preparing the MgAlON powder, and the powder synthesized by the method can be used for preparing the MgAlON transparent ceramic with good light transmission.
For preparing MgAlON transparent ceramics, mgO is generally selected as a Mg source when synthesizing MgAlON powder by a solid-phase reaction method (Xiao Liu, et al, J.am.Ceram.Soc.,97 (2014) 63-66, xiao Zong, et al, scr.Mater.178 (2020) 428-432, kai Li, et al, J.Eur.Ceram.Soc.,37 (2017) 4229-4233. In order to obtain a uniform fine powder of MgAlON, liu et al have tried to use MgAl of 1 to 1.5 μm 2 O 4 Powder as Mg source, with alpha-Al 2 O 3 And AlN is subjected to solid-phase reaction to synthesize MgAlON powder, a gas pressure sintering method is adopted, the temperature is kept at 1800 ℃ for 2h under the nitrogen condition of 0.48MPa, and pure-phase MgAlON powder is prepared, and the median particle size of the powder is 3.4 mu m (Lihong Liu, et al, J.Eur.Ceram.Soc.,39 (2019) 928-933). The MgAlON transparent ceramic with the transmittance of 67.7 percent is obtained by utilizing the prepared MgAlON powder and adopting a discharge plasma sintering technology and preserving the temperature for 5min at 1800 ℃ under the pressure of 80 MPa. As can be seen, mgAl 2 O 4 The MgAlON powder can be used as an Mg source to synthesize pure-phase MgAlON powder, but the wide application of the MgAlON powder is greatly limited due to the high requirement on equipment and the harsh requirement on equipment and process of air pressure sintering.
When the ceramic is prepared by adopting a powder densification sintering method, the sintering activity of the ceramic powder has great influence on the process requirement and the product performance, the excellent sintering activity can effectively reduce the temperature of the ceramic densification sintering, shorten the heat preservation time, reduce the dependence on external fields (such as plasma, microwave, gas pressure and mechanical pressure) and the like, and can improve the performance of the ceramic under the same process conditions. Therefore, a preparation technology of the high-sintering activity MgAlON powder, which is simple and easy to implement, low in equipment requirement, good in energy-saving effect, high in efficiency and low in cost, is needed to be explored so as to realize the preparation of the high-activity pure-phase MgAlON powder under the conditions of low equipment requirement, low temperature and short heat preservation time, and further promote the research and development and wide application of the MgAlON transparent ceramic.
Disclosure of Invention
The invention aims to provide a method for preparing a nano MgAl 2 O 4 The powder is used as Mg source and is mixed with nano gamma-Al 2 O 3 And micron AlN in normal pressure nitrogen atmosphere, through the method of preparing pure phase MgAlON fine powder of low temperature solid phase reaction of two-step heating process, moreover, mgAlON powder prepared has higher sintering activity. The method uses MgAl 2 O 4 、γ-Al 2 O 3 And AlN mixed powder is used as a raw material, the heat preservation is carried out for 20-60 min at 1500-1600 ℃ in a nitrogen environment at normal pressure, then the temperature is continuously raised to 1650-1750 ℃ and is preserved for 40-120 min, and MgAlON powder is synthesized through solid phase reaction. The synthesized pure-phase MgAlON powder has small primary particle size, high sintering activity fine powder with small particle size can be obtained by common ball milling, the relative density of the ceramic obtained by sintering at the temperature of 1880 ℃ without heat preservation reaches 99.03 percent, and the transmittance is 68.3 percent.
A method for preparing pure-phase MgAlON fine powder with high sintering activity comprises mixing MgAl with water 2 O 4 、γ-Al 2 O 3 Ball-milling and mixing the AlN powder with 15-20 wt.%, 65-75 wt.% and 10-15 wt.% of AlN powder, and heating the obtained mixed powder in a normal-pressure nitrogen atmosphere by adopting a two-step heating process to obtain a pure phaseThe MgAlON powder is prepared by a two-step heating process which comprises the following steps: keeping the temperature at 1500-1600 ℃ for 20-60 min, then continuing to heat to 1650-1750 ℃ and keeping the temperature for 40-120 min; and performing ball milling on the obtained pure-phase MgAlON powder to obtain pure-phase MgAlON fine powder with high sintering activity.
In the above technical scheme, mgAl 2 O 4 、γ-Al 2 O 3 And the sum of the mass fractions of the AlN powder and the AlN powder is 100 percent. Preferably, mgAl 2 O 4 17.40wt.％、γ-Al 2 O 3 70.03wt.％、AlN 12.57wt.％。
In the preparation method of the high-sintering activity pure-phase MgAlON fine powder, the MgAl is 2 O 4 Is nano powder with average grain size not more than 120nm and specific surface area not less than 15m 2 /g。
In the preparation method of the high-sintering activity pure-phase MgAlON fine powder, gamma-Al 2 O 3 Is nano powder with average grain size not more than 40nm and specific surface area not less than 120m 2 /g。
In the preparation method of the high-sintering activity pure-phase MgAlON fine powder, the median particle size of AlN powder is 1-2 mu m.
Preferably, the MgAl is ball-milled 2 O 4 、γ-Al 2 O 3 And drying the AlN mixed powder, sieving the AlN mixed powder by a sieve of 60 to 80 meshes, and then carrying out a two-step heating process.
Further, the ball milling process comprises the following steps: taking anhydrous ethanol as a medium, adding MgAl 2 O 4 、γ-Al 2 O 3 And ball milling AlN powder in a ball mill at 170rpm for 20-30 hr.
Preferably, mgAl is added 2 O 4 、γ-Al 2 O 3 And AlN mixed powder is filled into a graphite crucible, pure-phase MgAlON powder is prepared by adopting a two-step heating process under the nitrogen atmosphere of normal pressure in an atmosphere sintering furnace, wherein the heating rate of the two-step heating process is 10-30 ℃/min, and the pure-phase MgAlON powder is cooled along with the furnace after the second-step heat preservation is finished.
Preferably, the pure-phase MgAlON powder is ball-milled for 20 to 40 hours on a planetary ball mill at 170 to 210rpm to obtain the pure-phase MgAlON fine powder with high sintering activity.
It is another object of the present invention to provide a pure phase MgAlON fine powder with high sintering activity prepared by the above method.
D of high-sintering activity pure-phase MgAlON fine powder prepared by the method 50 =0.99 μm, particle size distribution range of 0.11-3.55 μm, specific surface area greater than or equal to 5m 2 /g。
It is still another object of the present invention to provide a method for preparing MgAlON ceramic using the above-mentioned high sintering activity pure phase MgAlON fine powder.
A preparation method of MgAlON ceramic comprises the step of adding 0.5wt.% of Y into MgAlON fine powder 2 O 3 After dry pressing and forming, the MgAlON ceramic is prepared by adopting a pressureless sintering method and heating to 1850-1900 ℃ in nitrogen and preserving the temperature for 0-60 min.
In the preparation method, the formed MgAlON blank is subjected to pressureless sintering, and the MgAlON ceramic block can be directly obtained after the temperature is raised to the preset sintering temperature and the heat is preserved for a period of time or not preserved.
Further, it is preferable that the sintering temperature is raised to 1880 ℃ without heat preservation, and the obtained MgAlON ceramic has a relative density of 99.03% and a transmittance of 68.3%.
The beneficial effects of the invention are as follows: the invention utilizes nano MgAl 2 O 4 The powder is used as Mg source and is mixed with nano gamma-Al 2 O 3 And the micron AlN powder is subjected to solid phase reaction at normal pressure and low temperature to synthesize pure-phase MgAlON powder with small primary particle size and high sintering activity, and a two-step heating process is adopted in the heating process of powder synthesis to inhibit crystal grains from growing, so that fine-particle pure-phase MgAlON powder with high sintering activity can be obtained at a lower temperature. Raw material MgAl 2 O 4 Has similar lattice structure with MgAlON product and small granularity, and is easier to form Al-rich Al by solid solution at lower temperature 2 O 3 The MgAlON powder can effectively prevent Al under high temperature condition by first-step heat preservation under lower temperature condition 2 O 3 The particles are aggregated and grown, and the difficulty of obtaining pure-phase MgAlON powder by further solid solution of AlN under the high-temperature condition is reduced, so that the pure-phase MgAlO with high sintering activity and smaller particles can be prepared at lower temperatureAnd (3) N powder. 0.5wt.% Y is added into the prepared MgAlON powder 2 O 3 As a sintering aid, the MgAlON transparent ceramic with the relative density of 99.03% and the transmittance of 68.3% is obtained by a pressureless sintering method under the condition of no heat preservation at 1880 ℃. Indicating that the nano MgAl is used 2 O 4 The powder is used as Mg source and is mixed with nano gamma-Al 2 O 3 The MgAlON powder prepared by the solid-phase reaction with the micron AlN powder has very good sintering activity and is beneficial to preparing high-density MgAlON transparent ceramics. In addition, the method has the advantages of simple and easy process, low requirement on equipment, convenient operation, high safety, high efficiency, low cost, good energy-saving effect and easy realization of industrialization, and the synthesis temperature of the MgAlON powder is effectively reduced by two-step heating.
Drawings
FIG. 1 shows MgAl as a raw material in example 1 2 O 4 Powder, gamma-Al 2 O 3 XRD patterns of the powder and the AlN powder;
FIG. 2 shows MgAl as a raw material in example 1 2 O 4 Powder, gamma-Al 2 O 3 SEM images of the powder and AlN powder;
FIG. 3 shows MgAl obtained in example 1 2 O 4 、γ-Al 2 O 3 SEM image of AlN mixed powder;
FIG. 4 is an XRD spectrum of MgAlON powder obtained in example 1, comparative example 1 and comparative example 2;
FIG. 5 is an SEM image of MgAlON powder obtained in example 1 and comparative example 2;
FIG. 6 is an SEM photograph of MgAlON powder after ball milling in example 1;
FIG. 7 is a graph showing the particle size distribution of MgAlON powder after ball milling in example 1;
FIG. 8 is the relative density of MgAlON ceramic when heated to different temperatures for example 1;
FIG. 9 is an SEM photograph of MgAlON ceramic of example 1 when heated to different temperatures;
FIG. 10 is an XRD pattern of MgAlON ceramic in example 1 under non-soak conditions at 1880 ℃;
FIG. 11 is a graph showing the transmittance of MgAlON ceramic in example 1 under conditions where the temperature is not maintained at 1880 ℃.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
One of the specific implementation modes is as follows:
a preparation method of high sintering activity pure-phase MgAlON fine powder comprises the following process steps:
(1) According to MgAl 2 O 4 17.40wt.％、γ-Al 2 O 3 70.03wt.% and AlN 12.57wt.% are weighed, wherein the MgAl is 2 O 4 And gamma-Al 2 O 3 Are all nano powder, wherein MgAl 2 O 4 The average particle diameter of the powder is less than or equal to 120nm, and the specific surface area is more than or equal to 15m 2 /g；γ-Al 2 O 3 Is nano powder with average grain size not more than 40nm and specific surface area not less than 120m 2 (ii)/g; the AlN median particle size is 1-2 mu m.
(2) Taking absolute ethyl alcohol as a medium, namely weighing MgAl 2 O 4 、γ-Al 2 O 3 Ball-milling and mixing AlN powder on a planetary ball mill for 20-30 h at 170 rpm;
(3) Drying the slurry after ball milling and mixing, and sieving the dried slurry with a 60-80 mesh sieve;
(4) Drying and granulating to obtain MgAl 2 O 4 、γ-Al 2 O 3 Putting the AlN mixed powder into a crucible, placing the crucible into an atmosphere sintering furnace, keeping the temperature at 1500-1600 ℃ for 20-60 min at the heating rate of 10-30 ℃/min in the nitrogen atmosphere at normal pressure, then continuously heating to 1650-1750 ℃ and keeping the temperature for 40-120 min, turning off a power supply after the temperature is kept, and cooling along with the furnace;
(5) Ball-milling the obtained pure-phase MgAlON powder on a planetary ball mill for 20-40 h at 170-210 rpm to obtain high-sintering activity pure-phase MgAlON fine powder, and D 50 =0.99 μm, particle size distribution range of 0.11-3.55 μm, and ratio tableThe area is more than or equal to 5m 2 /g。
Example 1
With pure phase nano MgAl 2 O 4 (average particle diameter: 101nm, specific surface area: 17 m) 2 G) nano gamma-Al 2 O 3 (average particle diameter 14nm, specific surface area 128 m) 2 Powder/g) and AlN powder (median particle size 1.68 μm) as raw materials (MgAl) 2 O 4 、γ-Al 2 O 3 The phase composition of AlN powder is shown in figure 1, and the appearance is shown in figure 2), according to MgAl 2 O 4 17.40wt.％、γ-Al 2 O 3 70.03wt.% and AlN 12.57wt.% are weighed to total 20g, and 100ml of absolute ethyl alcohol is added to prepare MgAl 2 O 4 、γ-Al 2 O 3 Ball-milling the mixed slurry with AlN for 24 hours on a planetary ball mill at 170rpm, drying the obtained mixed slurry, sieving the dried mixed slurry with a 60-mesh sieve, and MgAl 2 O 4 、γ-Al 2 O 3 The shape of the AlN mixed powder is shown in FIG. 3, and it can be seen that the AlN mixed powder is mainly composed of nanoparticles with small size.
MgAl is added 2 O 4 、γ-Al 2 O 3 And putting the AlN mixed powder into a graphite crucible, putting the graphite crucible into an atmosphere sintering furnace, firstly heating to 1550 ℃ at a speed of 20 ℃/min in a nitrogen environment at normal pressure, preserving heat for 30min, then continuously heating to 1700 ℃ and preserving heat for 60min, and turning off a power supply to cool along with the furnace. Fig. 4 is an XRD pattern of the synthesized powder, showing that a pure phase of MgAlON powder is obtained, and fig. 5 is an SEM image thereof, and it can be seen that the synthesized powder is mainly composed of particles having a small size.
Adding 20g of synthesized MgAlON powder into 100ml of absolute ethyl alcohol, and ball-milling for 24h on a planetary ball mill at 170rpm to obtain MgAlON fine powder. The morphology of the MgAlON fine powder after ball milling is shown in figure 6, the particle size of the MgAlON fine powder is smaller, figure 7 is the powder particle size distribution of the MgAlON fine powder measured by a laser particle sizer, which shows that the MgAlON fine powder after ball milling is D 50 =0.99 μm, particle size distribution range of 0.11-3.55 μm, specific surface area of 6.57m measured by gas adsorption method 2 /g。
0.5wt.% Y was added to MgAlON fine powder 2 O 3 As sintering aid, after dry pressing and forming, the mixture is raised in nitrogen by a pressureless sintering methodThe temperature is 1400 ℃, 1500 ℃, 1600 ℃, 1700 ℃, 1800 ℃ and 1880 ℃ (without heat preservation). FIG. 8 is the results of the relative density tests under different temperature conditions, FIG. 9 is the SEM image of the sample, and it can be seen that when the green body is heated to 1880 ℃, no obvious large pores exist in the fracture, and the relative density of the ceramic reaches 99.03%, indicating that the prepared MgAlON fine powder has good densification sintering capability. FIG. 10 is an XRD pattern of the ceramic at elevated temperature to 1880 ℃ showing that the ceramic produced is monophasic MgAlON. FIG. 11 is a graph showing the transmittance of a ceramic at 1880 ℃ and showing a transmittance of 68.3%.
Comparative example 1
The difference between the comparative example 1 and the example 1 is that the synthesis process of the MgAlON powder adopts a one-step heating method, namely: heating to 1700 deg.C at 20 deg.C/min, and maintaining for 60min, wherein the XRD pattern of the synthesized powder is shown in figure 4, and contains residual Al in addition to MgAlON as main phase 2 O 3 。
Comparative example 2
The difference between the comparative example 2 and the example 1 is that the synthesis process of the MgAlON powder adopts a one-step heating method, namely: directly heating to 1750 ℃ at the speed of 20 ℃/min, and preserving the temperature for 60min, wherein the XRD pattern of the synthesized powder is shown in figure 4, the synthesized powder is pure-phase MgAlON, the morphology of the synthesized powder is shown in figure 5, and the particle size is larger.
Claims (9)
1. A preparation method of pure-phase MgAlON fine powder with high sintering activity is characterized by comprising the following steps: mgAl is added 2 O 4 、γ-Al 2 O 3 Ball-milling and mixing 15-20 wt.%, 65-75 wt.% and 10-15 wt.% of AlN powder, and heating the obtained mixed powder in a normal-pressure nitrogen atmosphere by a two-step heating process to obtain pure-phase MgAlON powder, wherein the two-step heating process specifically comprises the following steps: keeping the temperature at 1500-1600 ℃ for 20-60 min, then continuing to heat to 1650-1750 ℃ and keeping the temperature for 40-120 min; and performing ball milling on the obtained pure-phase MgAlON powder to obtain pure-phase MgAlON fine powder with high sintering activity.
2. The method of claim 1, wherein: mgAl after ball milling 2 O 4 、γ-Al 2 O 3 Drying and filtering the mixed powder with AlNAfter 60-80 mesh sieve, two-step heating process is carried out.
3. The method according to claim 1 or 2, characterized in that: the ball milling process comprises the following steps: taking anhydrous ethanol as a medium, adding MgAl 2 O 4 、γ-Al 2 O 3 And ball milling AlN powder in a ball mill at 170rpm for 20-30 hr.
4. The method of claim 1, wherein: the MgAl 2 O 4 Is nano powder with average particle size not greater than 120nm and specific surface area not less than 15m 2 /g；γ-Al 2 O 3 Is nano powder with average grain size not more than 40nm and specific surface area not less than 120m 2 (ii)/g; the median particle size of the AlN powder is 1-2 mu m.
5. The method of claim 1, wherein: mgAl is added 2 O 4 、γ-Al 2 O 3 And AlN mixed powder is filled into a graphite crucible, pure-phase MgAlON powder is prepared by adopting a two-step heating process under the nitrogen atmosphere of normal pressure in an atmosphere sintering furnace, wherein the heating rate of the two-step heating process is 10-30 ℃/min, and the pure-phase MgAlON powder is cooled along with the furnace after the second-step heat preservation is finished.
6. The method of claim 1, wherein: ball-milling the obtained pure-phase MgAlON powder on a planetary ball mill for 20-40 h at 170-210 rpm to obtain pure-phase MgAlON fine powder with high sintering activity.
7. A fine powder of MgAlON with high sintering activity and pure phase prepared by the method of any one of claims 1 to 6.
8. MgAlON fine powder according to claim 7, characterized in that: d of the high-sintering activity pure-phase MgAlON fine powder 50 =0.99 μm, particle size distribution range of 0.11-3.55 μm, specific surface area greater than or equal to 5m 2 /g。
9. MgAlON ceramicThe preparation method is characterized by comprising the following steps: adding 0.5wt.% Y to the MgAlON fine powder of claim 7 2 O 3 After dry pressing and forming, the MgAlON ceramic is prepared by adopting a pressureless sintering method and heating to 1850-1900 ℃ in nitrogen and preserving the temperature for 0-60 min.
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