CN114988863B - Method for preparing magnesia-alumina spinel transparent ceramic by amorphous crystallization - Google Patents
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Abstract
The invention discloses a method for preparing magnesia-alumina spinel transparent ceramics by amorphous crystallization, which is characterized by comprising the following steps of 2 O 3 MgO and Al in 0.98-1.5 2 O 3 MgO and Al are weighed separately according to the molar ratio of (2) 2 O 3 The powder is taken as ceramic powder, and the weighed ceramic powder and a crystal nucleus agent P 2 O 5 SiO of network forming body 2 Mixing absolute ethyl alcohol according to a certain proportion, and ball milling to obtain mixed slurry; drying, and then heating and melting; pouring the molten mass into a preheated cylindrical steel plate mold, and rapidly cooling to obtain a glass precursor material; and obtaining the magnesia-alumina spinel transparent ceramic by adopting an amorphous crystallization method. The invention does not need nano powder with high sintering activity and high dispersibility as raw materials, has short crystallization time and heat preservation time, and the prepared transparent ceramic has the grain size of 45-110 nm, unique nano structure, uniform grain distribution and excellent mechanical property and optical property, and can be used in the military fields of transparent armor, infrared windows and the like.
Description
Technical Field
The invention relates to the technical field of advanced functional ceramic preparation, in particular to a method for preparing magnesia-alumina spinel transparent ceramic by amorphous crystallization.
Background
The magnesia-alumina spinel is MgO-Al 2 O 3 The only stable compound in the system has high melting point, high strength, large hardness and wide transmission band (0.19-7.0 mu m), can be used for manufacturing large-size transparent ceramics, and is widely applied to army and civil fields such as transparent armor, infrared windows, infrared fairings, pressure vessel windows and the like.
At present, magnesia-alumina spinel powder with high dispersibility and high sintering activity is not easy to prepare, and common methods for preparing magnesia-alumina spinel transparent ceramics such as pressureless sintering/hot isostatic pressing, hot pressing/hot isostatic pressing and spark plasma sintering have some defects: the transparent magnesia-alumina spinel ceramic prepared by pressureless sintering generally needs longer heat preservation time (20 hours) and slower heating rate (1-4 ℃/min) to reach high density so as to eliminate pores, and has longer preparation period and efficiency influence. LiF sintering auxiliary agents are often added in the preparation of magnesia-alumina spinel transparent ceramics by hot-pressed sintering, which easily results in larger grain sizes (200-300 mu m), and the preparation of samples with complex shapes is difficult due to equipment limitations. The transparent magnesia-alumina spinel ceramic prepared by spark plasma sintering is easy to be polluted by carbon to cause the reduction of optical performance, for example, S.Benaisa et al takes pure spinel nano powder as raw material, and performs spark plasma sintering at 1300 ℃ and 73MPa to obtain the transparent magnesia-alumina spinel ceramic with the average grain size of 250nm, the transmittance at 550nm is 70%, and the sample is light black and has not very good optical performance (S.Benaissa, M.Hamidouche, M.Kolli, characterization of nanostructured MgAl) 2 O 4 ceramics fabricated by spark plasma sintering[J].Ceramics International 42(2016)8839-8846)。
In summary, based on the important application of magnesia-alumina spinel transparent ceramics in military, civil and other fields, the traditional powder sintering method cannot meet the requirements of magnesia-alumina spinel on large size, complex shape, excellent optical and mechanical properties and the like.
Disclosure of Invention
The invention aims to provide a method for preparing magnesia-alumina spinel transparent ceramics by amorphous crystallization.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the method for preparing the magnesia-alumina spinel transparent ceramic by amorphous crystallization comprises the following steps:
(1) According to the chemical formula MgO nAL 2 O 3 MgO and Al in 0.98-1.5 2 O 3 MgO and Al are weighed separately according to the molar ratio of (2) 2 O 3 The powder is taken as ceramic powder, and the weighed ceramic powder and a crystal nucleus agent P 2 O 5 SiO of network forming body 2 Mixing absolute ethyl alcohol according to a certain proportion, and then placing the mixture in a ball milling tank for ball milling to obtain mixed slurry;
(2) Drying the mixed slurry in the step (1), pouring the dried mixed slurry into an alumina crucible, heating and melting the mixed slurry at 2150-2350 ℃;
(3) Pouring the melt in the step (2) into a preheated cylindrical steel plate mold, and then rapidly cooling to obtain a glass precursor material;
(4) And (3) adopting an amorphous crystallization method for the cylindrical glass precursor material obtained in the step (3): grinding and polishing a cylindrical sample into a glass raw sheet sample, raising the temperature from room temperature to a nucleation temperature of 790-820 ℃ at a speed of 4-6 ℃/min, preserving heat for 1-3 h, raising the temperature to a crystallization temperature of 890-910 ℃ at a speed of 2-4 ℃/min, preserving heat for 1-3 h, raising the temperature to an annealing temperature of 1150-1250 ℃ at a speed of 4-6 ℃/min, preserving heat for 2-5 h, lowering the temperature to 800 ℃ at a speed of 0.5-2 ℃/min, and lowering the temperature to the room temperature at a speed of 3-5 ℃/min, thus obtaining the magnesia-alumina spinel transparent ceramic.
Preferably, the P in step (1) 2 O 5 The addition amount of the SiO accounts for 0.1 to 1.8 weight percent of the total mass of the ceramic powder body 2 The addition amount of the ceramic powder is 0.1-1.5 wt% of the total mass of the ceramic powder。
Preferably, the ball milling rotating speed in the step (1) is 160-190 r/min, and the ball milling time is 10-20 h.
Preferably, the drying temperature of the mixed slurry in the step (2) is 70 ℃, and the drying time is 6-12 h.
Preferably, in the step (2), the heating and melting temperature rise schedule is: raising the temperature to 1180-1250 ℃ at the temperature of 6-10 ℃/min, preserving heat for 1-3 h, raising the temperature to the melting temperature at the temperature of 3-6 ℃/min, and preserving heat for 1-3 h.
Preferably, in the step (3), the preheating temperature of the cylindrical steel plate mold is 500 to 700 ℃.
Preferably, in step (3), liquid nitrogen is used for rapid cooling.
Compared with the prior art, the invention has the following beneficial effects:
(1) Compared with the traditional process for preparing the magnesia-alumina spinel transparent ceramic by a powder sintering method, the magnesia-alumina spinel transparent ceramic prepared by an amorphous crystallization method does not need nano powder with high sintering activity and high dispersibility as a raw material, and is subjected to low-temperature crystallization from a glass state, so that the fluidity of a glass melt is good, uniform and fine grains can be obtained, and the grain size can reach 45-110 nm.
(2) The crystallization rate is as high as 99.8% -100%, and the existence of any glass phase cannot be detected, so that the prepared ceramic has excellent optical performance, the transmittance in a visible light band can reach 79.8% -81.3%, the highest transmittance in a middle infrared band can reach 86.2%, and the transmittance is close to the theoretical transmittance.
(3) The amorphous crystallization method can be used for preparing 50-80-2 cm large-size magnesia-alumina spinel transparent ceramics, and can be used for preparing complex shapes such as columnar shapes, missile heads and the like.
(4) Compared with the process for preparing the magnesia-alumina spinel transparent ceramic by using the amorphous crystallization method and the traditional powder sintering method, the crystallization time and the heat preservation time required by the method are shorter, only 3-5 hours are required, and the efficiency is as high as 96%.
Drawings
FIG. 1 shows the preparation of MgO nAL by amorphous crystallization 2 O 3 A physical drawing of transparent ceramics.
FIG. 2 shows the preparation of MgO nAL by amorphous crystallization 2 O 3 The transmittance curve of the transparent ceramic, the dotted line represents n=0.98, the solid line represents n=1.2, and the dotted line represents n=1.5.
FIG. 3 shows the preparation of MgO.1.2 Al by amorphous crystallization 2 O 3 Experimental determination of transparent ceramics (circles) and X-ray spectra of full spectrum fitting (lines).
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific examples.
Example 1
A method for preparing magnesia-alumina spinel transparent ceramics by adopting an amorphous crystallization method comprises the following specific steps:
(1) According to the chemical formula MgO nAL 2 O 3 N=0.98 for weighing MgO and Al, respectively 2 O 3 The powder is taken as ceramic powder, 60g of the ceramic powder is weighed, wherein the mass of MgO is 17.2454g, and Al 2 O 3 The mass of the powder is 42.7546g, and the weighed ceramic powder and 0.06g of nucleating agent P 2 O 5 0.06g of network former SiO 2 Mixing (or sintering auxiliary agent) and absolute ethyl alcohol according to a certain proportion, placing into a ball milling tank, adopting planetary ball milling, wherein the ball milling rotating speed is 160r/min, and the ball milling time is 10h.
(2) Pouring the slurry prepared in the step (1) into an alumina crucible, heating the alumina crucible to 1180 ℃ from room temperature at 6 ℃/min, preserving heat for 1h, heating the alumina crucible to 2150 ℃ at 3 ℃/min, and preserving heat for 1h.
(3) Pouring the molten mass obtained in the step (2) into a cylindrical steel plate mold preheated at 500 ℃, wherein the size of the mold used in the embodiment is
And then, rapidly cooling by utilizing liquid nitrogen to obtain the glass precursor material.
(4) And (3) grinding and polishing the cylindrical glass precursor material obtained in the step (3) into a glass raw sheet sample by adopting an amorphous crystallization method, heating the glass raw sheet sample from room temperature to 790 ℃ at the speed of 4 ℃/min, preserving heat for 1h, heating the glass raw sheet sample to 890 ℃ at the speed of 2 ℃/min, preserving heat for 1h, heating the glass raw sheet material to 1150 ℃ at the heating speed of 4 ℃/min, preserving heat for 3h, carrying out annealing treatment, cooling the glass raw sheet sample to 800 ℃ at the speed of 1 ℃/min, and cooling the glass raw sheet sample to room temperature at the speed of 3 ℃/min to obtain the magnesia-alumina spinel transparent ceramic.
FIG. 2 shows the preparation of MgO nAL by amorphous crystallization 2 O 3 The transmittance curve of transparent ceramics, wherein the dotted line represents a sample with n=0.98, can reach 80% transmittance in the infrared region.
The crystallization rate of the prepared magnesia-alumina spinel transparent ceramic can be calculated to be up to 99.8% through XRD patterns; the average grain size measured by SEM and common linear intercept analysis was 80nm, and it was observed that the grain distribution was uniform; the prepared sample is subjected to three-point test by adopting a mechanical universal tester, the bending strength can reach 281MPa, and the hardness can reach 13.32GPa.
Example 2
A method for preparing magnesia-alumina spinel transparent ceramics by adopting an amorphous crystallization method comprises the following specific steps:
(1) According to the chemical formula MgO nAL 2 O 3 N=1.2, mgO and Al are weighed separately 2 O 3 The powder is taken as ceramic powder, 60g of ceramic powder is weighed, wherein the mass of MgO is 14.8672g, and Al 2 O 3 The mass of the powder is 45.1328g, and 1.02g of the crystal nucleus agent P is added into the weighed ceramic powder 2 O 5 0.6g of network former SiO 2 Mixing (or sintering auxiliary agent) and absolute ethyl alcohol according to a certain proportion, placing into a ball milling tank, adopting planetary ball milling, wherein the ball milling rotating speed is 190r/min, and the ball milling time is 15h.
(2) Pouring the slurry prepared in the step (1) into an alumina crucible, heating the alumina crucible to 1200 ℃ from room temperature at 10 ℃/min, preserving heat for 2 hours, heating the alumina crucible to a melting temperature of 2350 ℃ at 5 ℃/min, and preserving heat for 2 hours.
(3) Pouring the melt in the step (2) into a cylindrical steel plate mould preheated at 600 ℃, and the method comprises the following steps ofThe die used in the examples was of the size
And then, rapidly cooling by utilizing liquid nitrogen to obtain the glass precursor material.
(4) And (3) grinding and polishing the cylindrical glass precursor material obtained in the step (3) into a glass raw sheet sample by adopting an amorphous crystallization method, heating the glass raw sheet sample from room temperature to 800 ℃ at a speed of 5 ℃/min, preserving heat for 2 hours, heating the glass raw sheet sample to 900 ℃ at a speed of 3 ℃/min, preserving heat for 2 hours, heating the glass raw sheet sample to 1200 ℃ at a heating speed of 5 ℃/min, preserving heat for 2 hours, carrying out annealing treatment, and then cooling the glass raw sheet sample to 800 ℃ at a speed of 0.5 ℃/min, and cooling the glass raw sheet sample to room temperature at a speed of 5 ℃/min to obtain the magnesia-alumina spinel transparent ceramic.
Preparation of MgO.1.2 Al by amorphous crystallization of sample No. 2 in FIG. 1 2 O 3 The physical image of the transparent ceramic can also clearly see the letters underneath the ceramic.
FIG. 2 shows the preparation of MgO nAL by amorphous crystallization 2 O 3 The transmittance curve of the transparent ceramic, wherein the solid line represents a sample with n=1.2, can reach 85% transmittance in the infrared region.
FIG. 3 shows the preparation of MgO.1.2 Al by amorphous crystallization 2 O 3 The X-ray spectra of the transparent ceramics are experimentally measured (circles) and fitted (lines) in full spectrum, and as can be seen from the figures, all peaks are well fitted, and the finishing result shows that the crystallization rate of the sample after amorphous crystallization is 100%, and no amorphous phase exists, which indicates that the obtained material is completely crystallized magnesia-alumina spinel transparent ceramics, but not incompletely crystallized glass ceramic material under the conditions.
The average grain size measured by SEM and common linear intercept analysis was 45nm, and it was observed that the grain distribution was uniform; the prepared sample is subjected to three-point test by adopting a mechanical universal tester, the bending strength can reach 297MPa, and the hardness can reach 13.46GPa.
Example 3
A method for preparing magnesia-alumina spinel transparent ceramics by adopting an amorphous crystallization method comprises the following specific steps:
(1) According to the chemical formula MgO nAl 2 O 3 N=1.5 weighing MgO and Al, respectively 2 O 3 The powder is taken as ceramic powder, 60g of ceramic powder is weighed, wherein the mass of MgO is 12.5139g, and Al 2 O 3 The mass of the powder is 47.4861g, and 1.08g of the crystal nucleus agent P is added into the weighed ceramic powder 2 O 5 0.9g of network former SiO 2 (can also be used as sintering auxiliary agent) and absolute ethyl alcohol are mixed according to a certain proportion and then are placed in a ball milling tank, planetary ball milling is adopted, the ball milling rotating speed is 180r/min, and the ball milling time is 20h.
(2) Pouring the slurry prepared in the step (1) into an alumina crucible, heating the alumina crucible to 1250 ℃ from room temperature at 8 ℃/min, preserving heat for 3 hours, heating the alumina crucible to 2250 ℃ at 6 ℃/min, and preserving heat for 3 hours.
(3) Pouring the melt in the step (2) into a 700 ℃ preheated cylindrical steel plate die, wherein the die used in the invention has the size of
And then rapidly cooling by utilizing liquid nitrogen to obtain the glass precursor material.
(4) And (3) grinding and polishing the cylindrical glass precursor material obtained in the step (3) into a glass raw sheet sample by adopting an amorphous crystallization method, heating the glass raw sheet sample from room temperature to 820 ℃ at the speed of 6 ℃/min, preserving heat for 3 hours, heating the glass raw sheet sample to 910 ℃ at the speed of 4 ℃/min, preserving heat for 3 hours, heating the glass raw sheet sample to 1250 ℃ at the heating speed of 6 ℃/min, preserving heat for 5 hours, carrying out annealing treatment, cooling the glass raw sheet sample to 800 ℃ at the speed of 2 ℃/min, and cooling the glass raw sheet sample to room temperature at the speed of 4 ℃/min to obtain the magnesia-alumina spinel transparent ceramic.
Preparation of MgO.1.5 Al by amorphous crystallization of sample No. 3 in FIG. 1 2 O 3 The physical image of the transparent ceramic can also clearly see the letters underneath the ceramic.
FIG. 2 shows the preparation of MgO nAL by amorphous crystallization 2 O 3 The transmittance curve of transparent ceramics, wherein the dotted line represents a sample with n=1.5, can reach a transmittance of 82% in the infrared region.
The crystallization rate of the prepared magnesia-alumina spinel transparent ceramic can be calculated to be up to 99.8% through XRD patterns; the average grain size measured by SEM and common linear intercept analysis was 80nm, and it was observed that the grain distribution was uniform; the prepared sample is subjected to three-point test by a mechanical universal tester, the bending strength can reach 289MPa, and the hardness can reach 13.39GPa.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (6)
1. The method for preparing the magnesia-alumina spinel transparent ceramic by amorphous crystallization is characterized by comprising the following steps of:
(1) According to the chemical formula MgO nAL 2 O 3 MgO and Al in 0.98-1.5 2 O 3 MgO and Al are weighed separately according to the molar ratio of (2) 2 O 3 The powder is taken as ceramic powder, and the weighed ceramic powder and a crystal nucleus agent P 2 O 5 SiO of network forming body 2 Mixing absolute ethyl alcohol according to a certain proportion, and then placing the mixture in a ball milling tank for ball milling to obtain mixed slurry; wherein said P 2 O 5 The addition amount of the SiO accounts for 0.1-1.8wt% of the total mass of the ceramic powder body 2 The addition amount of the ceramic powder is 0.1-1.5wt.% of the total mass of the ceramic powder;
(2) Drying the mixed slurry in the step (1), and pouring the dried mixed slurry into an alumina crucible for heating and melting at 2150-2350 ℃;
(3) Pouring the melt in the step (2) into a preheated cylindrical steel plate mold, and then rapidly cooling to obtain a glass precursor material;
(4) And (3) adopting an amorphous crystallization method for the cylindrical glass precursor material obtained in the step (3): grinding and polishing a cylindrical sample into a glass raw sheet sample, raising the temperature from room temperature to a nucleation temperature of 790-820 ℃ at a speed of 4-6 ℃/min, preserving heat for 1-3 h, raising the temperature to a crystallization temperature of 890-910 ℃ at a speed of 2-4 ℃/min, preserving heat for 1-3 h, raising the temperature to an annealing temperature of 1150-1250 ℃ at a speed of 4-6 ℃/min, preserving heat for 2-5 h, lowering the temperature to 800 ℃ at a speed of 0.5-2 ℃/min, and lowering the temperature to the room temperature at a speed of 3-5 ℃/min, thus obtaining the magnesia-alumina spinel transparent ceramic.
2. The method for preparing magnesia-alumina spinel transparent ceramics by amorphous crystallization according to claim 1, wherein the ball milling rotation speed in the step (1) is 160-190 r/min, and the ball milling time is 10-20 h.
3. The method for preparing magnesia-alumina spinel transparent ceramics by amorphous crystallization according to claim 1, wherein the drying temperature of the mixed slurry in the step (2) is 70 ℃ and the drying time is 6-12 h.
4. The method for preparing magnesia-alumina spinel transparent ceramics by amorphous crystallization according to claim 1, wherein in the step (2), the heating and melting temperature rise schedule is: and (3) raising the temperature to 1180-1250 ℃ at the room temperature at the heating rate of 6-10 ℃/min, preserving heat for 1-3 h, raising the temperature to the melting temperature at the heating rate of 3-6 ℃/min, and preserving heat for 1-3 h.
5. The method for preparing magnesia-alumina spinel transparent ceramics by amorphous crystallization according to claim 1, wherein in the step (3), the preheating temperature of the cylindrical steel plate mold is 500-700 ℃.
6. The method for preparing magnesia-alumina spinel transparent ceramics by amorphous crystallization according to claim 1, wherein in the step (3), liquid nitrogen is used for rapid cooling.
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| DE102009055987B4 (en) * | 2009-11-20 | 2018-10-18 | Schott Ag | Spinel opto-ceramics |
| CN111348835A (en) * | 2014-11-19 | 2020-06-30 | 成都光明光电股份有限公司 | High-hardness transparent glass ceramics and preparation method thereof |
| CN105601115A (en) * | 2014-11-19 | 2016-05-25 | 成都光明光电股份有限公司 | Microcrystalline glass by taking spinel as main component and preparation method thereof |
| CN104478219B (en) * | 2014-12-31 | 2017-02-22 | 海南大学 | Nano-scale spinel glass ceramic and preparation method thereof |
| CN109809696A (en) * | 2018-12-19 | 2019-05-28 | 温州市康尔微晶器皿有限公司 | A kind of magnalium silicon spinel devitrified glass |
| CN111018354B (en) * | 2020-01-06 | 2021-04-02 | 武汉理工大学 | Spinel transparent glass-ceramic with low melting temperature and preparation and performance enhancement method thereof |
| CN111592224A (en) * | 2020-04-29 | 2020-08-28 | 深圳精匠云创科技有限公司 | Magnesium aluminum silicate nanocrystalline transparent ceramic, preparation method and product thereof |
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