CN109053192A - A kind of preparation method of MgAlON transparent ceramic powder - Google Patents

A kind of preparation method of MgAlON transparent ceramic powder Download PDF

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CN109053192A
CN109053192A CN201811157930.2A CN201811157930A CN109053192A CN 109053192 A CN109053192 A CN 109053192A CN 201811157930 A CN201811157930 A CN 201811157930A CN 109053192 A CN109053192 A CN 109053192A
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transparent ceramic
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mgalon
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CN109053192B (en
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谢忠祥
刘海艳
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Hunan Institute of Technology
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Abstract

A kind of preparation method of MgAlON transparent ceramic powder, comprising the following steps: (1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3 powder and MgO powder, obtain mixed powder, spare；(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling obtains slurry；(3) slurry is dry: taking slurry obtained by step (2) dry, obtains dry powder；(4) reaction synthesis: dry powder obtained by step (3) is taken, it is fitted into crucible, it is placed in high temperature sintering furnace together again, it is passed through flowing nitrogen, with the heating rate of 5 DEG C~15 DEG C/min, 1500 DEG C~1700 DEG C heat preservation 1h~3h are warming up to, then natural cooling, obtains MgAlON transparent ceramic powder.MgAlON transparent ceramic powder made from this method, purity is high, granularity is thin, is suitble to production crystalline ceramics.

Description

A kind of preparation method of MgAlON transparent ceramic powder
Technical field
The present invention relates to a kind of preparation methods of MgAlON transparent ceramic powder, belong to optical material field.
Background technique
MgAlON is that one kind consolidates AlON structural material by MgO, and the MgAlON crystalline ceramics for being fabricated to block is one The new material of kind structure and function integration, it has and AlON, MgAl2O4Deng performance as typical spinel structure ceramic-like, Such as: wide electromagnetic wave through range (0.2 μm~6.5 μm), optical isotropy, excellent mechanical property (bending strength is high, Hardness is big), etc., it is expected to it is applied to infrared window, antenna house, detector optical window, the first-class field of see-through look.
Report about material preparation is there are mainly two types of method: first is that reaction sintering, usually using AlN (or Al、 N2)、Al2O3, MgO be raw material, by reaction-sintered after mixing, settle at one go and obtain MgAlON crystalline ceramics, thus can also To be referred to as one-step method (J.Eur.Ceram.Soc, 15 (2015), 249-254)；Second is that first synthesizing MgAlON powder, then pass through Sintering, obtains MgAlON crystalline ceramics, also referred to as two-step method, and this respect can refer to the document (J.Am. of Liu et al. people Ceram.Soc,97(2014),63-66).Reaction sintering (one-step method) technical difficult points are: sintering is usually synchronous with reaction It carries out, process is complex, is easy to produce the second phase；Moreover, for the reaction process of this kind of material, there are also volume expansion generations The problem of secondary blowhole, these all can cause to seriously affect to optical property.In contrast, these problems are not present in two-step method, It is thus the preferred method for obtaining MgAlON crystalline ceramics, in the preparation of MgAlON crystalline ceramics large scale, optical transmittance etc. Aspect general performance is more preferable.
The premise of two-step method is to prepare high performance MgAlON transparent ceramic powder.Currently, about the transparent pottery of MgAlON Porcelain raw powder's production technology mainly has: (1) with AlN, Al2O3, MgO be raw material, pass through solid reaction process obtain (referenced patent CN 200910272607.4)；(2) with C, Al2O3、N2, MgO be raw material, pass through carbothermal reduction-nitridation reaction obtain (reference Ceram.Inter.,44(2018),4512-4515).Both methods is the current master for obtaining MgAlON transparent ceramic powder Want method.By the MgAlON transparent ceramic powder sintering densification of acquisition, MgAlON crystalline ceramics can be obtained.It is worth mentioning It is solid reaction process therein, since the market price of raw material AlN of use is expensive, virtually improves preparation cost；And carbon is warm Reduction method is due to using C for raw material, and remaining C is generally difficult to exclude in product, and follow-up link is usually required in air or oxygen Middle calcination processing also inevitably causes the oxidation of MgAlON although this link can exclude a part remnants C.
For two methods above-mentioned some problems existing for MgAlON transparent ceramic powder preparation process, there is text It offers report and proposes direct nitridation method (also referred to as Al thermal reduction).Al has lower fusing point, thus can be at a lower temperature Nitridation.For example, Su et al. (J.Eur.Ceram.Soc, 35 (2015), 1173-1178) uses Al, N2、Al2O3For the straight of raw material The powder for connecing nitriding, having synthesized AlON powder, and obtained for the first time using this method, it is excellent to prepare optical transmittance AlON crystalline ceramics.For another example, Yan et al. (Ceram.Int.44 (2018), 3856-3861) proposes that this method is used to prepare MgAlON, but be mainly used for refractory material, and it is strictly upper for his this method belong to step sintering and obtain MgAlON, pottery The porosity is usually higher in porcelain, is difficult to reach optical clear grade in performance.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of powder purity that raw material cost is low, synthesizes height, contain C Low, the preparation method of the excellent MgAlON transparent ceramic powder of optical transmittance is measured, the powder of this method preparation may be used as The raw material of MgAlON crystalline ceramics.
The technical solution adopted by the present invention to solve the technical problems is: a kind of preparation side of MgAlON transparent ceramic powder Method, comprising the following steps:
(1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3Powder and MgO powder, obtain mixed powder, spare；
The ratio are as follows: Al powder, γ-Al2O3Powder, MgO powder mass fraction be respectively 4wt%~9wt%, 78wt% ~88wt%, 7wt%~16wt%；
(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling obtains slurry；
(3) slurry is dry: taking slurry obtained by step (2) dry, obtains dry powder；
(4) reaction synthesis: dry powder obtained by step (3) is taken, is fitted into crucible, then be placed in high temperature sintering furnace together In, it is passed through flowing nitrogen, with the heating rate of 5 DEG C~15 DEG C/min, is warming up to 1500 DEG C~1700 DEG C heat preservation 1h~3h, then Natural cooling obtains MgAlON transparent ceramic powder.
Further, in step (1), average particle size≤2.5 μm of the Al powder, purity >=99wt%；γ-Al2O3Powder Average particle size≤100nm, purity >=99.5wt%；MgO powder average particle size≤100nm, purity >=99.5wt%.
Further, in step (2), rotational speed of ball-mill is 60r~120r/m；Ball-milling Time >=16h.
Further, in step (2), the abrading-ball that ball milling is selected is alumina balls or zirconia ball, purity >=99wt%；
Further, in step (2), the mass ratio of abrading-ball and mixed powder is 5:1~10:1.
Further, it is to avoid the oxidation of Al powder in raw material as far as possible in step (3), slurry is placed in vacuum chamber to (air pressure is not Higher than 20Pa), drying temperature >=60 DEG C make the dehydrated alcohol in slurry sufficiently volatilize.
Further, in step (4), the crucible is aluminium oxide or boron nitride crucible, purity >=97wt%；
Further, in step (4), the flowing nitrogen, air pressure absolute value be 0.1MPa~0.3MPa, purity >= 99.99 vol%, flow rate are 0.1L~1.0L/min.
Beneficial effects of the present invention:
1) it in the case where expensive AlN powder or fusing point height can not be selected, be not easy the C powder excluded completely, selects Price is low, low-melting Al powder as raw material passes through direct nitridation method, it is also possible to obtain MgAlON powder, and raw material at This low, synthesis powder purity is high, C content is low, is very suitable to promote and apply；
2) the MgAlON powder obtained can be used for preparing transparent MgAlON ceramics, and optical transmittance is excellent, for this The preparation of class material provides new method.
Detailed description of the invention
Fig. 1 is the XRD spectrum for the MgAlON powder that the embodiment of the present invention 1,3,5 synthesizes；
Fig. 2 is to use the transmitance of MgAlON crystalline ceramics made from the MgAlON powder of the synthesis of the embodiment of the present invention 3 bent Line.
Specific embodiment
For a better understanding of the present invention, the content that the present invention is further explained with reference to the accompanying drawings and examples, but this The content of invention is not limited solely to the following examples.
Embodiment 1
A kind of preparation method of MgAlON transparent ceramic powder, comprising the following steps:
(1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3Powder and MgO powder, obtain mixed powder, spare；
The ratio are as follows: Al powder, γ-Al2O3Powder, MgO powder mass fraction be respectively 4wt%, 80wt%, 16wt%；
The average particle size of the Al powder is 2.5 μm, purity 99.95wt%；γ-Al2O3Powder average particle size 20nm, Purity 99.5wt%；MgO powder average particle size 100nm, purity 99.99wt%；
(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling 16h obtains slurry；
Rotational speed of ball-mill is 120r/m；The abrading-ball that ball milling is selected is alumina balls, purity 99wt%；Abrading-ball and mixed powder Mass ratio is 5:1；
(3) slurry is dry: taking slurry obtained by step (2) dry, obtains dry powder；
For the oxidation for avoiding Al powder in raw material as far as possible, slurry is placed in vacuum chamber (air pressure 20Pa), 60 DEG C of drying temperature, Drying time 4h；
(4) reaction synthesis: dry powder obtained by step (3) is taken, is fitted into crucible, then be placed in high temperature sintering furnace together In, it is passed through flowing nitrogen, with the heating rate of 5 DEG C/min, is warming up to 1500 DEG C of heat preservation 3h, then natural cooling, obtains MgAlON Transparent ceramic powder；
The crucible is alumina crucible, purity 97wt%；
The flowing nitrogen, air pressure absolute value are 0.1MPa, purity 99.99vol%, flow rate 0.1L/min.
Embodiment 2
A kind of preparation method of MgAlON transparent ceramic powder, comprising the following steps:
(1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3Powder and MgO powder, obtain mixed powder, spare；
The ratio are as follows: Al powder, γ-Al2O3Powder, MgO powder mass fraction be respectively 5wt%, 88wt%, 7wt%；
2.5 μm of the average particle size of the Al powder, purity 99.5wt%；γ-Al2O3Powder average particle size 20nm, purity 99.99wt%；MgO powder average particle size 100nm, purity 99.5wt%；
(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling 18h obtains slurry；
Rotational speed of ball-mill is 100r/m；The abrading-ball that ball milling is selected is zirconia ball, purity 99wt%；Abrading-ball and mixed powder Mass ratio is 5:1；
(3) slurry is dry: taking slurry obtained by step (2) dry, obtains dry powder；
For the oxidation for avoiding Al powder in raw material as far as possible, slurry is placed in vacuum chamber (air pressure 20Pa), 60 DEG C of drying temperature, Drying time 10h；
(4) reaction synthesis: dry powder obtained by step (3) is taken, is fitted into crucible, then be placed in high temperature sintering furnace together In, it is passed through flowing nitrogen, with the heating rate of 15 DEG C/min, is warming up to 1550 DEG C of heat preservation 2.5h, then natural cooling, obtains MgAlON transparent ceramic powder；
The crucible is boron nitride crucible, purity 97wt%；
The flowing nitrogen, air pressure absolute value are 0.3MPa, purity 99.99wt%, flow rate 0.3L/min.
Embodiment 3
A kind of preparation method of MgAlON transparent ceramic powder, comprising the following steps:
(1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3Powder and MgO powder, obtain mixed powder, spare；
The ratio are as follows: Al powder, γ-Al2O3Powder, MgO powder mass fraction be respectively 6wt%, 82wt%, 12wt%；
2 μm of the average particle size of the Al powder, purity 99.9wt%；γ-Al2O3Powder average particle size 50nm, purity 99.99 wt%；MgO powder average particle size 70nm, purity 99.5wt%；
(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling 20h obtains slurry；
Rotational speed of ball-mill is 100r/m；The abrading-ball that ball milling is selected is alumina balls, purity 99.9wt%；Abrading-ball and mixed powder Mass ratio be 8:1；
(3) slurry is dry: taking slurry obtained by step (2) dry, obtains dry powder；
For the oxidation for avoiding Al powder in raw material as far as possible, slurry is placed in vacuum chamber (air pressure 10Pa), 70 DEG C of drying temperature, Drying time 8h；
(4) reaction synthesis: dry powder obtained by step (3) is taken, is fitted into crucible, then be placed in high temperature sintering furnace together In, it is passed through flowing nitrogen, with the heating rate of 10 DEG C/min, is warming up to 1600 DEG C of heat preservation 2h, then natural cooling, obtains MgAlON Transparent ceramic powder；
The crucible is alumina crucible, purity 98wt%；
The flowing nitrogen, air pressure absolute value are 0.2MPa, purity 99.995vol%, flow rate 0.5L/min.
Embodiment 4
A kind of preparation method of MgAlON transparent ceramic powder, comprising the following steps:
(1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3Powder and MgO powder, obtain mixed powder, spare；
The ratio are as follows: Al powder, γ-Al2O3Powder, MgO powder mass fraction be respectively 7wt%, 83wt%, 10wt%；
1.5 μm of the average particle size of the Al powder, purity 99.5wt%；γ-Al2O3Powder average particle size 50nm, purity 99.5wt%；MgO powder average particle size 70nm, purity 99.99wt%；
(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling 20h obtains slurry；
Rotational speed of ball-mill is 80r/m；The abrading-ball that ball milling is selected is zirconia ball, purity 99.9wt%；Abrading-ball and mixed powder Mass ratio be 8:1；
(3) slurry is dry: taking slurry obtained by step (2) dry, obtains dry powder；
For the oxidation for avoiding Al powder in raw material as far as possible, slurry is placed in vacuum chamber (air pressure 10Pa), 70 DEG C of drying temperature, Drying time 8h；
(4) reaction synthesis: dry powder obtained by step (3) is taken, is fitted into crucible, then be placed in high temperature sintering furnace together In, it is passed through flowing nitrogen, with the heating rate of 10 DEG C/min, is warming up to 1600 DEG C of heat preservation 2h, then natural cooling, obtains MgAlON Transparent ceramic powder；
The crucible is boron nitride crucible, purity 98wt%；
The flowing nitrogen, air pressure absolute value are 0.2MPa, purity 99.995vol%, flow rate 0.7L/min.
Embodiment 5
A kind of preparation method of MgAlON transparent ceramic powder, comprising the following steps:
(1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3Powder and MgO powder, obtain mixed powder, spare；
The ratio are as follows: Al powder, γ-Al2O3Powder, MgO powder mass fraction be respectively 8wt%, 85wt%, 7wt%；
1 μm of the average particle size of the Al powder, purity 99wt%；γ-Al2O3Powder average particle size 80nm, purity 99.5 Wt%；MgO powder average particle size 40nm, purity 99.99wt%；
(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling for 24 hours, obtains slurry；
Rotational speed of ball-mill is 60r/m；The abrading-ball that ball milling is selected is alumina balls, purity 99.99wt%；Abrading-ball and mixed powder Mass ratio be 10:1；
(3) slurry is dry: taking slurry obtained by step (2) dry, obtains dry powder；
For the oxidation for avoiding Al powder in raw material as far as possible, slurry is placed in vacuum chamber (air pressure 5Pa), 80 DEG C of drying temperature, Drying time 4h；
(4) reaction synthesis: dry powder obtained by step (3) is taken, is fitted into crucible, then be placed in high temperature sintering furnace together In, it is passed through flowing nitrogen, with the heating rate of 5 DEG C/min, is warming up to 1700 DEG C of heat preservation 1h, then natural cooling, obtains MgAlON Transparent ceramic powder；
The crucible is alumina crucible, purity 99.5wt%；
The flowing nitrogen, air pressure absolute value are 0.1MPa, purity 99.999vol%, flow rate 1.0L/min.
Embodiment 6
A kind of preparation method of MgAlON transparent ceramic powder, which is characterized in that it the following steps are included:
(1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3Powder and MgO powder, obtain mixed powder, spare；
The ratio are as follows: Al powder, γ-Al2O3Powder, MgO powder mass fraction be respectively 9wt%, 78wt%, 13wt%；
1 μm of the average particle size of the Al powder, purity 99.95wt%；γ-Al2O3Powder average particle size 100nm, purity 99.99wt%；MgO powder average particle size 40nm, purity 99.5wt%；
(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling for 24 hours, obtains slurry；
Rotational speed of ball-mill is 60r/m；The abrading-ball that ball milling is selected is zirconia ball, purity 99.99wt%；Abrading-ball and mixed powder Mass ratio be 10:1；
(3) slurry is dry: taking slurry sample obtained by step (2) dry, obtains dry powder；
For the oxidation for avoiding Al powder in raw material as far as possible, slurry is placed in vacuum chamber (air pressure 5Pa), 80 DEG C of drying temperature, Drying time 10h；
(4) reaction synthesis: dry powder sample obtained by step (3) is taken, is fitted into crucible, then be placed in high temperature sintering together In furnace, it is passed through flowing nitrogen, with the heating rate of 15 DEG C/min, is warming up to 1700 DEG C of heat preservation 3h, then natural cooling, obtains MgAlON transparent ceramic powder；
The crucible is boron nitride crucible, purity 99.5wt%；
The flowing nitrogen, air pressure absolute value are 0.3MPa, purity 99.999vol%, flow rate 1.0L/min.
The XRD spectrum for the MgAlON powder that embodiment described above 1,3,5 synthesizes, can as shown in Figure 1, according to XRD spectrum With judgement, the product of synthesis is MgAlON single-phase material, without other obvious last phases.
MgAlON powder thing phase purity, the carbon content, average particle size of embodiment described above 1-6 synthesis, are shown in Table 1.
Table 1
As can be seen from Table 1, MgAlON powder purity obtained in case study on implementation high (being not less than 99.5%), carbon content pole Low (31ppm~60ppm)；Granularity is very tiny (1000nm or less), and powder characteristic is excellent, suitable for the transparent pottery of production Porcelain.
Transmittance curve such as Fig. 2 of MgAlON crystalline ceramics made from the MgAlON powder that embodiment described above 3 synthesizes Crystalline ceramics that is shown, being made of MgAlON, transparency range is wide, covers ultraviolet-visible light-laser-near infrared band (0.2 μm -2.0 μm), and optical transmittance with higher, at 0.4 μm, 1.0 μm, 2.0 μm transmitance respectively reach~75%, 77%, 80% or so, optical transmittance is excellent.

Claims (8)

1. a kind of preparation method of MgAlON transparent ceramic powder, which comprises the following steps:
(1) raw material weighs: according to a certain percentage, weighing Al powder, γ-Al2O3Powder and MgO powder, obtain mixed powder, spare；
The ratio are as follows: Al powder, γ-Al2O3Powder, MgO powder mass fraction be respectively 4wt%~9wt%, 78wt%~ 88wt%, 7wt%~16wt%；
(2) ball milling disperses: dispersing mixed powder obtained by step (1) in dehydrated alcohol, ball milling obtains slurry；
(3) slurry is dry: taking slurry obtained by step (2) dry, obtains dry powder；
(4) reaction synthesis: dry powder obtained by step (3) is taken, is fitted into crucible, then be placed in high temperature sintering furnace together, leads to Enter flowing nitrogen, with the heating rate of 5 DEG C~15 DEG C/min, is warming up to 1500 DEG C~1700 DEG C heat preservation 1h~3h, it is then natural It is cooling, obtain MgAlON transparent ceramic powder.
2. the preparation method of MgAlON transparent ceramic powder according to claim 1, which is characterized in that in step (1), institute Average particle size≤2.5 μm for the Al powder stated, purity >=99wt%；γ-Al2O3Powder average particle size≤100nm, purity >= 99.5wt%；MgO powder average particle size≤100nm, purity >=99.5wt%.
3. the preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, which is characterized in that step (2) In, rotational speed of ball-mill is 60r~120r/m；Ball-milling Time >=16h.
4. the preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, which is characterized in that step (2) In, the abrading-ball that ball milling is selected is alumina balls or zirconia ball, purity >=99wt%；
5. the preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, which is characterized in that step (2) In, the mass ratio of abrading-ball and mixed powder is 5:1~10:1.
6. the preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, which is characterized in that step (3) In, it is the oxidation for avoiding Al powder in raw material as far as possible, slurry is placed in vacuum chamber (air pressure is not higher than 20Pa), drying temperature >=60 DEG C, so that the dehydrated alcohol in slurry is sufficiently volatilized.
7. the preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, which is characterized in that step (4) In, the crucible is aluminium oxide or boron nitride crucible, purity >=97wt%；
8. the preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, which is characterized in that step (4) In, the flowing nitrogen, air pressure absolute value is 0.1MPa~0.3MPa, purity >=99.99vol%, flow rate 0.1L ~1.0L/min.
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