CN1260178C - Alpha sialon ceramic materials with high infrared transmittance and method for preparing same - Google Patents
Alpha sialon ceramic materials with high infrared transmittance and method for preparing same Download PDFInfo
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- CN1260178C CN1260178C CN 200310109016 CN200310109016A CN1260178C CN 1260178 C CN1260178 C CN 1260178C CN 200310109016 CN200310109016 CN 200310109016 CN 200310109016 A CN200310109016 A CN 200310109016A CN 1260178 C CN1260178 C CN 1260178C
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- stupalith
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Abstract
The present invention relates to an alpha-Sialon ceramic material with high infrared transmissivity and a preparation method thereof, which belongs to the field of the application and preparation of silicon nitride base ceramics. The present invention is characterized in that the alpha-Sialon ceramic material has good light transmission performance within the range of infrared bands; no less than 99.5 wt% of high-purity Si3N4 powder, AlN powder, Al2O3 powder and rare earth oxide M2O3 (M is Dy, Y, Gd, Yb and Nd) are used as raw materials, and x, m and n in the alpha-Sialon formation general formula of MxSi(12-(m+n))Al(m+n)OnN(16-n)are used as parameters for component point selection for compounding, wherein m equals to 3x, m is larger than 0.3 and smaller than 1.2, and n is larger than 0.6 and smaller than 2.0; the raw materials are treated by ball milling, drying and hot pressing at the temperature of 1700 DEG C to 1850 DEG C for 1 to 5 hours, before the temperature reaches the sintering temperature, the sintering process is carefully controlled during the middle heat preservation hot pressing within the temperature of 1500 DEG C to 1650 DEG C for 0.5 to 2 hours, and the compact single-phase alpha-Sialon is prepared.
Description
Technical field
That the present invention relates to is a kind of stupalith A Erfa Sialon with high IR transmitance (α-Sialon) and preparation method thereof.More precisely providing the highly purified silicon nitride of a kind of usefulness, aluminium nitride, aluminum oxide and rare earth oxide is main raw material, by the hot-pressing sintering technique of careful control, prepare A Erfa Sialon with high IR transmitance (α-Sialon) stupalith and corresponding preparation method thereof.This material also has good mechanical property.
Background technology
Development along with lighting engineering, optics, extraordinary instrument manufacturing, Wireless Electronics, high-temperature technology and war industry, crystalline ceramics as outer cover and window material has been proposed more harsh service requirements, except requiring certain wavelength region has than high permeability, also to require material to have otherwise premium properties as higher mechanical property.Some traditional materials often exist such or such deficiency, and for example, materials such as traditional glass, Si, Ge monocrystalline can lose light transmission very soon under high temperature, violent friction environment, thereby are restricted at aspects such as high temperature Real Time Observation, guided missile infrared guidances.Much opticglass is short through wavelength region, and when temperature surpassed 500 ℃, the light transmission of glass sharply descended, and the not attrition resistant problem of the same existence of glass.In contrast to this, the preparation cost of high-performance ceramic is just much lower, mixes easily evenly, makes big, the complex-shaped parts of size easily, and some stupaliths such as silicon-nitride-based ceramic have excellent mechanical property.In view of above various reasons, the application of polycrystalline ceramics aspect optics comes into one's own always.
Report about light transparent ceramic can be traced back to 1962, and promptly R.L.Coble prepares translucent sintered alumina.Pass through the researchdevelopment of decades since then, prepared MgO, Al
2O
3, MgAl
2O
4, Y
3Al
5O
12(YAG) etc. from seeing the oxide ceramics of infrared high transmission rate, and the first-class field of mirror for taking photograph of working under infrared laser window, high temperature window, infrared guidance guided missile ball cover and high temperature or severe radiation is used, in addition also relevant for the report of non-oxidized substance such as AlN, AlON crystalline ceramics, but research that is that all right is ripe.Compare with oxide compound, not only room temperature strength is higher for non-oxidized substance mostly, and also has good mechanical property when high temperature.They also have the cold causus impact property of good anti-play.Therefore, optical property just is expected to and can more using under the exacting terms if having preferably.
Sialon is Si
3N
4Sosoloid, have people such as K.H.Jack at first to propose in 1972.Corresponding Si
3N
4α-and β-two kind of variant, the sosoloid of two kinds of structures of Sialon is called α-Sialon and beta-Sialon.For α-Sialon, have higher thermal shock resistance and oxidation-resistance than the transparent material of known oxide-base; Has wideer color gamut, easier sintering than known non-oxidized substance base transparent material.But for a long time, mainly α-Sialon is studied as typical structural ceramics, seldom noted its function application facet.Several years up to date just gradually relevant for the report of α-Sialon light transmission, reported the α-Sialon pottery of different colours with relative high-clarity as B.S.B.Karunaratne, H.Mandal prepares translucent α-Sialon with hot isostatic pressing and thermal treatment, and M.Jones et al has then reported at visible light wave range to have alpha-beta-Sialon matrix material than high permeability.But these light transmission results of study all obtain when sample quite approaches (0.5mm), also do not have the very correlative study of system.And, there is not the disclosed relevant high patent of infrared Sialon pottery thoroughly at present abroad.
Summary of the invention
The object of the present invention is to provide a kind of stupalith A Erfa Sialon with high IR transmitance (α-Sialon) and preparation method thereof.
The objective of the invention is to implement by following manner.Promptly in conjunction with existing Ln
2O
3-Si
3N
4-AlN-Al
2O
3The knowledge of α in the multicomponent system-Sialon phase plane, utilize mass percent to be not less than 99.5% high purity silicon nitride, aluminium nitride, aluminum oxide and rare earth oxide, by the hot-pressing sintering technique of careful control, prepare stupalith A Erfa Sialon with high IR transmitance (α-Sialon).
Specifically:
(1) according to existing Ln
2O
3-Si
3N
4-AlN-Al
2O
3The knowledge of α in the multicomponent system-Sialon phase plane is with α-Sialon formula M
xSi
12-(m+n)Al
M+nO
nN
16-nIn x, m, n for selecting the parameter of component point, m=3x, 0.3＜m＜1.2,0.6＜n＜2.0.M is Dy, Y, Gd, Yb, any or not of the same race by a certain percentage compound mutually among the Nd.When single rare earth oxide compound or different rare earth oxide were composite mixed, it was in the 5-20% scope that total doping should be controlled at mass percent
(2) raw material: comprise that mass percent is not less than 99.5% high purity silicon nitride powder, aluminum nitride powder, aluminum oxide powder and rareearth oxidate powder.By after the composition proportioning weighing of above-mentioned (1), in plastics pot, be dispersion medium with the dehydrated alcohol, Si
3N
4Ball is that ball-milling medium mixed 24 hours, after the oven dry of taking-up slurry, sieves through being not less than 100 purpose screen clothes.
(3) preparation: the powder that mixes is put in the graphite jig, and the mould that will install powder again is placed in the hot pressing furnace.In order to prevent that powder and graphite jig from reacting, mould inner surface scribbles boron nitride powder.Vacuumize earlier before burning till, feed the N that flows then
2Protection gas.Earlier through interior 0.5-2 hour middle hot pressing sintering process of 1500-1650 ℃ of necessary scope, elevated temperature is to 1700-1800 ℃ then in the sintering process, and high temperature hot pressing sintering time is 1-5 hour.Average temperature rise rate in the sintering process is 10-50 ℃/min, and hot pressing pressure is not less than 15MPa.Treat after the burning-out to take out behind the sample naturally cooling, with grinding machine and polishing machine sample is worked into and requires size and smooth finish, just obtain having the α-Sialon material of good light transmission.
(4) material: the unique crystallization phases in this material is α-Sialon.To the thick sample of 1.0mm, be not less than 60% at the maximum transmission of infrared band.To the thick sample of 1.5mm, be not less than 50% at the maximum transmission of infrared band.The hardness of this material reaches 20GPa, and fracture toughness property reaches 5.0MPam
1/2
Advantage of the present invention is:
(1) preparation technology has the characteristics of self, and simple relatively; Technology is controlled easily, prepares the needed time weak point of this material; Prepare large size and complex-shaped parts easily.
(2) material has good infrared property.To 1.0mm and the thick sample of 1.5mm, be not less than 60% and 50% respectively at the maximum transmission of infrared band.
(3) mechanical property of material is good.The hardness of material can reach 20GPa, and fracture toughness property can reach 5MPam
1/2
Description of drawings
Fig. 1 is the XRD figure of the stupalith prepared of embodiment 1 provided by the invention.
Fig. 2 is the microstructure pattern photo of the stupalith that obtains of embodiment 1 provided by the invention.
Fig. 3 is that embodiment 1 provided by the invention obtains the transmittance curve of the thick stupalith of 1.0mm and 1.5mm at infrared band.
Fig. 4 is the stupalith photo that embodiment 1 provided by the invention obtains.Left figure sample thickness is 1.0mm, and right figure sample thickness is 1.5mm.
Embodiment
Embodiment 1
Mixing with dysprosium oxide, is raw material with mass percent greater than 99.5% high purity silicon nitride powder, aluminum nitride powder, aluminum oxide powder.Selecting the batching point in the single-phase plane of α-Sialon, is dispersion medium with the dehydrated alcohol with the powder for preparing in plastics pot, is ball-milling medium with silicon nitride, ball milling 24 hours.Mixed material oven dry back adopts foregoing hot-pressing sintering technique to prepare Dy-α-Sialon material, again the stupalith that obtains requiring with grinding machine and polishing machine processing.Do interior mark with the Si powder, XRD determining result is single-phase α-Sialon, and its XRD figure spectrum and microstructure are respectively as depicted in figs. 1 and 2.The maximum transmission of the thick sample of the 1.0mm that is prepared in infrared band reaches 65.7%, and the maximum infrared transmittivity of the thick sample of 1.5mm reaches 52%.The transmittance curve of sample in infrared band respectively as shown in Figure 3.Prepare the thick material sample of 1.0mm and 1.5mm and see Fig. 4.After testing, the hardness of this material is 20GPa, and fracture toughness property is 5.1MPam
1/2
Embodiment 2
With yttrium oxide is doping agent, Application Example 1 described high purity silicon nitride, aluminium nitride and alumina raw material, adopt single-phase α-Sialon material that the prepared of embodiment 1 goes out when 1.0mm and 1.5mm are thick, still to have respectively to be not less than 60% and 50% infrared transmittivity, have good mechanical property simultaneously.
Embodiment 3
Adopt dysprosium oxide and yttrium oxide composite mixed, Application Example 1 described high pure raw material and heat pressing process, single-phase α-the Sialon for preparing still has respectively when 1.0mm and 1.5mm are thick and is not less than 60% and 50% infrared transmittivity, has excellent mechanical property.
Embodiment 4
The employing gadolinium sesquioxide is a doping agent, adopt embodiment 1 described technology and high purity silicon nitride, aluminium nitride and alumina raw material, the α for preparing-Sialon material still has respectively when 1.0mm and 1.5mm are thick and is not less than 60% and 50% infrared transmittivity, has good mechanical property simultaneously.
Embodiment 5
The employing ytterbium oxide is a doping agent, Application Example 1 described high purity silicon nitride, aluminium nitride and alumina raw material, and α-Sialon material that the prepared of employing embodiment 1 goes out still has good saturating infrared property and mechanical property.
Claims (4)
1. the preparation method with stupalith α Sialon stupalith of high IR transmitance presses earlier M
xSi
12-(m+n)Al
M+nO
nN
16-nBatching, 0.3＜m in the formula＜1.2,0.6＜n＜2.0, m=3x, M are Dy, Y, Gd, Yb, a kind of in five kinds of rare earth elements of Nd or theirs is compound; The batching back is a dispersion medium with the dehydrated alcohol, with Si
3N
4Ball is a ball-milling medium, mixes in plastics pot 24 hours, takes out that slurry is dried, sieved, sintering, it is characterized in that:
(1) when batching functional quality per-cent to be not less than 99.5% high purity silicon nitride, aluminium nitride, aluminum oxide and RE oxide powder be main raw material;
(2) in the sintering process earlier through the necessary middle hot pressing sintering process that in 1500-1650 ℃ of scope, has 0.5-2 hour, and then elevated temperature is to 1700-1800 ℃ of hot pressed sintering, sintering time is 1-5 hour, carries out in flowing nitrogen atmosphere, and hot pressing pressure is not less than 15MPa.
2. by the described a kind of preparation method of claim 1 with stupalith α Sialon stupalith of high IR transmitance, when it is characterized in that utilizing single rare earth oxide compound or different rare earth oxide composite mixed, it is in the 5-20% scope that total doping is controlled at mass percent.
3. by the described a kind of preparation method of claim 1 with stupalith α Sialon stupalith of high IR transmitance, it is characterized in that the slurry oven dry after, sieving is not less than 100 orders.
4. by the described a kind of preparation method with stupalith α Sialon stupalith of high IR transmitance of claim 1, the average temperature rise rate when it is characterized in that hot pressed sintering is 10-50 ℃/min.
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| CN 200310109016 CN1260178C (en) | 2003-12-03 | 2003-12-03 | Alpha sialon ceramic materials with high infrared transmittance and method for preparing same |
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| CN1260178C true CN1260178C (en) | 2006-06-21 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234902B (en) * | 2008-02-21 | 2010-07-21 | 上海交通大学 | Method for synthesizing alpha-Sialon ceramic material by using aluminum ash and blast furnace slag |
| CN104418595B (en) * | 2013-08-22 | 2016-12-28 | 宁波江丰电子材料股份有限公司 | A kind of manufacture method of Sialon ceramics target |
| CN109666480B (en) * | 2017-10-17 | 2021-12-07 | 中国科学院上海硅酸盐研究所 | Rare earth doped SiAlON luminescent film and preparation method thereof |
| CN113735563B (en) * | 2021-08-10 | 2022-10-18 | 上海理工大学 | Probe material for ultrasonic metallurgy and preparation method thereof |
| CN113943162B (en) * | 2021-10-20 | 2023-01-17 | 西北工业大学 | alpha-SiAlON high-entropy transparent ceramic material and preparation method thereof |
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