CN1915907A - Infrared permeated alpha-sialon ceramic material and preparation method - Google Patents

Infrared permeated alpha-sialon ceramic material and preparation method Download PDF

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CN1915907A
CN1915907A CN 200610010503 CN200610010503A CN1915907A CN 1915907 A CN1915907 A CN 1915907A CN 200610010503 CN200610010503 CN 200610010503 CN 200610010503 A CN200610010503 A CN 200610010503A CN 1915907 A CN1915907 A CN 1915907A
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alpha
ceramic material
sialon
infrared
sialon ceramic
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叶枫
刘利盟
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

This invention provides a method for preparing IR-transmitting alpha-sialon ceramic with the molecular formula of Rem/3Si12-(m+n)Alm+nOnN16-n, wherein m is 1, n is in 0.5-2, and Re is rare earth metal. The alpha-sialon ceramic is prepared from Si3N4, AlN, Al2O3 and Re2O3 powder. The method comprises: (1)c preparing the above raw materials according to the molecular formula; (2) preparing photic alpha-sialon material by hot-pressing sintering; (3) nitrifying at high temperatures, and cooling in the temperature range higher than 1200 deg.C. The alpha-sialon content is adjusted to alpha-beta phase boundary to reduce the content of inter-crystal phase.

Description

Infrared permeated alpha-sialon ceramic material and preparation method thereof
Technical field
The invention belongs to infrared ceramic material technology field, particularly a kind of infrared permeated alpha-sialon material and preparation technology thereof.
Background technology
Sialon (Sialon) has been taken as always since finding that use temperature can reach 1500 ℃ high-temperature structural material and the funds support that obtains to continue.Wherein have characteristics such as easy densification, chemical stability are good, wear-resisting, anti-oxidant, have excellent normal temperature and mechanical behavior under high temperature concurrently, have wide practical use in the Aeronautics and Astronautics field from the malleableize alpha--sialon ceramic.
Research has found that the sialon pottery has good optical property [J Mater Res 1,996 11 (11) 2790～2794; J Mater Sci Lett 1,982 1 25～26], the fine and close sample of 0.5～1.0mm thickness can clearly reflect up underlaid literal; The Sialon pottery adds different rare earth elements and presents multicoloured color; When being subjected to X ray or uviolizing, fluorescence, flicker effect are arranged.These phenomenons show that alpha--sialon ceramic has very big application potential at optical field.Compare with existing optical material, α-sialon also has (1) better room temperature and mechanical behavior under high temperature, hardness height; (2) anti-wear wearing and tearing ability is superior; (3) heat-resisting, anti-thermal shock; (4) has better oxidation-resistance; (5) have feature such as wideer transparency range (and abundant color), so it can use at normal temperatures not only, more can be used as infrared window, lens material under high temperature, the extreme condition, and the optical function material of other purposes.With BAS-Si 3N 4Matrix material [US6184164-B1; US5538925-A; US7982535-N; WO200064835-A] analogy, can predict it has the potential using value at aspects such as hypersonic missile radome, microwave and infrared eye windows.
Considerably less in the international coverage about the open report of α-sialon light transmission.Mandal etc. [J EuroCeram Soc 1,999 19 2949～2957] have prepared the Nd with certain transmittancy 2O 3And Yb 2O 3Stable alpha--sialon ceramic, but transmittance is not carried out quantitative examination.[J Am Ceram Soc 2,003 86 (3) 520～522 such as Jones; J Am Ceram So.200487 (4) 714～716] find that α/β-sialon pottery is the highest 30% transmittance arranged; Adopt the no crystal boundary phase of the full densification Lu-of the uniform formation alpha-sialon ceramic material of hot-pressing sintering method preparation, for the visible light transmissivity of 600nm about 70%.Doctor Su Xinlu [the J Am Ceram Soc 2,004 87 730～732 of domestic Shanghai silicate institute; Mater Letters 2,004 58 1985～1988] studied the light transmission of hot pressing and plasma agglomeration Y, Eu, alpha--sialon ceramics such as Dy, Yb, best Dy-alpha--sialon ceramic has 65% transmittance at infrared band.According to optical principle, intergranular is the important factor that influences the polycrystalline ceramics light transmission mutually.
Summary of the invention
In order to improve the light transmission of alpha--sialon ceramic, reduce the influence of the relative polycrystalline ceramics light transmission of intergranular, the invention provides a kind of high rigidity, wear-resistant, resistant to elevated temperatures infrared permeated alpha-sialon ceramic material and preparation method thereof.
The molecular formula of infrared permeated alpha-sialon ceramic material of the present invention is Re M/3Si 12-(m+n)Al M+nO nN 16-n, m=1 in the formula, 0.5＜n＜2, Re is a rare earth element, its preparation method is: a, batching: adopt Si 3N 4, AlN, Al 2O 3, Re 2O 3Powder is a raw material, is Re by molecular formula M/3Si 12-(m+n)Al M+nO nN 16-nBatching; B, sintering: adopt hot-pressing sintering technique to prepare printing opacity α-sialon material, furnace chamber vacuumizes before heating up, and charges into purity greater than 99.9% N 2To a normal atmosphere, the control heat-up rate is that 5～50 ℃/min, sintering temperature are that 1800～1900 ℃, axle pressure are that 20～40MPa, sintering time are 30～90min; C, nitrogenize: material is carried out high-temperature ammonolysis handle, treatment process is 2.0～4.0MPa, N 21800～1900 ℃ of insulations in the atmosphere, nitrogenize finish the back in temperature range control cooling more than 1200 ℃.
The present invention is adjusted to the alpha-beta phase boundary with α-sialon composition, reduced the intergranular phase content to greatest extent, promote densification by adding a spot of rare earth oxide then, realized the control of material densification and intergranular phase content, adopt hot-pressing sintering technique to prepare the alpha--sialon ceramic of printing opacity.
The invention has the beneficial effects as follows: (1) is adjusted to and assigns to alpha-beta phase border, has obtained the mutually single alpha--sialon ceramic of thing, and XRD material phase analysis result as Figure 1-3; (2) by adding the Re of excess 2wt% 2O 3Reach means such as adopting hot-pressing sintering technique and realized that composition is Re 1/3Si 10Al 2ON 15The full densification of alpha-sialon ceramic material; (3) impel intergranular impurity dispensing volatile further by follow-up nitriding treatment, having reduced influences the intergranular of transmittance phase content, as the Yb of Fig. 8 1/3Si 10Al 2ON 15-2wt%Yb 2O 3Shown in the TEM tissue of material; (4) low cost has been synthesized the alpha--sialon ceramic that satisfies cruising missile guidance window working conditions.Adopting the thickness of this method preparation is light transmittance curve and the Dy of α-sialon material of 1.0mm at 200-3000nm wavelength light 1/3Si 10Al 2ON 15-2wt%Dy 2O 3Material sees through the photo in kind of visible light and sees Fig. 4-7; (5) be a kind of high rigidity, anti-scratching, resistant to elevated temperatures optical material, basic mechanical performance is shown in subordinate list 1.
Table 1 printing opacity Re 1/3Si 10Al 2ON 15-2wt%Re 2O 3The mechanical property of-α-sialon
The Re type H v10，GPa σ，MPa K IC，MPam 1/2
Y Dy Yb Lu 19.9±0.3 20.0±0.2 19.8±0.2 19.5±0.4 471±16 459±14 423±20 558±15 4.1±0.3 3.9±0.1 3.1±0.2 4.4±0.1
Description of drawings
Fig. 1 is Y 1/3Si 10Al 2ON 15-2wt%Y 2O 3The XRD figure spectrum of material, Fig. 2 is Dy 1/3Si 10Al 2ON 15-2wt%Dy 2O 3The XRD figure spectrum of material, Fig. 3 is Yb 1/3Si 10Al 2ON 15-2wt%Yb 2O 3The XRD figure spectrum of material, Fig. 4 is Y 1/3Si 10Al 2ON 15-2wt%Y 2O 3Material is to the transmittance of 200-3000nm wavelength light, and Fig. 5 is Dy 1/3Si 10Al 2ON 15-2wt%Dy 2O 3Material is to the transmittance of 200-3000nm wavelength light, and Fig. 6 is Yb 1/3Si 10Al 2ON 15-2wt%Yb 2O 3Material is to the transmittance of 200-3000nm wavelength light, and Fig. 7 thickness is the Dy of 1.0mm 1/3Si 10Al 2ON 15-2wt%Dy 2O 3Material sees through the photo in kind of visible light, and Fig. 8 is Yb 1/3Si 10Al 2ON 15-2wt%Yb 2O 3The TEM of material organizes photo.
Embodiment
Embodiment one: the molecular formula of the infrared permeated alpha-sialon ceramic material of present embodiment is Re M/3Si 12-(m+n)Al M+nO nN 16-n, m=1 in the formula, 0.5＜n＜2, Re is rare earth element (Y, Yb, Dy, Lu and other α-sialon stablizer).
Embodiment two: present embodiment is prepared as follows infrared permeated alpha-sialon ceramic material:
A, by molecular formula Re M/3Si 12-(m+n)Al M+nO nN 16-nTo α-sialon batching, adopt Si 3N 4, AlN, Al 2O 3, Re 2O 3Powder is a raw material, and above-mentioned substance is mixed.
B, employing hot-pressing sintering technique prepare printing opacity α-sialon material, and sintering condition is (1800-1900 ℃)/(20-40MPa axle pressure)/(30～90min).Furnace chamber vacuumizes before heating up, and charges into purity greater than 99.9% N 2To a normal atmosphere, heat-up rate is 5～50 ℃/min.
C, material is carried out high-temperature ammonolysis handle, technology is 2.0～4.0MPaN 21800-1900 ℃ of insulation in the atmosphere, (unit, min) (unit mm) is directly proportional soaking time, is the 15-30 multiple of product thickness, and nitrogenize finishes the back in temperature range cooling more than 1200 ℃, and the control cooling rate is not less than 50 ℃/min with product thickness.
Embodiment three: what present embodiment and embodiment two were different is that also adding in the raw material among the step a has sintering agent (Re 2O 3), its add-on is Re M/3Si 12-(m+n)Al M+nO nN 16-n0.1～10% of weight.Add a spot of rare earth oxide and can promote densification, realize the control of material densification and intergranular phase content.
Embodiment four: present embodiment prepares Y according to following step 1/3Si 10Al 2ON 15-2wt%Y 2O 3Material:
One, gets Si 3N 4(specification and the place of production: E10 grade, UBE Industries Ltd., Tokyo, Japan) 78.05 grams, AlN (specification and the place of production: grade C, H.C.Starck, Berlin, Germany) 13.27 grams, Al 2O 3(specification and the place of production: grade A16SG, Alcoa, Pittsburgh, PA) 0.47 gram, Y 2O 3(specification and the place of production: gradefine, H.C.Starck, Berlin, Germany) 8.21 grams are put into the polyvinyl chloride jar, add an amount of Virahol and silicon nitride ceramic ball, and ball milling mixed 12～15 hours.
Two, mixed slurry is poured open container into, puts into 100 ℃ of oven dryings 60 minutes, the screening of 20 order mesh screens, granulation.
Three, adopt hot-pressing sintering technique to prepare printing opacity Y 1/3Si 10Al 2ON 15-2wt%Y 2O 3Material, technological process is: powder is got the graphite jig that mixed powder 40 restrains the Φ 50mm that packs into, goes into stove; Furnace chamber is evacuated down to less than 0.1 * 10 -3Pa, charge into purity greater than 99.9% nitrogen to 1 standard atmospheric pressure; Sintering condition is 1800 ℃/25MPa/60min, and heat-up rate is 20 ℃/min; After finishing, sintering stops heating, furnace cooling.
Four, grind off surface contamination layer after the sintered compact demoulding, put into air pressure stove nitriding treatment, specific embodiment is: the air pressure stove evacuation arrives less than 0.1 * 10 -3Pa, charge into purity greater than 99.9% nitrogen to 2.0MPa, 1850 ℃ of insulation 60min turn off heating power supply, are guaranteeing to be chilled to room temperature greater than 50 ℃/min speed of cooling stove more than 1200 ℃.
Adopting hot-pressing sintering technique to obtain density is Y greater than 99.5% composition 1/3Si 10Al 2ON 15-2wt%Y 2O 3Single phase α-sialon material, weight saving 0.2% behind the nitriding treatment, density does not reduce, thing constitutes mutually and does not change.
In the 200-3000nm test specification, along with the increase of wavelength, thickness is the trend that the material transmittance of 1.0mm is continuous increase, and when wavelength reached 3000nm, the transmitance of sample reached 52%.
Embodiment five: present embodiment prepares Dy according to following step 1/3Si 10Al 2ON 15-2wt%Dy 2O 3Material:
One, gets Si 3N 4(specification and the place of production: E10 grade, UBE Industries Ltd., Tokyo, Japan) 74.93 grams, AlN (specification and the place of production: grade C, H.C.Starck, Berlin, Germany) 12.74 grams, Al 2O 3(specification and the place of production: grade A16SG, Alcoa, Pittsburgh, PA) 0.45 gram, Dy 2O 3(specification and the place of production: gradefine, H.C.Starck, Berlin, Germany) 11.87 grams are put into the polyvinyl chloride jar, add an amount of Virahol and silicon nitride ceramic ball, and ball milling mixed 12～15 hours.
Two, mixed slurry is poured open container into, puts into 100 ℃ of oven dryings 60 minutes, the screening of 20 order mesh screens, granulation.
Three, adopt hot-pressing sintering technique to prepare printing opacity Dy 1/3Si 10Al 2ON 15-2wt%Dy 2O 3Material, technological process is: powder is got the graphite jig that mixed powder 40 restrains the Φ 50mm that packs into, goes into stove; Furnace chamber is evacuated down to less than 0.1 * 10 -3Pa, charge into purity greater than 99.9% nitrogen to 1 standard atmospheric pressure; Sintering schedule is 1800 ℃/25MPa/60min, and heat-up rate is with 20 ℃/min; After finishing, sintering stops heating, furnace cooling.
Four, grind off surface contamination layer after the sintered compact demoulding, put into air pressure stove nitriding treatment, specific embodiment is: the air pressure stove evacuation arrives less than 0.1 * 10 -3Pa, charge into purity greater than 99.9% nitrogen to 2.0MPa, 1850 ℃ of insulation 60min turn off heating power supply, are guaranteeing to be chilled to room temperature greater than 50 ℃/min speed of cooling stove more than 1200 ℃.
Adopting hot-pressing sintering technique to obtain density is Dy greater than 99.7% composition 1/3Si 10Al 2ON 15-2wt%Dy 2O 3Single phase α-sialon material, weight saving 0.2% behind the nitriding treatment, density does not reduce, thing constitutes mutually and does not change.
In the 200-3000nm test specification, along with the increase of wavelength, thickness is the trend that the material transmittance of 1.0mm is continuous increase, reaches 50% in the transmitance of 1900-2500nm wave band sample.
Embodiment six: present embodiment prepares Yb according to following step 1/3Si 10Al 2ON 15-2wt%Yb 2O 3Material:
One, gets Si 3N 4(specification and the place of production: E10 grade, UBE Industries Ltd., Tokyo, Japan) 74.51 grams, AlN (specification and the place of production: grade C, H.C.Starck, Berlin, Germany) 12.67 grams, Al 2O 3(specification and the place of production: grade A16SG, Alcoa, Pittsburgh, PA) 0.45 gram, Yb 2O 3(specification and the place of production: gradefine, H.C.Starck, Berlin, Germany) 12.37 grams are put into the polyvinyl chloride jar, add an amount of Virahol and silicon nitride ceramic ball, and ball milling mixed 12～15 hours.
Two, mixed slurry is poured open container into, puts into 100 ℃ of oven dryings 60 minutes, the screening of 20 order mesh screens, granulation.
Three, adopt hot-pressing sintering technique to prepare printing opacity Yb 1/3Si 10Al 2ON 15-2wt%Yb 2O 3Material, technological process is: powder is got the stone mill mould that mixed powder 40 restrains the Φ 50 that packs into, goes into stove; Furnace chamber is evacuated down to less than 0.1 * 10 -3Pa, charge into purity greater than 99.9% nitrogen to 1 standard atmospheric pressure; Sintering condition is 1800 ℃/25MPa/60min, and heat-up rate is 20 ℃/min; After finishing, sintering stops heating, furnace cooling.
Four, grind off surface contamination layer after the sintered compact demoulding, put into air pressure stove nitriding treatment, specific embodiment is: the air pressure stove evacuation arrives less than 0.1 * 10 -3Pa, charge into purity greater than 99.9% nitrogen to 2.0MPa, 1850 ℃ of insulation 60min turn off heating power supply, are guaranteeing to be chilled to room temperature greater than 50 ℃/min speed of cooling stove more than 1200 ℃.
Adopting hot-pressing sintering technique to obtain density is Yb greater than 99.6% composition 1/3Si 10Al 2ON 15-2wt%Yb 2O 3Single phase α-sialon material, weight saving 0.2% behind the nitriding treatment, density does not reduce, thing constitutes mutually and does not change.
In the 200-3000nm test specification, along with the increase of wavelength, thickness is the trend that the material transmittance of 1.0mm is continuous increase, wavelength greater than the infrared light transmitance numerical value of 1100nm always more than 42%, in the 2000-3000nm wavelength band, transmitance is greater than 60%.

Claims (7)

1, a kind of infrared permeated alpha-sialon ceramic material, the molecular formula that it is characterized in that described alpha-sialon ceramic material is Re M/3Si 12-(m+n)Al M+nO nN 16-n, m=1 in the formula, 0.5＜n＜2, Re is a rare earth element.
2, infrared permeated alpha-sialon ceramic material according to claim 1, the molecular formula that it is characterized in that described alpha-sialon ceramic material is Y 1/3Si 10Al 2ON 15
3, infrared permeated alpha-sialon ceramic material according to claim 1, the molecular formula that it is characterized in that described alpha-sialon ceramic material is Dy 1/3Si 10Al 2ON 15
4, the preparation method of the described infrared permeated alpha-sialon ceramic material of a kind of claim 1 is characterized in that described method is: a, batching: adopt Si 3N 4, AlN, Al 2O 3, Re 2O 3Powder is a raw material, is Re by molecular formula M/3Si 12-(m+n)Al M+nO nN 16-nBatching; B, sintering: adopt hot-pressing sintering technique to prepare printing opacity α-sialon material, furnace chamber vacuumizes before heating up, and charges into purity greater than 99.9% N 2To a normal atmosphere, the control heat-up rate is that 5～50 ℃/min, sintering temperature are that 1800～1900 ℃, axle pressure are that 20～40MPa, sintering time are 30～90min; C, nitrogenize: material is carried out high-temperature ammonolysis handle, treatment process is 2.0～4.0MPa, N 21800～1900 ℃ of insulations in the atmosphere, nitrogenize finish the back in temperature range control cooling more than 1200 ℃.
5, the preparation method of infrared permeated alpha-sialon ceramic material according to claim 4 is characterized in that cooling rate is not less than 50 ℃/min.
6, the preparation method of infrared permeated alpha-sialon ceramic material according to claim 4 is characterized in that in the raw material among the step a also adding that sintering agent, its add-on are arranged is Re M/3Si 12-(m+n)Al M+nO nN 16-n0.1～10% of weight.
7, the preparation method of infrared permeated alpha-sialon ceramic material according to claim 4 is characterized in that described sintering agent is Re 2O 3
CN 200610010503 2006-09-06 2006-09-06 Infrared permeated alpha-sialon ceramic material and preparation method Pending CN1915907A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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
CN102180679A (en) * 2011-01-22 2011-09-14 安徽工业大学 Preparation method of multiphase alpha-beta-Sialon ceramic material added with La2O3
CN109666480A (en) * 2017-10-17 2019-04-23 中国科学院上海硅酸盐研究所 A kind of rear-earth-doped SiAlON light-emitting film and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
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
CN102180679A (en) * 2011-01-22 2011-09-14 安徽工业大学 Preparation method of multiphase alpha-beta-Sialon ceramic material added with La2O3
CN109666480A (en) * 2017-10-17 2019-04-23 中国科学院上海硅酸盐研究所 A kind of rear-earth-doped SiAlON light-emitting film and preparation method thereof
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

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