CN107540372A - Medium-wave infrared window and preparation method thereof - Google Patents
Medium-wave infrared window and preparation method thereof Download PDFInfo
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- CN107540372A CN107540372A CN201610465700.7A CN201610465700A CN107540372A CN 107540372 A CN107540372 A CN 107540372A CN 201610465700 A CN201610465700 A CN 201610465700A CN 107540372 A CN107540372 A CN 107540372A
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Abstract
A kind of medium-wave infrared window and preparation method thereof, the medium-wave infrared window is Y2O3Stable cubic polycrystal zirconia ceramics, raw material is 2.5 3.0mol%Y2O3ZrO2Nano-powder, ceramic average grain size are 200 600nm.Obtained using discharge plasma sintering (SPS) or high temperature insostatic pressing (HIP) (HIP) sintering method.Medium-wave infrared window of the present invention can use in room temperature to 300 DEG C of scopes, and the transmitance of 3.7 4.8 μm of medium-wave infrared wave bands is not less than 75%；The radiation coefficient of 0 300 DEG C of scopes is not more than 0.05；Bending strength is not less than 1000MPa.It can be used in the infrared dome of hypersonic missile, or the medium-wave infrared window for other high temperature applicationss.
Description
Technical field
The present invention relates to medium-wave infrared window, the medium-wave infrared window of particularly a kind of high temperature resistance and high strength and its preparation side
Method.
Background technology
Infrared detection technique occupies highly important status in modern national defense technology, and the guidance of various guided missiles is infrared pre-
Alert, observation aims at many fields such as (high energy beam intercept weapon etc.) and is related to infrared detection technique.Infrared window is that missile IR is led
The important component of leader, play a part of protecting each component of internal detection system, while and can enough effectively transmits infrared signal.
In recent years, as the speed of the aircraft such as guided missile is more and more faster, infrared window by air high-speed friction, pneumatically
Fuel factor causes the temperature of infrared electro window to rise rapidly, and new challenge is proposed to material of infrared window.Window under high temperature
The infra-red radiation of material itself is by the extraneous infrared signal entered of strong interference, or even causes detector saturation.It is most of red
Outer material has significant infra-red radiation at high operating temperatures, has been difficult to meet hypersonic flight condition to infrared window
It is required that.In addition, for thermal stress caused by resisting pneumatic fuel factor, material of infrared window also needs to have excellent mechanical property
Energy.
The research of Raytheon companies of the U.S. confirms Y2O3Ceramic window can keep good under 4Ma flying condition
Infrared imaging performance, without extra Cooling Design【P.Hogan,T.Stefanik,C.Willingham,et.al.,
the 10th DoD Electromagnetic Windows Symposium,(2004)】；But due to Y2O3Ceramics strength and
Thermal shock resistance deficiency, in order to obtain the Low emissivity material of infrared window of higher intensity, project offices of U.S. Department of Defense in 2007 and sea
Research department of army (DARPA/ONR) starts nanocomposite optical ceramic research project (NCOC)【http:// www.darpa.mil/Our_Work/DSO/Programs/Nano_Composite_Optical_Cer amics_(NCOC)
.aspx】, exploitation high intensity Y2O3- MgO Nanocomposite infra-red chinas【D.C.Harris,L.Cambrea,L.Johnson,
et.al.,J.Am.Ceram.Soc.,96(12),3828-35(2013)】.However, MgO nano particles have strong moisture absorption
Property, the moisture in preparation and process easily in absorption air forms hydroxide and carbonate, causes the height of the material
Warm infrared transmittivity and radiation coefficient are difficult to reach expected requirement.Therefore, high temperature resistance and high strength medium-wave infrared window is developed, is
Develop hypersonic vehicle Infrared and be badly in need of one of crucial problem of solution.
Y2O3Stable cubic polycrystal zirconia (Y-TZP) ceramics are because of Tetragonal t-ZrO2The martensitic traoformation toughness reinforcing of crystal grain,
And the excellent mechanical performance for being difficult to reach with other ceramic materials.But due to tetragonal structure, Y-TZP ceramics are difficult to obtain good
Good optical transmittance, and be considered as being difficult to as crystalline ceramics for a long time.Study【Adv.Funct.Mater.2007,17,
3267–3273】It was found that the Y prepared using advanced sintering process2O3Stable cubic polycrystal zirconia (Y-TZP) ceramics have height
Intensity and certain optical transmittance.
The content of the invention
The problem of in order to overcome existing infra-red material to exist under pneumatic thermal environment, the present invention propose a kind of medium-wave infrared window
Mouthful and preparation method thereof, the medium-wave infrared window has the characteristics of high temperature resistant, high intensity.
The technical solution of the present invention is as follows：
A kind of medium-wave infrared window, the medium-wave infrared window is Y2O3Stable cubic polycrystal zirconia ceramics, its feature exist
In raw material be 2.5-3.0mol%Y2O3ZrO2Nano-powder, ceramic average grain size are 200-600nm, and ceramics strength is not
Less than 1000MPa.
The preparation method of above-mentioned medium-wave infrared window, this method comprise the following steps：
1) to contain 2.5-3.0mol%Y2O3ZrO2Nano-powder is as raw material, material purity 99.99%, granularity
20-100nm；
2) discharge plasma sintering (hereinafter referred to as SPS) or high temperature insostatic pressing (HIP) (hereinafter referred to as HIP) sintering side are used
Method, in 1100~1250 DEG C of sintering, obtain ceramic sintered bodies；
3) then by ceramic sintered bodies in atmosphere 1000 DEG C annealing 10-20h.
Described SPS sintering methods use graphite jig, and pressure is 50MPa in sintering process, with 100 under vacuum atmosphere
DEG C/min speed is warming up to 1100 DEG C of maximum temperature, sintering time 5-30min.
Described HIP sintering methods include：Raw material is first pressed into biscuit in stainless steel mould, biscuit in vacuum or
Pre-sintered in air atmosphere to obtain pre-sintered body, the relative density that described pre-sintered body is tested with densimetry is more than 95%；So
The pre-sintered body of gained is put into high temperature insostatic pressing (HIP) stove using Ar as pressure medium afterwards, 3h is handled under conditions of 200MPa.
The technique effect of the present invention：
Medium-wave infrared window of the present invention can be used below at 300 DEG C, and the medium-wave infrared window is red in 3.7-4.8 μm of medium wave
The transmitance of wave section is high, and radiation is low, and intensity is high；It can be used in the infrared dome of hypersonic missile, or be used for
The medium-wave infrared window of other high temperature applicationss.
The preparation method of medium-wave infrared window of the present invention, have step simple, the advantages of easily realization.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
Contain 2.5mol%Y using average grain diameter as 20-50 nanometers2O3ZrO2Nano-powder is as raw material, material purity
99.99%；Using SPS sintering methods, it would be desirable to which the powder of sintering is mounted in graphite jig, and 50MPa pressures are kept in sintering process
Power；1100 DEG C, soaking time 5-30min of maximum temperature is warming up to 100 DEG C/min speed under vacuum atmosphere, preferably
Soaking time is 10min.
Sample after SPS sintering is heated to 1000 DEG C of annealing 10-20h in atmosphere, remaining when vacuum SPS is sintered to eliminate
The defects of.
Sample polishing both surfaces after annealing, sample of the sample thick using 3mm as optical performance test.The test of intensity is pressed
Requirement according to fine ceramics strength test standard is carried out；Optical transmittance is tested in infrared spectrometer, and equipped with to sample
The heating chamber of product heating；Wherein the test of hyperthermia radiation coefficient according to【Infrared Physics&Technology 39_
1998.251–261】Middle Fig. 1 method is carried out, and using carbon dioxide laser as heating source, radiation of the sample in opposite side is received
The emittance of sample at identical temperature and the emittance of standard blackbody are contrasted, obtained into infrared spectrometer by collection
3.7-4.8 μm medium-wave infrared radiation coefficient.
Test result is as follows：
Bending strength：1520MPa；
Average grain diameter：220nm；
3.7-4.8 mu m waveband infrared transmittivities：78% (room temperature~300 DEG C)；
Infrared radiation coefficient：0.04 (at 300 DEG C), 0.02 (room temperature~250 DEG C).
Embodiment 2
Contain 3mol%Y using average grain diameter as 50-100 nanometers2O3ZrO2Nano-powder as raw material, material purity
99.99%；Biscuit is suppressed in 200MPa using cold isostatic pressing method；The pre-burning in vacuum or air atmosphere of gained biscuit
Knot, 1300 DEG C of sintering temperature, time 3h；Then the pre-sintered body of gained is put into HIP stoves, using Ar as pressure medium,
3h is handled under conditions of 1250 DEG C and 200MPa.
Products obtained therefrom after annealing same as Example 1, processing and test process also with the phase of embodiment 1
Together.
Test result is as follows：
Bending strength：1230MPa；
Average crystal grain size 580nm；
3.7-4.8 mu m waveband infrared transmittivities：75% (room temperature~300 DEG C)；
Infrared radiation coefficient：0.03 (at 300 DEG C), 0.02 (room temperature~250 DEG C).
By the Y-TZP ceramic windows manufactured by embodiment 1 and embodiment 2, after being previously heated to more than 300 DEG C, it is placed on
Before thermal infrared imager, as a result it is shown in the temperature range that window temperature is room temperature~300 DEG C, thermal imaging system passes through ceramic window
Original image can be still clearly showed that, experiment shows, medium-wave infrared window of the present invention can be in room temperature to 300 DEG C of models
Use is enclosed, the transmitance of 3.7-4.8 μm of medium-wave infrared wave band is not less than 75%；The radiation coefficient of 0-300 DEG C of scope is not more than
0.05；Bending strength is not less than 1000MPa.It can be used in the infrared dome of hypersonic missile, or for other high temperature
The medium-wave infrared window of occasion.
Claims (4)
1. a kind of medium-wave infrared window, the medium-wave infrared window is Y2O3Stable cubic polycrystal zirconia (Y-TZP) ceramics, its
It is 2.5-3.0mol%Y to be characterised by raw material2O3ZrO2Nano-powder, ceramic average grain size are 200-600nm, ceramics
Intensity is not less than 1000MPa.
2. the preparation method of the medium-wave infrared window described in claim 1, it is characterized in that this method comprises the following steps：
1) to contain 2.5-3.0mol%Y2O3ZrO2Nano-powder is as raw material, material purity 99.99%, granularity 20-
100nm；
2) SPS or HIP sintering methods are used, in 1100~1250 DEG C of sintering, obtain ceramic sintered bodies；
3) then by ceramic sintered bodies in atmosphere 1000 DEG C annealing 10-20h.
3. the manufacture method of medium-wave infrared window according to claim 2, it is characterized in that described SPS sintering methods use
Graphite jig, pressure is 50MPa in sintering process, and maximum temperature is warming up to 100 DEG C/min speed under vacuum atmosphere
1100 DEG C, sintering time 5-30min.
4. the manufacture method of medium-wave infrared window according to claim 2, it is characterized in that described HIP sintering method bags
Include：Raw material is first pressed into biscuit in stainless steel mould, biscuit is pre-sintered in vacuum or air atmosphere to obtain pre-sintering
Body, the relative density that described pre-sintered body is tested with densimetry are more than 95%；Then the pre-sintered body of gained is put into heat etc.
Using Ar as pressure medium in static pressure stove, 3h is handled under conditions of 200MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114349500A (en) * | 2022-01-21 | 2022-04-15 | 中国科学院上海硅酸盐研究所 | Medium-wave infrared transparent zirconia ceramic material and preparation method thereof |
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