CN104829220A - Multiband laser protection transparent ceramic material and preparation method thereof - Google Patents
Multiband laser protection transparent ceramic material and preparation method thereof Download PDFInfo
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- CN104829220A CN104829220A CN201510161523.9A CN201510161523A CN104829220A CN 104829220 A CN104829220 A CN 104829220A CN 201510161523 A CN201510161523 A CN 201510161523A CN 104829220 A CN104829220 A CN 104829220A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 18
- 229910002106 crystalline ceramic Inorganic materials 0.000 claims description 17
- 239000011222 crystalline ceramic Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 230000001681 protective effect Effects 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 11
- 235000015895 biscuits Nutrition 0.000 claims description 10
- 230000003287 optical effect Effects 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000005056 compaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000007493 shaping process Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 9
- 239000007790 solid phase Substances 0.000 abstract 1
- 238000002834 transmittance Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000001778 solid-state sintering Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Abstract
The invention provides a multiband laser protection transparent ceramic material and a preparation method thereof. The multiband laser protection transparent ceramic material has an expression formula of (Er1-xDyx)3Al5O12, wherein x is greater than or equal to 0.005 and less than or equal to 1. The multiband laser protection transparent ceramic material is prepared by vacuum solid phase sintering. Through adjustment of a value of x in the expression formula of (Er1-xDyx)3Al5O12, the multiband laser-prevention transparent ceramic material has special absorption capabilities at wavelengths of 525-540nm, 808nm, 880-920nm, 970nm and 1064nm, and satisfies people and equipment requirements on laser protection wavelength.
Description
Technical field
The present invention relates to a kind of Multi-wavelength Laser Protective transparent ceramic material and preparation method thereof, Absorbable rod is in the laser of ultraviolet, visible ray and near-infrared region different wave length, is mainly used in lasing safety field, is particularly useful for the protection of high energy blinding laser.
Background technology
Satellite, spacecraft, space station etc. often become without the object of attack under the modernized war pattern of the smoke of gunpowder.When it is subject to the attack of laser weapon, if effectively protected, then can cause the instability of serviceability, even cause the damage of equipment.In existing lasing safety technology, mostly adopt the protective material comprising glass, phase-change thin film and organic dye type.Although these material for laser light can form good absorption, these protective material spininess, to the protection of the laser of a certain specific wavelength, limit its use range; Meanwhile, these material at high temperature physics, poor chemical stability, easily aging, and structural failure and permanent failure is easily caused under superlaser irradiation.In addition, organic dye, Semiconductor Powder etc. in the plastic dispersiveness are difficult to control, and glass material easily causes component segregation in preparation process, and are difficult to the protective material constructing composite configuration.
Garnet-base transparent ceramic has high optical transmittance, and the feature such as high optical homogeneity, high temperature resistant, high strength, high heat conductance, has excellent resisting laser damage performance, more and more extensive in field application such as solid lasers.Its rare earth ion doped amount is high, not easily segregation, by the mode of solid solution, can prepare the transparent ceramic material of Absorbable rod different-waveband laser.In addition, by the technique simply laminated, the material of multilayer, multi-functional composite structure can be prepared.In technology of preparing, crystalline ceramics have can large size preparation, the short advantage of preparation cycle, the ceramic component of complex configuration can be designed to simultaneously.
Summary of the invention
The object of the invention is to provide a kind of Multi-wavelength Laser Protective transparent ceramic material to improve the deficiencies in the prior art, another object of the present invention is to provide the preparation method of above-mentioned Multi-wavelength Laser Protective transparent ceramic material.
Technical scheme of the present invention is: a kind of Multi-wavelength Laser Protective transparent ceramic material, is characterized in that: transparent ceramic material composition expression formula is (Er
1-xdy
x)
3al
5o
12, wherein 0.005≤x≤1.
Present invention also offers the preparation method of above-mentioned Multi-wavelength Laser Protective transparent ceramic material, adopt vacuum solid sintering technology to be prepared from, its concrete steps are as follows:
(1) according to chemical general formula (Er
1-xdy
x)
3al
5o
12, accurately take required α-Al
2o
3, Er
2o
3, Dy
2o
3powder; In material powder, add sintering aid, sintering aid is made up of jointly tetraethoxy (TEOS) and magnesium oxide (MgO) simultaneously; By above-mentioned raw materials powder and sintering aid blended, carry out ball milling mixing, then dry and sieve, the ceramic powder compound needed for acquisition;
(2) ceramic powder first adopts axially unidirectional pressuring method to carry out pre-molding, and after through cold isostatic compaction, form biscuit;
(3) shaping biscuit forms through 1720 ~ 1850 DEG C of vacuum sinterings, and soaking time is 6 ~ 12h;
(4) in air atmosphere anneal hour is carried out to the pottery of vacuum sintering; Sample twin polishing after annealing, the preventing laser crystalline ceramics of obtained high optical quality.
The add-on of preferred tetraethoxy accounts for 0.5 ~ 0.8% of material powder quality, and magnesian add-on accounts for 0.03 ~ 0.1% of material powder quality.
Drying temperature in preferred steps (1) is 60 ~ 80 DEG C, and time of drying is 12 ~ 24h.Sieving as crossing 200 mesh sieves described in preferred steps (1).
In preferred steps (2), the pressure of cold isostatic compaction is 150 ~ 300MPa.In preferred steps (3), the vacuum tightness of vacuum sintering is 10
-4~ 10
-3pa.
In preferred steps (4), the temperature of anneal is 1400 ~ 1550 DEG C, and the time of anneal is 4 ~ 10 hours.
By controlling chemical general formula (Er
1-xdy
x)
3al
5o
12the size of middle x value, can change the relative proportion of Dy and Er in crystalline ceramics, makes crystalline ceramics obtain corresponding laser absorption function in different laser wave strong points such as 525 ~ 540nm, 808nm, 880 ~ 920nm, 970nm and 1064nm.
Beneficial effect:
The present invention adopts the technique of vacuum solid state sintering to prepare the crystalline ceramics had, and it has strong absorption characteristic to 525 ~ 540nm, 808nm, 880 ~ 920nm, 970nm and 1064nm laser.Crystalline ceramics is as matrix, and the material prepared has high optical quality, thickness be the block ceramic of 5mm in visible light wave range place transmitance higher than 55%; Overcome an incident component segregation difficult problem in the material preparation process such as glass, the material homogeneity prepared is good simultaneously.In addition, the preparation technology of crystalline ceramics is simple, and easily preparation has the preventing laser transparent ceramic material of complex configuration; In crystalline ceramics matrix, Dy and Er can infinitely solid solution, thus pass through the solid solution capacity of simple control Dy, namely adjustable material is to the specific absorption of 1064nm, 808nm, 880 ~ 920nm and 530nm, 970nm laser, it has vital role in the superlaser protection of the special dimensions such as satellite window, spacecraft, space station, protective ocular.
Accompanying drawing illustrates:
Fig. 1 is the thickness that the invention process case 1 provides is the Dy of 5mm
3al
5o
12the transmittance curve of crystalline ceramics;
Fig. 2 is the thick (Er of 1mm that the invention process case 2 provides
0.5dy
0.5)
3al
5o
12the transmittance curve of single-phase composite transparent ceramic;
Fig. 3 is the thickness that the invention process case 3 provides is (the Er of 1mm
0.5dy
0.5)
3al
5o
12the transmittance curve of crystalline ceramics.
Embodiment:
Below in conjunction with specific examples, the invention will be further described.
Embodiment 1
A kind of preventing laser material of the present invention, according to Dy
3al
5o
12chemical general formula, precise α-Al
2o
312.2352g, Dy
2o
326.8560g, and add MgO powder 0.0390g and high-purity TEOS reagent 0.1955g as complex sintering aids, adopt planetary mills fully to mix.Slurry after ball milling after dry 24 hours, grinds and crosses 200 mesh sieves in the constant temperature oven of 60 DEG C.Take the ceramic powder 7.5g after grinding, after pre-molding, carry out isostatic cool pressing process, pressure is 300MPa, obtains fine and close biscuit.Biscuit adopts vacuum reaction technology to sinter, and be heated to 1840 DEG C, be incubated 10 hours, vacuum tightness is 10
-3pa.After furnace cooling in 1540 DEG C of annealing furnaces anneal 10h.After twin polishing, obtain High-quality transparent pottery.The light of this crystalline ceramics to 1064nm, 808nm, 880 ~ 920nm, 355nm, 200 ~ 275nm wave band has the absorption of more than 99.5%, and especially, at 1064nm, 808nm place, specific absorption is up to 99.99%.At visible light wave range, there is higher optical transmittance simultaneously.The Dy that 5mm is thick
3al
5o
12the transmittance curve of crystalline ceramics as shown in Figure 1.
Embodiment 2
A kind of two waveband lasing safety transparent ceramic material of the present invention, according to (Er
0.5dy
0.5)
3al
5o
12chemical general formula, precise α-Al
2o
33.5686g, Dy
2o
33.9165g, Er
2o
34.0165g, and add 0.0035g MgO powder and the high-purity TEOS reagent of 0.0920g as complex sintering aids, blended rear employing planetary mills fully mixes.Slurry after ball milling after dry 24 hours, grinds and crosses 200 mesh sieves in the constant temperature oven of 60 DEG C.Take the ceramic powder 2g after grinding, after pre-molding, carry out isostatic cool pressing process, pressure is 150MPa, obtains fine and close biscuit.Biscuit adopts vacuum reaction technology to sinter, and be heated to 1780 DEG C, be incubated 6 hours, vacuum tightness is 10
-4pa.After furnace cooling in 1450 DEG C of annealing furnaces anneal 4 hours.After twin polishing, obtain High-quality transparent pottery.The light of this crystalline ceramics to 524nm, 650nm, 1064nm, 970nm, 808nm, 880 ~ 920nm, 355nm, 200 ~ 275nm wave band has strong absorption, has higher optical transmittance at some visible light wave band simultaneously.(the Er that 1mm is thick
0.5dy
0.5)
3al
5o
12the transmittance curve of crystalline ceramics as shown in Figure 2.
Embodiment 3
A kind of two waveband lasing safety transparent ceramic material of the present invention, according to (Er
0.995dy
0.005)
3al
5o
12chemical general formula, precise α-Al
2o
310.1960g, Er
2o
322.8364g, Dy
2o
30.1119g, and add 0.0165g MgO powder and the high-purity TEOS reagent of 0.1988g as complex sintering aids, blended rear employing planetary mills fully mixes.Slurry after ball milling after dry 24 hours, grinds and crosses 200 mesh sieves in the constant temperature oven of 60 DEG C.Take the ceramic powder 4g after grinding, after pre-molding, carry out isostatic cool pressing process, pressure is 200MPa, obtains fine and close biscuit.Biscuit adopts vacuum reaction technology to sinter, and be heated to 1720 DEG C, be incubated 12 hours, vacuum tightness is 10
-4pa.After furnace cooling in 1400 DEG C of annealing furnaces anneal 5 hours.After twin polishing, obtain High-quality transparent pottery.The light of this crystalline ceramics to 524nm, 530nm, 650nm, 970nm wave band has strong absorption, has higher optical transmittance at some visible light wave band simultaneously.(the Er that 1mm is thick
0.995dy
0.005)
3al
5o
12the transmittance curve of crystalline ceramics as shown in Figure 3.
Claims (8)
1. a Multi-wavelength Laser Protective transparent ceramic material, is characterized in that: transparent ceramic material composition expression formula is (Er
1-xdy
x)
3al
5o
12, wherein 0.005≤x≤1.
2. prepare a method for Multi-wavelength Laser Protective transparent ceramic material as claimed in claim 1, its concrete steps are as follows:
(1) according to chemical general formula (Er
1-xdy
x)
3al
5o
12, accurately take required α-Al
2o
3, Er
2o
3, Dy
2o
3powder; In material powder, add sintering aid, sintering aid is made up of jointly tetraethoxy and magnesium oxide simultaneously; By above-mentioned raw materials powder and sintering aid blended, carry out ball milling mixing, then dry and sieve, the ceramic powder compound needed for acquisition;
(2) ceramic powder first adopts axially unidirectional pressuring method to carry out pre-molding, and after through cold isostatic compaction, form biscuit;
(3) shaping biscuit forms through 1720 ~ 1850 DEG C of vacuum sinterings, and soaking time is 6 ~ 12h;
(4) in air atmosphere anneal hour is carried out to the pottery of vacuum sintering; Sample twin polishing after annealing, the preventing laser crystalline ceramics of obtained high optical quality.
3. method according to claim 2, it is characterized in that the add-on of tetraethoxy accounts for 0.5 ~ 0.8% of material powder quality, magnesian add-on accounts for 0.03 ~ 0.1% of material powder quality.
4. method according to claim 2, it is characterized in that the drying temperature in step (1) is 60 ~ 80 DEG C, time of drying is 12 ~ 24h.
5. method according to claim 2, is characterized in that sieving as crossing 200 mesh sieves described in step (1).
6. method according to claim 2, is characterized in that the pressure of cold isostatic compaction in step (2) is 150 ~ 300MPa.
7. method according to claim 2, is characterized in that the vacuum tightness of vacuum sintering in step (3) is 10
-4~ 10
-3pa.
8. method according to claim 2, it is characterized in that the temperature of anneal in step (4) is 1400 ~ 1550 DEG C, the time of anneal is 4 ~ 10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510161523.9A CN104829220B (en) | 2015-04-07 | 2015-04-07 | A kind of Multi-wavelength Laser Protective transparent ceramic material and preparation method thereof |
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|---|---|---|---|
| CN201510161523.9A CN104829220B (en) | 2015-04-07 | 2015-04-07 | A kind of Multi-wavelength Laser Protective transparent ceramic material and preparation method thereof |
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| CN104829220B CN104829220B (en) | 2017-03-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106316373A (en) * | 2016-07-29 | 2017-01-11 | 江苏罗化新材料有限公司 | Preparing method for high power illuminant fluoride florescent and crystalline ceramics |
Citations (4)
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|---|---|---|---|---|
| CN101284733A (en) * | 2007-04-10 | 2008-10-15 | 中国科学院上海硅酸盐研究所 | Yttrium aluminium garnet and yttria double crystal transparent ceramic and method for making same |
| CN101798228A (en) * | 2009-12-18 | 2010-08-11 | 贵州大学 | Synthesis method for preparing yttrium aluminum garnet ceramic powder material through laser sintering and product |
| CN101851096A (en) * | 2009-04-03 | 2010-10-06 | 中国科学院上海硅酸盐研究所 | Highly doped Yb, Er: YAG transparent ceramic and manufacturing method thereof |
| CN103205254A (en) * | 2013-04-10 | 2013-07-17 | 中国科学院福建物质结构研究所 | White-light LED (light-emitting diode) containing novel solid-state transparent fluorescent materials and preparation method thereof |
-
2015
- 2015-04-07 CN CN201510161523.9A patent/CN104829220B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284733A (en) * | 2007-04-10 | 2008-10-15 | 中国科学院上海硅酸盐研究所 | Yttrium aluminium garnet and yttria double crystal transparent ceramic and method for making same |
| CN101851096A (en) * | 2009-04-03 | 2010-10-06 | 中国科学院上海硅酸盐研究所 | Highly doped Yb, Er: YAG transparent ceramic and manufacturing method thereof |
| CN101798228A (en) * | 2009-12-18 | 2010-08-11 | 贵州大学 | Synthesis method for preparing yttrium aluminum garnet ceramic powder material through laser sintering and product |
| CN103205254A (en) * | 2013-04-10 | 2013-07-17 | 中国科学院福建物质结构研究所 | White-light LED (light-emitting diode) containing novel solid-state transparent fluorescent materials and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106316373A (en) * | 2016-07-29 | 2017-01-11 | 江苏罗化新材料有限公司 | Preparing method for high power illuminant fluoride florescent and crystalline ceramics |
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| CN104829220B (en) | 2017-03-01 |
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