CN101050122A - Method for preparing functional ceramic of lithium niobate - Google Patents
Method for preparing functional ceramic of lithium niobate Download PDFInfo
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- CN101050122A CN101050122A CN 200710099428 CN200710099428A CN101050122A CN 101050122 A CN101050122 A CN 101050122A CN 200710099428 CN200710099428 CN 200710099428 CN 200710099428 A CN200710099428 A CN 200710099428A CN 101050122 A CN101050122 A CN 101050122A
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- laser irradiation
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- 239000000919 ceramic Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 18
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 230000005855 radiation Effects 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 40
- 238000000498 ball milling Methods 0.000 claims description 22
- PSVBHJWAIYBPRO-UHFFFAOYSA-N lithium;niobium(5+);oxygen(2-) Chemical compound [Li+].[O-2].[O-2].[O-2].[Nb+5] PSVBHJWAIYBPRO-UHFFFAOYSA-N 0.000 claims description 21
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000084 colloidal system Substances 0.000 claims description 12
- 238000005469 granulation Methods 0.000 claims description 12
- 230000003179 granulation Effects 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 235000015895 biscuits Nutrition 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 230000004447 accommodation reflex Effects 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 6
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 9
- 230000010287 polarization Effects 0.000 abstract description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract 1
- 229910052744 lithium Inorganic materials 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000001778 solid-state sintering Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
This invention relates to a method for preparing functional lithium niobate ceramic by laser radiation. The method comprises: preparing ceramic green body by traditional method, and sintering at 960-980 deg.C for 10-30 min by laser radiation. The method has such advantages as short period, little lithium volatilation during sintering, low polarization temperature of ceramic, easy operation, and high controllability.
Description
Technical field
The present invention relates to a kind of preparation method of function ceramics, particularly a kind of preparation method of Lithium niobium trioxide pottery.
Background technology
Lithium niobium trioxide (standard chemical formula: LiNbO
3) crystal is that present known Curie temperature the highest (1210 ℃) and spontaneous polarization maximum (are about 0.70C/m during room temperature
2) ferroelectrics, belong to trigonal system, 3m point group.It is a kind of current collection light, acousto-optic, piezoelectricity, photoelastic, non-linear, light is sold off and effect rare crystal such as laser activity, have a wide range of applications in fields such as optical information storage, electro-optical device and surface acoustic wave devices.
For many years, Lithium niobium trioxide is widely studied and applied with the monocrystalline form, and the research report of relevant Lithium niobium trioxide pottery but seldom.Major cause is that each step of the preparation technology of Lithium niobium trioxide pottery all exists suitable difficulty.The volatilization of Li when being in particular in sintering, coercive field and polarization temperature are high.At present, the preparation of Lithium niobium trioxide pottery mainly is to adopt traditional solid state reaction sintering process, but this method sintering period is grown, can't monitor in real time.To the tight demand of leadless piezoelectric ceramics, Lithium niobium trioxide pottery excellent ferroelectric is subjected to extensive concern along with in recent years, and the lithium niobate base leadless piezoelectric ceramics has become the another important leadless piezoelectric ceramics system after BNT.Therefore, shorten preparation technology, prepare and be easy to the emphasis that polar Lithium niobium trioxide pottery becomes this research field.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art and provide a kind of preparation quickly and easily to be easy to the method for polar Lithium niobium trioxide pottery.
The object of the present invention is achieved like this: be prepared with the following step:
(1) raw material is prepared: raw materials used is the congruent Lithium niobium trioxide powder of purity 99.9%;
(2) ball milling: with pack in same ball grinder ball milling 8～12 hours of load weighted powder;
(3) oven dry: the slurry behind the ball milling was dried under 70～90 ℃ temperature 12～16 hours;
(4) sieve: the powder after the oven dry is sieved by 180 purpose screen clothes;
(5) add the glue granulation: the PVAC polyvinylalcohol colloid that adds 6% quality percentage composition in powder carries out granulation, and the mass ratio of colloid and powder is 1: 25～1: 15, sieves with 40 purpose screen clothes after mixing again;
(6) compression molding: use tabletting machine under the pressure of 150～200MPa, the powder pressure to be formed sheet;
(7) laser irradiation: accommodation reflex mirror, make laser radiation that laser apparatus 1 sends center at worktable, biscuit of ceramics 4 is positioned on the central position of worktable, improve laser power, with 3～5 fens clock times the ceramic surface temperature is brought up to 960～980 ℃ earlier, beginning laser irradiation process, after 10～30 minutes laser irradiation, laser power is reduced to zero gradually with 3～5 minutes times, laser closes light, and pottery is placed cooling.
Described laser apparatus 1 is a carbon dioxide laser.
Compared with prior art, beneficial effect of the present invention is:
(1) shortens preparation cycle, reduced the volatilization of Li in the sintering process;
(2) the prepared functional ceramic of lithium niobate of the present invention under the 100V/cm current field condition, the polarization temperature just can make when reaching 980 ℃ and ceramicly polarize smoothly and obtain bigger piezoelectric constant d
33,, help using far below 1200 ℃ of the polarization temperature values of traditional solid state sintering;
(3) laser sintered process is at room temperature carried out, and is simple to operate, and controllability is strong, and repeatability is high.
Description of drawings
Fig. 1 laser irradiation experimental installation synoptic diagram
Among the figure: 1, laser apparatus, 2, laser beam, 3, speculum, 4, biscuit of ceramics, 5, worktable, 6, the integral mirror system, 7, infrared thermometer;
The Raman spectrogram of the pottery that the pottery of Fig. 2 embodiment 1 preparation and traditional solid sintering technology are prepared.
Embodiment
Be described in further details below in conjunction with embodiment:
1) raw material: test raw material is the congruent Lithium niobium trioxide powder of purity 99.9%
2) ball milling: it is organic jar that powder is packed into, is solvent with the dehydrated alcohol, volume account for organic jar 2/3, then with ZrO
2Ceramic Balls is as ball-milling medium, and ball milling is 8 hours on ball mill;
3) oven dry: pour the slip behind the ball milling into the glass square position, put into baking oven and under 80 ℃ temperature, dried 12 hours;
4) sieve: the powder after the oven dry sieves through 180 purpose screen clothes;
5) add the glue granulation: the PVAC polyvinylalcohol colloid that adds 6% quality percentage composition in powder carries out granulation, and the mass ratio of colloid and powder is 1: 25, sieves with 40 purpose screen clothes after mixing again;
6) compressing tablet: use electronic balance to take by weighing some parts of powders, adopt unidirectional dry pressing, under the pressure of 150MPa, the powder pressure is formed diameter 13mm by every part of 1g, the round ceramic sheet of thickness 2mm, the time that keep-ups pressure is 1 minute;
7) laser irradiation: according to Fig. 1, adopting rated output is that 1 pair of Lithium niobium trioxide biscuit of ceramics of HX-150WL type carbon dioxide laser of 150W carries out laser irradiation, and laser is by integral mirror system 6, light beam be shaped to light intensity evenly, the length of side is the square hot spot of 8mm.Accommodation reflex mirror 3, make the center of laser radiation at worktable 5, biscuit of ceramics 4 is positioned near the center of worktable 5 on the position, improves laser power, adopt infrared thermometer 7 to monitor in real time, earlier the ceramic surface temperature is brought up to 980 ℃ with 5 fens clock times, beginning laser irradiation process after 30 minutes laser irradiation, is reduced to laser power density zero with 5 minutes times gradually, laser closes light, and pottery is placed cooling.
1) raw material: test raw material is the congruent Lithium niobium trioxide powder of purity 99.9%
2) ball milling: it is organic jar that powder is packed into, is solvent with the dehydrated alcohol, volume account for organic jar 2/3, then with ZrO
2Ceramic Balls is as ball-milling medium, and ball milling is 10 hours on ball mill;
3) oven dry: pour the slip behind the ball milling into the glass square position, put into baking oven and under 70 ℃ temperature, dried 16 hours;
4) sieve: the powder after the oven dry sieves through 180 purpose screen clothes;
5) add the glue granulation: the PVAC polyvinylalcohol colloid that adds 6% quality percentage composition in powder carries out granulation, and the mass ratio of colloid and powder is 1: 25, sieves with 40 purpose screen clothes after mixing again;
6) compressing tablet: use electronic balance to take by weighing some parts of powders, adopt unidirectional dry pressing, under the pressure of 150MPa, the powder pressure is formed diameter 13mm by every part of 1g, the round ceramic sheet of thickness 2mm, the time that keep-ups pressure is 1 minute;
7) laser irradiation: according to Fig. 1, adopting rated output is that 1 pair of Lithium niobium trioxide biscuit of ceramics of HX-150WL type carbon dioxide laser of 150W carries out laser irradiation, and laser is by integral mirror system 6, light beam be shaped to light intensity evenly, the length of side is the square hot spot of 8mm.Accommodation reflex mirror 3, make the center of laser radiation at worktable 5, biscuit of ceramics 4 is positioned near the center of worktable 5 on the position, improves laser power, adopt infrared thermometer 7 to monitor in real time, earlier the ceramic surface temperature is brought up to 960 ℃ with 4 fens clock times, beginning laser irradiation process after 30 minutes laser irradiation, is reduced to laser power density zero with 4 minutes times gradually, laser closes light, and pottery is placed cooling.
Embodiment 3
1) raw material: test raw material is the congruent Lithium niobium trioxide powder of purity 99.9%
2) ball milling: it is organic jar that powder is packed into, is solvent with the dehydrated alcohol, volume account for organic jar 2/3, then with ZrO
2Ceramic Balls is as ball-milling medium, and ball milling is 10 hours on ball mill;
3) oven dry: pour the slip behind the ball milling into the glass square position, put into baking oven and under 90 ℃ temperature, dried 14 hours;
4) sieve: the powder after the oven dry sieves through 180 purpose screen clothes;
5) add the glue granulation: the PVAC polyvinylalcohol colloid that adds 6% quality percentage composition in powder carries out granulation, and the mass ratio of colloid and powder is 1: 20, sieves with 40 purpose screen clothes after mixing again;
6) compressing tablet: use electronic balance to take by weighing some parts of powders, adopt unidirectional dry pressing, under the pressure of 180MPa, the powder pressure is formed diameter 13mm by every part of 1g, the round ceramic sheet of thickness 2mm, the time that keep-ups pressure is 1 minute;
7) laser irradiation: according to Fig. 1, adopting rated output is that 1 pair of Lithium niobium trioxide biscuit of ceramics of HX-150WL type carbon dioxide laser of 150W carries out laser irradiation, and laser is by integral mirror system 6, light beam be shaped to light intensity evenly, the length of side is the square hot spot of 8mm.Accommodation reflex mirror 3, make the center of laser radiation at worktable 5, biscuit of ceramics 4 is positioned near the center of worktable 5 on the position, improves laser power, adopt infrared thermometer 7 to monitor in real time, earlier the ceramic surface temperature is brought up to 970 ℃ with 3 fens clock times, beginning laser irradiation process after 20 minutes laser irradiation, is reduced to laser power density zero with 5 minutes times gradually, laser closes light, and pottery is placed cooling.
1) raw material: test raw material is the congruent Lithium niobium trioxide powder of purity 99.9%
2) ball milling: it is organic jar that powder is packed into, is solvent with the dehydrated alcohol, volume account for organic jar 2/3, then with ZrO
2Ceramic Balls is as ball-milling medium, and ball milling is 12 hours on ball mill;
3) oven dry: pour the slip behind the ball milling into the glass square position, put into baking oven and under 80 ℃ temperature, dried 16 hours;
4) sieve: the powder after the oven dry sieves through 180 purpose screen clothes;
5) add the glue granulation: the PVAC polyvinylalcohol colloid that adds 6% quality percentage composition in powder carries out granulation, and the mass ratio of colloid and powder is 1: 15, sieves with 40 purpose screen clothes after mixing again;
6) compressing tablet: use electronic balance to take by weighing some parts of powders, adopt unidirectional dry pressing, under the pressure of 200MPa, the powder pressure is formed diameter 13mm by every part of 1g, the round ceramic sheet of thickness 2mm, the time that keep-ups pressure is 1 minute;
7) laser irradiation: according to Fig. 1, adopting rated output is that 1 pair of Lithium niobium trioxide biscuit of ceramics of HX-150WL type carbon dioxide laser of 150W carries out laser irradiation, and laser is by integral mirror system 6, light beam be shaped to light intensity evenly, the length of side is the square hot spot of 8mm.Accommodation reflex mirror 3, make the center of laser radiation at worktable 5, biscuit of ceramics 4 is positioned near the center of worktable 5 on the position, improves laser power, adopt infrared thermometer 7 to monitor in real time, earlier the ceramic surface temperature is brought up to 980 ℃ with 5 fens clock times, beginning laser irradiation process after 10 minutes laser irradiation, is reduced to laser power density zero with 3 minutes times gradually, laser closes light, and pottery is placed cooling.
Lithium niobium trioxide pottery by above scheme is prepared polarizes under the 100V/cm current field condition, and measured polarization temperature is minimum can to reach 980 ℃, piezoelectric constant d
33Reach 6.0pC/N, measured result is listed as follows:
| Embodiment | The polarization temperature (unit: ℃) | Piezoelectric constant d 33(unit: pC/N) |
| 1 | 980 | 6.0 |
| 2 | 980 | 5.5 |
| 3 | 990 | 5.8 |
| 4 | 995 | 5.6 |
The Lithium niobium trioxide pottery of embodiment 1 and traditional solid-phase sintering method being prepared by Raman spectrogram (Fig. 2) compares, and finds that the Raman peaks of embodiment 1 prepared pottery shows slightly sharply, and live width is slightly narrow.Because the ratio of spectral line live width reflection [Li]/[Nb] illustrates the laser sintered volatilization that helps reducing Li in the sintering process.
Claims (2)
1, the preparation method of functional ceramic of lithium niobate may further comprise the steps:
1) raw material is prepared: raw materials used is the congruent Lithium niobium trioxide powder of purity 99.9%;
2) ball milling: with pack in same ball grinder ball milling 8～12 hours of load weighted powder;
3) oven dry: the slurry behind the ball milling was dried under 70～90 ℃ temperature 12～16 hours;
4) sieve: the powder after the oven dry is sieved by 180 purpose screen clothes;
5) add the glue granulation: the PVAC polyvinylalcohol colloid that adds 6% quality percentage composition in powder carries out granulation, and the mass ratio of colloid and powder is 1: 25～1: 15, sieves with 40 purpose screen clothes after mixing again;
6) compression molding: use tabletting machine under the pressure of 150～200MPa, the powder pressure to be formed sheet;
It is characterized in that, further comprising the steps of:
7) laser irradiation: accommodation reflex mirror (3), make laser radiation that laser apparatus (1) sends center in worktable (5), biscuit of ceramics (4) is positioned on the central position of worktable (5), improve laser power, with 3～5 fens clock times the ceramic surface temperature is brought up to 960～980 ℃ earlier, beginning laser irradiation process, after 10～30 minutes laser irradiation, laser power is reduced to zero gradually with 3～5 minutes times, laser closes light, and pottery is placed cooling.
2, the preparation method of functional ceramic of lithium niobate according to claim 1 is characterized in that: described laser apparatus (1) is a carbon dioxide laser.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100994286A CN101050122B (en) | 2007-05-21 | 2007-05-21 | Method for preparing functional ceramic of lithium niobate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100994286A CN101050122B (en) | 2007-05-21 | 2007-05-21 | Method for preparing functional ceramic of lithium niobate |
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| Publication Number | Publication Date |
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| CN101050122A true CN101050122A (en) | 2007-10-10 |
| CN101050122B CN101050122B (en) | 2010-07-07 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206092A (en) * | 2011-03-17 | 2011-10-05 | 南开大学 | Preparation method and preparation materials of Er-doped lithium niobate porous material |
| CN111939647A (en) * | 2016-07-05 | 2020-11-17 | 北京中科艾加科技有限公司 | Pyroelectric crystal particle, application thereof, composite material and screening method |
| CN114773058A (en) * | 2022-03-24 | 2022-07-22 | 华南理工大学 | Anion functional material and preparation method and application thereof |
-
2007
- 2007-05-21 CN CN2007100994286A patent/CN101050122B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206092A (en) * | 2011-03-17 | 2011-10-05 | 南开大学 | Preparation method and preparation materials of Er-doped lithium niobate porous material |
| CN102206092B (en) * | 2011-03-17 | 2013-01-09 | 南开大学 | Preparation method and preparation materials of Er-doped lithium niobate porous material |
| CN111939647A (en) * | 2016-07-05 | 2020-11-17 | 北京中科艾加科技有限公司 | Pyroelectric crystal particle, application thereof, composite material and screening method |
| CN111939647B (en) * | 2016-07-05 | 2022-07-15 | 北京中科艾加科技有限公司 | Pyroelectric crystal particle, application thereof, composite material and screening method |
| CN114773058A (en) * | 2022-03-24 | 2022-07-22 | 华南理工大学 | Anion functional material and preparation method and application thereof |
| CN114773058B (en) * | 2022-03-24 | 2023-06-20 | 华南理工大学 | Negative ion functional material and preparation method and application thereof |
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| CN101050122B (en) | 2010-07-07 |
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