CN101063232A - Lanthanum titanates single-crystal and upgrowth technology thereof - Google Patents
Lanthanum titanates single-crystal and upgrowth technology thereof Download PDFInfo
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- CN101063232A CN101063232A CN 200710041328 CN200710041328A CN101063232A CN 101063232 A CN101063232 A CN 101063232A CN 200710041328 CN200710041328 CN 200710041328 CN 200710041328 A CN200710041328 A CN 200710041328A CN 101063232 A CN101063232 A CN 101063232A
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Abstract
The invention discloses a lanthanum titanate crystal with chemical composition as La2Ti2O7 and growing technology, which comprises the following steps: (1) adopting TiO2 and La2O3 as initial raw material; choosing the usage ration in pursuance of chemical composition of La2Ti2O7; mixing evenly; briquetting; (2) transferring copple with briquette raw material of the step (1) into vacuum reduced furnace; heating the whole system; evacuating to 10-2-10-4Pa; charging into inert protective gas when temperature at 1500-1700 deg. c; heating to setting temperature continually; setting the setting temperature at 1850-1950 deg. c; (3) adjusting the position of copple in furnace tank; melting the raw material and seed crystal top; realizing seeding growth; controlling solid-liquid interface thermal gradient of crystal growth at 20-80 deg. c/cm; controlling dropped ratio at 0. 2-10mm/h; (4) finishing the crystal growth; decreasing the temperature to room temperature with 30-120 deg. c/h speed; annealing for crystal. This product possesses good crystallization property, big dielectric constant and high refracting power.
Description
Technical field
The present invention relates to a kind of lanthanum titanates single-crystal, and the growth method of preparation lanthanum titanates single-crystal, more specifically relate to the lanthanum titanates single-crystal of high dielectric, high refractive index and the Bridgman-Stockbarge method for growing technology of this monocrystalline.The invention belongs to the single crystal growing field.
Background technology
Lanthanium titanate crystal La
2Ti
2O
7(the following LTO that abbreviates as sometimes) belongs to oblique system, perovskite-like structure, and the spacer under the room temperature is P2
1The LTO crystal has good ferroelectric, photochemical catalysis, electro-optical characteristic, in light, the electrical domain prospect that is widely used.It has very high Curie temperature (1500 ℃) and very big coercive field (45kV/cm), can be applied on pyritous electro-optic device and the message memory, as high temperature frequency transformer, ferroelectric RAM (FRAM) etc.In recent years, microwave technology has obtained fast development, and the application in every field is also increasingly extensive, so the work of development of new high performance microwave dielectric material also just more and more is subjected to numerous scientific research personnel's attention, and the LTO crystal has high specific inductivity (ε
r=42-62), low dielectric temperature coefficient and dielectric loss (100kHz-1MHz), so it has become the research focus at home and abroad as a kind of important microwave dielectric material.Simultaneously, it also has good piezoelectric property, can be used for making devices such as pyrostat and microwave piezoelectrics.In addition, LTO also has outstanding photocatalytic activity, has a good application prospect at aspects such as water decomposition reaction, fuel cell and other energy conversion techniques.In China, rare earth element is of a great variety especially, and reserves are abundant, for the research of LTO crystalline provides advantageous platform.
Along with going deep into of research, people find that also LTO can be used as the coated material of excellent performance and is applied in the manufacturing of opto-electronic device, as the integrated device of technique of display, imaging technique, light output and light etc.The LTO coated material has stable high specific refractory power, high uniformity and high transmitance.At present, LTO has been widely used in the manufacturing of high-performance optical electrical part as coated material, and China still is in space state in this field; As on the precision optics manufacturing platform, owing to lack advanced material, China also is in the production phase of low side technical products.
At present, the target that is used to prepare the LTO coated material adopts polycrystalline ceramics mostly, mainly prepares by methods such as low-temperature hydrothermal synthesis method, sol-gel method, high temperature solid phase synthesis, the precipitator method, organo-metallic decomposition methods.Though polycrystalline ceramics LTO preparation is easily, in preparation process, introduce impurity easily, form a large amount of pores, and be difficult to guarantee the homogeneity of composition and structure, and these factors are to preparing high-quality LTO film decisive role.
Therefore, in order to satisfy light, the electric demand of using high quality LTO material, the LTO monocrystalline has also just become the task of top priority.Be compared to polycrystalline ceramics, the LTO monocrystalline has more crystalline and does not have ceramic grain-boundary and glassy phase, utilizes the characteristic of crystal self impurities removal in the process of growth, can also improve crystalline purity.In addition, because therefore the growth cost of monocrystalline, is starved of a kind of technology of the LTO monocrystalline of can growing at lower cost, so that advantageously carry out suitability for industrialized production usually above polycrystalline ceramics.
Summary of the invention
An object of the present invention is to provide a kind of lanthanum titanates single-crystal.
Another object of the present invention provides a kind of growing technology of lanthanum titanates single-crystal.
One aspect of the present invention provides a kind of lanthanium titanate crystal, it is characterized in that, the chemical constitution of lanthanium titanate is La
2Ti
2O
7, described crystal is a monocrystalline.
The present invention provides a kind of growth lanthanium titanate La on the other hand
2Ti
2O
7The Bridgman-Stockbarge method for growing technology of monocrystalline, this technology may further comprise the steps:
(1) adopts TiO
2And La
2O
3As initial feed, both amount ratios are according to La
2Ti
2O
7Chemical constitution, mix briquetting;
(2) crucible that step (1) gained briquetting raw material will be housed moves in the breaking of vacuum stove, and total system is heated up and is evacuated to 10
-2-10
-4Pa charges into inert protective gas when furnace temperature rises to 1500-1700 ℃, continue to be warming up to design temperature, and described design temperature is in 1850-1950 ℃ scope;
(3) adjust the position of crucible in burner hearth, make the fusing of raw material and crystal seed top, realize the inoculation growth, the temperature gradient of solid-liquid interface of crystal growth is in the scope of 20-80 ℃/cm, and the crucible fall off rate is controlled between the 0.2-10mm/h;
(4) treat that crystal growth finishes after, with the speed of 30-120 ℃/h furnace temperature is reduced to room temperature, the crystal of being grown is carried out anneal.
In a preferred embodiment, in step (2), the crystal seed of packing in advance in the crucible.Be more preferably, the orientation of described crystal seed be selected from＜001,＜100,＜210,＜112,＜212 the direction of growth.Be more preferably, use the lanthanium titanate crystal as crystal seed, the ratio of the sectional area of this crystal seed and the crystalline sectional area of being grown be 10% and more than, i.e. 10-100%.
In a preferred embodiment, the shape of described crucible is selected from the polygon cylindricality of cylindrical, cube cylindricality, rectangular cylindricality or required growth.
In a preferred embodiment, the temperature gradient of solid-liquid interface with the described crystal growth in the step (3) is set in the scope of 40-70 ℃/cm.
In a preferred embodiment, the crucible fall off rate is controlled between the 1.0-3.0mm/h.
In a preferred embodiment, with in the step (4) with the speed of the 40-80 ℃/h back cooling anneal of growing.
In a preferred embodiment, lay many crucibles in crystal furnace, each crucible has equal growth conditions and work efficiency, to realize a stove many lanthanium titanate crystal of growing simultaneously.
In a preferred embodiment, use many crucible growth lanthanium titanate crystal of different wall.
In a preferred embodiment, the lanthanium titanate crystal of growth different orientation in same growth furnace.
In a preferred embodiment, described raw material La
2O
3Purity 99.999wt% and more than, TiO
2Purity 99.9wt% and more than.
Description of drawings
Fig. 1 is the x-ray diffractogram of powder spectrum of the lanthanum titanates single-crystal that makes of the embodiment of the invention 1.
Fig. 2 is two rocking curve figure of the lanthanum titanates single-crystal that makes of the embodiment of the invention 1.
Embodiment
The present invention realizes by following technological approaches.At first with high-purity initial feed TiO
2(99.9wt%) and La
2O
3(99.999wt%) press La
2Ti
2O
7Chemical constitution batching, uniform mixing and at 0.5-5t/cm
2Wait under the static pressure and forge into piece; the briquetting material is put into crucible with the crystal seed of optional certain orientation; crucible is placed crystal growing furnace; vacuumize, heat up, charge into inert protective gas after 1500-1700 ℃; continue to be warming up to the raw material temperature of fusion again; melt raw material and crystal seed top are by controlling furnace temperature, regulating temperature gradient of solid-liquid interface and select suitable processing parameters such as crucible fall off rate to realize the crystalline stable growth, to obtain complete transparent high quality LTO crystal.After treating that crystal growth finishes, the crystal of growing is carried out in-situ annealing handle.
Below the crucible melt growth technology of LTO monocrystalline of the present invention is elaborated.This growing technology mainly may further comprise the steps:
1. the pre-treatment of raw material: with high pure raw material TiO
2And La
2O
3Press La
2Ti
2O
7The chemical constitution batch mixes, mixed powder grinds to mix on mortar or shredder, forges into piece on isostatic pressing machine;
2. above-mentioned synthetic material and crystal seed are put into crucible, crucible moves on in the high temperature decline stove, adjusts to certain altitude, and total system sealing back energising heats up, and successively starts mechanical pump, diffusion pump, is evacuated to 10
-2-10
-4Pa charges into inert protective gas when furnace temperature arrives 1500-1700 ℃, continue to be warming up to design temperature 1850-1950 ℃;
3. adjust the position of crucible in burner hearth, fused raw material and crystal seed top and inoculation, growth gradually, the growth interface thermograde is controlled in the scope of 20-80 ℃/cm,, can obtains the complete LTO monocrystalline identical with the crucible shape with the speed decline crucible of 0.2-10mm/h;
4. after treating that crystal growth finishes, furnace temperature is reduced to room temperature, the crystal of growing is carried out in-situ annealing handle with the speed of 30-120 ℃/h.
In the step of raw materials pretreatment, preferably, raw material TiO
2Purity 99.9wt% and more than, raw material La
2O
3Purity 99.999wt% and more than.The size of material piece is decided according to situation such as crucible size.
There is no particular restriction to described inert protective gas for Technology of the present invention, if this gas neither the oxidation crucible again not with melt generation chemical reaction.Preferred inert protective gas can be such as but not limited to: argon gas, helium, nitrogen or other rare gas elementes.Argon gas especially preferably, its purity preferably 99.99 volume % and more than.
After furnace temperature reaches design temperature, be incubated 4-8 hour, raw material is constantly melted, form stable thermograde, the temperature gradient of solid-liquid interface of crystal growth maintains in the scope of 20-80 ℃/cm, and the crucible fall off rate is between 0.2-10mm/h.In crystal when growth inoculation, by adjust crucible in burner hearth the position and temperature gradient of solid-liquid interface finely tuned realizes optimized growth.
After crystal growth finishes, regulate bushing position and thermograde, the crystal of being grown being carried out in-situ annealing handle, specifically is to make crystal appropriate location in growth furnace of being grown reduce to room temperature with the speed of 30-120 ℃/h, finally obtains thus and the identical LTO crystal of crucible shape.Annealed processing can be eliminated the lattice defect that thermal stresses causes, and reduces crystal cleavage.
In Technology of the present invention, can be according to the shape and size of crystal application need design crucible, the LTO crystal of can grow different shapes, different size for example can be the shape of cylindrical, rectangular cylindricality, cube cylindricality or other actual needs.Can also design many crucibles high-temperature growth furnace according to industrial scale, realize laying in the stove scale production of many crucibles thus, obtain the LTO crystal of different orientation, different shapes, different size simultaneously.
The lanthanum titanates single-crystal that utilizes Bridgman-Stockbarge method for growing technology of the present invention to make has following characteristics: this monocrystalline belongs to oblique system, and its unit cell parameters is 1.30179nm; Two rocking curves of lanthanum titanates single-crystal as shown in Figure 2; Specific refractory power (n) under different wave length (λ) is as shown in table 1.
The relation of specific refractory power of table 1 lanthanum titanates single-crystal (n) and wavelength (λ)
| Wavelength (λ, nm) | 406.92 | 475.45 | 591.97 | 769.67 | 1139.3 |
| Specific refractory power (n) | 2.288 | 2.2098 | 2.1222 | 2.0658 | 1.9893 |
The lanthanum titanates single-crystal that the present invention makes has good crystal property, and does not have ceramic grain-boundary and glassy phase, utilizes the characteristic of crystal self impurities removal in the process of growth, has improved crystalline purity, and has high dielectric property and high refractive index.Lanthanum titanates single-crystal can satisfy the high request of light, electrical domain, has broad application prospects.
The growing technology of Bridgman-Stockbarge method for growing lanthanum titanates single-crystal of the present invention mainly has the following advantages:
(1) working method is simple, preparation cost is cheap, production efficiency is higher;
(2) warm field structure is stable, thermograde is adjustable;
(3) Sheng Chang crystalline size and profile are controlled;
(4) processing unit is simple, and is easy to operate, and average energy consumption is low;
(5) crystal of being grown can in time carry out anneal, with the thermal stresses of elimination crystals remnants,
(6) pass through Proper Design, can in same stove, place a plurality of crucibles, the many crystal of growing simultaneously, can also be according to the shape and size of crystal application need design crucible, obtain the LTO crystal of different orientation, different shapes, different size simultaneously, realize a stove fecund thus, single crystal on average consumes energy low, helps saving energy consumption and realizes LTO crystalline large-scale industrial production.
Substantive distinguishing features that the present invention gives prominence to and significant technical progress can fully show, but limit the present invention absolutely not that the present invention also absolutely not only is confined to following embodiment by following embodiment.The experimental technique of unreceipted actual conditions in the following example usually according to normal condition, or carries out according to the condition that manufacturer advises.
With purity is the TiO of 99.9wt%
2La with 99.999wt%
2O
3Press La
2Ti
2O
7The chemical constitution batch mixes, mixed powder ground and mixed on mortar or shredder is even, at 2t/cm
2The static pressure that waits depress to nahlock; Then with selected orientation＜001〉crystal seed place cylindrical crucible.Crucible places in the decline stove, adjusts to certain altitude, and total system sealing back energising heats up, and successively starts mechanical pump, diffusion pump, is evacuated to 10
-3Pa, when arriving 1500 ℃, furnace temperature charges into the argon gas of 99.99 volume %, continue to be warming up to 1850 ℃, melt raw material also makes the fusion of crystal seed top by adjusting the stove position, inoculate, growth, the growth interface thermograde maintains about 30 ℃/cm, with the speed decline crucible of 3mm/h, the cylindrical LTO crystal of growing.Crystal growth finishes the back and with the speed about 30 ℃/h furnace temperature is reduced to room temperature, opens bell, takes out crucible.
Gained LTO crystal is tested with RIGAKU D/max 2550V instrument, and the XRD figure that obtains as shown in Figure 1.Test with BRUKER D8 DISCOVER instrument, the two rocking curves that obtain as shown in Figure 2.By Fig. 1 and Fig. 2 as can be known, with growing technology of the present invention can access lanthanium titanate thing phase, crystalline quality good monocrystalline.
With purity is the TiO of 99.99wt%
2La with 99.999wt%
2O
3Press La
2Ti
2O
7The chemical constitution batch mixes, mixed powder ground and mixed on mortar or shredder is even, at 3t/cm
2The static pressure that waits depress to square; Then together with＜100〉the rectangular cylindricality crystal seed of direction puts into rectangular skittele pot.Crucible places in the decline stove, adjusts to certain altitude, and total system sealing back energising heats up, and is evacuated to 10
-4Pa charges into the argon gas of 99.99 volume % when furnace temperature arrives 1600 ℃, continue to heat up, at 1900 ℃, melt raw material and inoculation are grown with Control for Kiln Temperature, and the growth interface thermograde is about 60 ℃/cm, speed decline crucible with 8.8mm/h grows rectangular cylindricality LTO perfect crystal.Crystal growth finishes the back and with the speed about 60 ℃/h furnace temperature is reduced to room temperature, opens bell, takes out crucible.
Embodiment 3
With purity is the TiO of 99.9wt%
2La with 99.999wt%
2O
3Press La
2Ti
2O
7The chemical constitution batch mixes, mixed powder ground and mixed on mortar or shredder is even, is pressed into nahlock; Be respectively charged in the crucible of 3 diameter 70mm, place the high temperature decline stove with 3 bushing positions then, adjust to certain altitude, total system sealing back energising heats up, and is evacuated to 10
-2Pa charges into the argon gas of 99.99 volume % when furnace temperature arrives 1700 ℃, continue to heat up, with Control for Kiln Temperature at 1950 ℃.The stove position of going into of adjusting 3 crucibles respectively can both be inoculated the seed crystal in every crucible well, and the growth interface thermograde is about 70 ℃/cm, and the crucible fall off rate is 1.0mm/h, can obtain 3 cylindric LTO crystal simultaneously.Crystal growth finishes the back and with the speed about 80 ℃/h furnace temperature is reduced to room temperature, opens bell, takes out crucible.
Should be appreciated that after having read above-mentioned teachings of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (10)
1. a lanthanium titanate crystal is characterized in that, the chemical constitution of lanthanium titanate is La
2Ti
2O
7, described crystal is a monocrystalline.
2. growth lanthanium titanate La
2Ti
2O
7The Bridgman-Stockbarge method for growing technology of monocrystalline, this technology may further comprise the steps:
(1) adopts TiO
2And La
2O
3As initial feed, both amount ratios are according to La
2Ti
2O
7Chemical constitution, mix briquetting;
(2) crucible that step (1) gained briquetting raw material will be housed moves in the breaking of vacuum stove, and total system is heated up and is evacuated to 10
-2-10
-4Pa charges into inert protective gas when furnace temperature rises to 1500-1700 ℃, continue to be warming up to design temperature, and described design temperature is in 1850-1950 ℃ scope;
(3) adjust the position of crucible in burner hearth, make the fusing of raw material and crystal seed top, realize the inoculation growth, the temperature gradient of solid-liquid interface of crystal growth is in the scope of 20-80 ℃/cm, and the crucible fall off rate is controlled between the 0.2-10mm/h;
(4) treat that crystal growth finishes after, with the speed of 30-120 ℃/h furnace temperature is reduced to room temperature, the crystal of being grown is carried out anneal.
3. growing technology as claimed in claim 2 is characterized in that, in step (2), and the crystal seed of packing in advance in the crucible.
4. by claim 2 or 3 described growing technologies, it is characterized in that that the shape of described crucible is selected from is cylindrical, the polygon cylindricality of cube cylindricality, rectangular cylindricality or required growth.
5. by claim 2 or 3 described growing technologies, it is characterized in that, the temperature gradient of solid-liquid interface of the described crystal growth in the step (3) is set in the scope of 40-70 ℃/cm; And/or
The crucible fall off rate is controlled between the 1.0-3.0mm/h.
6. by claim 2 or 3 described growing technologies, it is characterized in that, the cooling anneal after growing with the speed of 40-80 ℃/h in the step (4).
7. by claim 2 or 3 described growing technologies, it is characterized in that lay many crucibles in crystal furnace, each crucible has equal growth conditions and work efficiency, to realize a stove many lanthanium titanate crystal of growing simultaneously;
Or, many crucibles growth lanthanium titanate crystal of use different wall;
Or, the lanthanium titanate crystal of growth different orientation in same growth furnace.
8. by the described growing technology of claim 3, it is characterized in that, the orientation of described crystal seed be selected from＜001,＜100,＜210,＜112,＜212 the direction of growth.
9. by the described growing technology of claim 3, it is characterized in that, use the lanthanium titanate crystal as crystal seed, the ratio of the sectional area of this crystal seed and the crystalline sectional area of being grown be 10% and more than.
10. by claim 2 or 3 described growing technologies, it is characterized in that described raw material La
2O
3Purity 99.999wt% and more than, TiO
2Purity 99.9wt% and more than.
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|---|---|---|---|---|
| CN104028285A (en) * | 2014-05-17 | 2014-09-10 | 北京工业大学 | Preparation method of Cu2ZnSnS4/La2Ti2O7 heterojunction photocatalytic composite material |
| CN104088015A (en) * | 2014-07-30 | 2014-10-08 | 上海晶生实业有限公司 | Bridgman-stockbarger growth method for zirconium titanate crystals |
| CN104389021A (en) * | 2014-11-06 | 2015-03-04 | 常州瞻驰光电科技有限公司 | Nonstoichiometric lanthanum titanate polycrystalline coating material and growth technology thereof |
| CN105645469A (en) * | 2016-03-09 | 2016-06-08 | 武汉科技大学 | Nano rodlike lanthanum titanate powder and preparation method thereof |
| CN105986316A (en) * | 2015-01-27 | 2016-10-05 | 常州瞻驰光电科技有限公司 | Tantalum oxide polycrystal film-coated material and growth method of same |
| CN106868477A (en) * | 2017-03-12 | 2017-06-20 | 苏州南尔材料科技有限公司 | A kind of method that colloidal sol rubbing method prepares metatitanic acid lanthanum film |
| CN107955963A (en) * | 2017-12-18 | 2018-04-24 | 中国科学院上海硅酸盐研究所 | A kind of La of float-zone method growth doping various concentrations Ta2Ti2O7The method of monocrystalline |
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|---|---|---|---|---|
| CN104028285A (en) * | 2014-05-17 | 2014-09-10 | 北京工业大学 | Preparation method of Cu2ZnSnS4/La2Ti2O7 heterojunction photocatalytic composite material |
| CN104088015A (en) * | 2014-07-30 | 2014-10-08 | 上海晶生实业有限公司 | Bridgman-stockbarger growth method for zirconium titanate crystals |
| CN104389021A (en) * | 2014-11-06 | 2015-03-04 | 常州瞻驰光电科技有限公司 | Nonstoichiometric lanthanum titanate polycrystalline coating material and growth technology thereof |
| CN105986316A (en) * | 2015-01-27 | 2016-10-05 | 常州瞻驰光电科技有限公司 | Tantalum oxide polycrystal film-coated material and growth method of same |
| CN105645469A (en) * | 2016-03-09 | 2016-06-08 | 武汉科技大学 | Nano rodlike lanthanum titanate powder and preparation method thereof |
| CN106868477A (en) * | 2017-03-12 | 2017-06-20 | 苏州南尔材料科技有限公司 | A kind of method that colloidal sol rubbing method prepares metatitanic acid lanthanum film |
| CN107955963A (en) * | 2017-12-18 | 2018-04-24 | 中国科学院上海硅酸盐研究所 | A kind of La of float-zone method growth doping various concentrations Ta2Ti2O7The method of monocrystalline |
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