CN101280456A - Growing method by Ti3O5 by bridgman method - Google Patents

Growing method by Ti3O5 by bridgman method Download PDF

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Publication number
CN101280456A
CN101280456A CNA2007101736046A CN200710173604A CN101280456A CN 101280456 A CN101280456 A CN 101280456A CN A2007101736046 A CNA2007101736046 A CN A2007101736046A CN 200710173604 A CN200710173604 A CN 200710173604A CN 101280456 A CN101280456 A CN 101280456A
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temperature
crucible
growth
crystal
furnace
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CN101280456B (en
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李新华
吴宪君
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Suzhou Jingsheng New Material Co., Ltd
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SHANGHAI JINGSHENG INDUSTRIAL Co Ltd
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Abstract

The invention provides the bridgman growing method for the growth of Ti3O5 crystal, which includes that (1) the raw materials TiO2 and Ti are in proportioning according to Ti3O5 and mixed evenly, pressed. (2) The raw briquetting is loaded in a crucible that then transferred to the inside of a high-temperature decreasing furnace, and the whole system is heated and pumped to 10-3-10-4Pa. When the furnace temperature reaches 1400 to 1700 DEG C, the furnace is charged with an insert protection gas and continuously heated to 1800 to 1900 DEG C. (3) When the temperature reaches the set temperature, the heat is preserved for 3 to 6 hours so that the raw materials can be fully melted. The temperature gradient of solid-liquid interface for the crystal growth is within a framework of 20 to 60 DEG C/cm, and the crucible decline rate is between 0.1 to 5.0mm/h. (4) After the end of the crystal growth, in an appropriate position inside the growing furnace, the heat is preserved for 10 to 24 hours. Afterwards, the furnace temperature is reduced to a room temperature with the speed of 25 to 80 DEG C/h. The annealing treatment is implemented for the growing crystals.

Description

Five oxidation Tritanium/Trititanium crystalline Bridgman-Stockbarger methods
Technical field
The present invention relates to a kind of crystalline Bridgman-Stockbarge method for growing technology, promptly use Bridgman-Stockbarge method for growing five oxidations three titanium crystals, belong to field of crystal growth.
Background technology
Five oxidation Tritanium/Trititanium (Ti 3O 5) crystal belongs to rhombic system, density～4.60g/cm3, fusing point～1760 ℃.Ti 3O 5It is metastable compound in the low price series oxide compound of titanium, have the metalloid characteristic, have very high electroconductibility at normal temperatures, compare with the noble metal electrode material, it is cheap, acid-alkali-corrosive-resisting is strong, therefore can substitute precious metal as electrode materials.Ti 3O 5Be a kind of non-stoichiometric compound, O/Ti can change between 1.66-1.70, and a large amount of oxygen rooms is contained in its inside, and quasi-free electron concentration is higher, and its resistance can change with the change of atmosphere, is a kind of potential oxygen-sensitive material therefore.
At present, Ti 3O 5As titanium dioxide (TiO 2) the evaporation target of coating is widely used in the manufacturing of opto-electronic device, as the integrated device of technique of display, imaging technique, light output and light etc.TiO 2Rete has very high specific refractory power, satisfactory stability and stability in visible light and near infrared spectral range.In earlier stage, people mainly use TiO 2Coating materials comes evaporation TiO 2Coating, but TiO 2Coating materials can discharge a large amount of oxygen in the heating and the process of fritting, even carry out sufficient preheating, sputter is still inevitable, and is difficult to obtain thickness homogeneous, rete that specific refractory power is stable.Along with going deep into of research, it is found that TiO 2Its chemical constitution is about Ti after the coating materials fritting 3O 5Thereby, can cause emitting of a large amount of oxygen; And, if TiO 2Coating materials fritting insufficient, the discordance of its melt composition then can cause being difficult to obtain the rete of stable optical feature.And if use Ti 3O 5Then can avoid TiO as deposition material 2The shortcoming of coating materials reduces discharge quantity, avoids sputter, obtains thickness homogeneous, high-performance rete that specific refractory power is stable.Now, Ti 3O 5Coating materials progressively replaces TiO 2Coating materials and in high index film material, occupy main status.
At present, be used to prepare TiO 2The Ti of coating 3O 5The coating materials major part is a polycrystalline ceramics.Polycrystalline ceramics Ti 3O 5Though preparation is with low cost 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 TiO 2The film decisive role.Therefore, in order to satisfy light, electricity application to high quality Ti 3O 5The demand of material, Ti 3O 5The crystalline preparation has also just become the task of top priority.Be compared to polycrystalline ceramics, Ti 3O 5Crystal structure is better, and density is bigger; In addition, utilize the characteristic of crystal self impurities removal in the process of growth, can also improve the purity of material.Ti 3O 5Crystal is widely used as a kind of high index film material, but about Ti 3O 5The research report of crystal preparation does not then almost have, and therefore, is starved of a kind of Ti that can grow at lower cost 3O 5The crystalline method is so that advantageously carry out suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide the Ti that a kind of working method is simple, growth is with low cost 3O 5The crystal Bridgman-Stockbarger method is to realize this crystalline industrialization preparation.
The invention provides a kind of growth five oxidation Tritanium/Trititanium crystalline Bridgman-Stockbarger methods, may further comprise the steps:
(1) with raw material TiO 2Press Ti with Ti 3O 5Batching mixes, briquetting;
(2) during the raw material that step (1) is obtained briquetting was packed crucible into, crucible was transferred in the high temperature decline stove, and total system is heated up and is evacuated to 10 -3-10 -4Pa charges into inert protective gas when furnace temperature reaches 1400-1700 ℃, continue to be warming up to design temperature, and described design temperature is in 1800-1900 ℃ scope;
(3) after furnace temperature reaches design temperature, be incubated 3-6 hour, make the raw material fusing fully, the temperature gradient of solid-liquid interface of crystal growth is in the scope of 20-60 ℃/cm, and the crucible fall off rate is controlled between the 0.1-5.0mm/h;
(4) treat that crystal growth finishes after, the appropriate location insulation is 10-24 hour in growth furnace, with the speed of 25-80 ℃/h furnace temperature is reduced to room temperature then, and the crystal of being grown is carried out anneal.
In a specific embodiment of the present invention, described crucible be shaped as required shape, described crucible is the high temperature material that is selected from molybdenum, tungsten or miramint.
In a specific embodiment of the present invention, the temperature gradient of solid-liquid interface of the described crystal growth in the step (1) is set in the scope of 30-50 ℃/cm; The crucible fall off rate is controlled between the 1.0-4.0mm/h.
In a specific embodiment of the present invention, the speed with 25-50 ℃/h in the step (1) is carried out anneal.
In a specific embodiment of the present invention, in crystal furnace, lay many crucibles, each crucible has equal growth conditions and work efficiency, to realize a stove many crucibles Ti that grows simultaneously 3O 5Crystal.
In a specific embodiment of the present invention, described raw material TiO 2Purity is more than 99.9 weight % reach, and the purity of Ti is more than 99.99 weight % reach.
Embodiment
The present invention realizes by following technological approaches.At first with high-purity initial feed TiO 2(99.9%) and Ti (99.99%) press Ti 3O 5Chemical constitution is prepared burden, is mixed, and at 1.0-5.0t/cm 2Wait briquetting under the static pressure; the briquetting material is put into crucible; crucible is placed crystal growing furnace; vacuumize, be warming up to 1400-1700 ℃ after, charge into inert protective gas; continue to be warming up to the raw material temperature of fusion again; raw material is melted fully, 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 high-quality Ti 3O 5Crystal.
Below to Ti of the present invention 3O 5The crystalline Bridgman-Stockbarger method is elaborated.This growth method mainly may further comprise the steps:
1. the pre-treatment of raw material: with TiO 2(99.9%) and Ti (99.999%) press Ti 3O 5Chemical constitution batch mixes, mixed powder are ground on mortar or shredder to mix, as required briquetting on isostatic pressing machine;
2. the briquetting material that step 1. is obtained is packed in the molybdenum crucible, and molybdenum crucible is transferred 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 -3-10 -4Pa charges into inert protective gas when furnace temperature reaches 1400-1700 ℃, continue to be warming up to design temperature, and described design temperature is in 1800-1900 ℃ scope;
3. after furnace temperature reaches design temperature, be incubated 3-6 hour, make raw material fusing fully, the solid-liquid interface place thermograde of crystal growth is set in the scope of 20-60 ℃/cm, the crucible fall off rate is controlled between the 0.1-5.0mm/h;
4. after crystal growth finished, insulation 10-24h in appropriate location reduced to room temperature with the speed of 25-80 ℃/h then in growth furnace, is more preferably with the speed of 25-50 ℃/h and reduces to room temperature.Handle by this in-situ annealing, can eliminate the thermal stresses of crystals, reduce lattice defect.
In the step of raw materials pretreatment, raw material TiO preferably 2Purity 99.9% and more than, the purity of raw material Ti 99.99% and more than, the size of material piece is decided according to situation such as the size of crucible.
Used crucible preferably is selected from the high temperature material of molybdenum, tungsten or miramint.The shape of crucible can be decided according to growth needs, for example can be rectangular cylindricality, cylindrical, cube cylindricality or other Polygons.
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 argon gas, helium, nitrogen or other rare gas elementes.Argon gas especially preferably, its purity preferably 99.99% and more than.
In processing method of the present invention, can design many crucibles high-temperature growth furnace according to industrial scale, realize laying in the stove scale production of many crucibles thus, to improve the crystalline growth efficiency, to reduce production costs.
In melting process of raw material, the method for melt raw material is not specifically limited, as long as make the raw material fusing fully.For example by suitable adjusting fire box temperature and bushing position, make raw material melt particularly.
In annealing process, the concrete grammar of cooling without limits, as long as make described crystal lower the temperature according to required cooling rate.Particularly for example, can make crystal reduce to room temperature by regulating bushing position and thermograde after crystal growth finishes.
The Ti that utilizes Bridgman-Stockbarger method of the present invention to make 3O 5Crystal has following characteristics: component is even, does not have common black dephasign; Good crystallinity is difficult for broken; Density is big, and discharge quantity is few.
Ti 3O 5The specific refractory power (n) of crystal under different wave length (λ) is as shown in table 1, and measuring method is followed " GB/T7962.12-1987 colouless optical glass testing method ".
Table 1 Ti 3O 5The relation of crystalline specific refractory power (n) and wavelength (λ)
Wavelength (nm) 400 560 666 773 880 986 1146
Specific refractory power (n) 2.521 2.309 2.260 2.234 2.218 2.207 2.197
Bridgman-Stockbarge method for growing Ti of the present invention 3O 5The crystalline growth method 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) processing unit is simple, and is easy to operate, and average energy consumption is low;
(4) crystal of being grown can in time carry out anneal, with the thermal stresses of elimination crystals remnants,
(5) by Proper Design, can place a plurality of crucibles in same stove, the many crystal of growing are simultaneously realized a stove fecund thus, help saving energy consumption, reduce production costs and realize the 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.
Embodiment 1
With purity 99.9% TiO 2Press Ti with 99.99% Ti 3O 5The 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 the briquetting material is placed cylindrical molybdenum crucible.Molybdenum crucible places in the decline stove, adjusts to the position, high-temperature zone, and total system sealing back energising heats up, and successively starts mechanical pump, diffusion pump, is evacuated to 10 -3Pa charges into 99.99% argon gas when furnace temperature arrives 1500 ℃, continue to be warming up to 1850 ℃, is incubated 3 hours raw material is melted fully, and the growth interface thermograde maintains about 30 ℃/cm, and the speed decline crucible with 1.0mm/h grows Ti 3O 5Crystal is according to GB/T 7962.12-1987 colouless optical glass testing method, described Ti 3O 5The specific refractory power (n) of crystal under wavelength 560nm (λ) is 2.309.
Embodiment 2
With purity 99.9% TiO 2Press Ti with 99.99% Ti 3O 5The 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 nahlock; Then the briquetting material is placed cylindrical molybdenum crucible.Molybdenum crucible places in the decline stove, adjusts to the position, high-temperature zone, and total system sealing back energising heats up, and is evacuated to 10 -4Pa charges into 99.99% argon gas when furnace temperature arrives 1600 ℃, continue to heat up, and Control for Kiln Temperature at 1800 ℃, is incubated 4 hours, and raw material is melted fully, and the growth interface thermograde is about 50 ℃/cm, and the speed decline crucible with 3.0mm/h grows Ti 3O 5Crystal.According to GB/T 7962.12-1987 colouless optical glass testing method, described Ti 3O 5The specific refractory power (n) of crystal under wavelength 560nm (λ) is 2.308.
Embodiment 3
With purity 99.9% TiO 2Press Ti with 99.99% Ti 3O 5The chemical constitution batch mixes, mixed powder ground and mixed on mortar or shredder is even, is pressed into nahlock; Be respectively charged in the molybdenum crucible of 3 diameter 70mm, place the high temperature decline stove with 3 bushing positions then, adjust to the position, high-temperature zone, total system sealing back energising heats up, and is evacuated to 10 -3Pa charges into 99.99% argon gas when furnace temperature arrives 1700 ℃, continue to heat up, with Control for Kiln Temperature at 1900 ℃.That adjusts 3 crucibles respectively goes into the stove position, is incubated 3 hours, and raw material is melted fully, and the growth interface thermograde is about 60 ℃/cm, and the crucible fall off rate is 3.0mm/h, can obtain 3 crucible Ti simultaneously 3O 5Crystal.According to GB/T 7962.12-1987 colouless optical glass testing method, described Ti 3O 5The specific refractory power (n) of crystal under wavelength 560nm (λ) is 2.307.
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 (6)

  1. One kind the growth five oxidation Tritanium/Trititanium crystalline Bridgman-Stockbarger methods, may further comprise the steps:
    (1) with raw material TiO 2Press Ti with Ti 3O 5Batching mixes, briquetting;
    (2) during the raw material that step (1) is obtained briquetting was packed crucible into, crucible was transferred in the high temperature decline stove, and total system is heated up and is evacuated to 10 -3-10 -4Pa charges into inert protective gas when furnace temperature reaches 1400-1700 ℃, continue to be warming up to design temperature, and described design temperature is in 1800-1900 ℃ scope;
    (3) after furnace temperature reaches design temperature, be incubated 3-6 hour, make the raw material fusing fully, the temperature gradient of solid-liquid interface of crystal growth is in the scope of 20-60 ℃/cm, and the crucible fall off rate is controlled between the 0.1-5.0mm/h;
    (4) treat that crystal growth finishes after, the appropriate location insulation is 10-24 hour in growth furnace, with the speed of 25-80 ℃/h furnace temperature is reduced to room temperature then, and the crystal of being grown is carried out anneal.
  2. 2. growth method according to claim 1 is characterized in that, described crucible be shaped as required shape, described crucible is the high temperature material that is selected from molybdenum, tungsten or miramint.
  3. 3. growth method according to claim 1 is characterized in that, the temperature gradient of solid-liquid interface of the described crystal growth in the step (1) is set in the scope of 30-50 ℃/cm; The crucible fall off rate is controlled between the 1.0-4.0mm/h.
  4. 4. growth method according to claim 1 is characterized in that, the speed with 25-50 ℃/h in the step (1) is carried out anneal.
  5. 5. growth method according to claim 1 is characterized in that, lays many crucibles in crystal furnace, and each crucible has equal growth conditions and work efficiency, to realize a stove many crucibles Ti that grows simultaneously 3O 5Crystal.
  6. 6. growth method according to claim 1 is characterized in that, described raw material TiO 2Purity is more than 99.9 weight % reach, and the purity of Ti is more than 99.99 weight % reach.
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103806100A (en) * 2014-02-12 2014-05-21 常州瞻驰光电科技有限公司 Vertical temperature gradient growing method of trititanium pentoxide polycrystal
CN103806099A (en) * 2014-01-20 2014-05-21 福州阿石创光电子材料有限公司 Method for preparing titanium oxide crystal
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
CN105506737A (en) * 2015-12-28 2016-04-20 常州瞻驰光电科技有限公司 Non-stoichiometric-ratio niobium oxide poly-crystal coating material and growing technology thereof
CN105887182A (en) * 2014-12-15 2016-08-24 盱眙新远光学科技有限公司 Preparation technology of trititanium pentoxide crystal
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
CN111217390A (en) * 2020-03-04 2020-06-02 四川大学 Lambda-Ti3O5Powder preparation method
CN114197041A (en) * 2021-12-14 2022-03-18 苏州科睿浦光电科技有限公司 Preparation method of trititanium pentoxide polycrystal material and trititanium pentoxide polycrystal material
CN115142137A (en) * 2021-12-14 2022-10-04 常州瞻驰光电科技股份有限公司 Novel optical coating material and preparation method thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103806099A (en) * 2014-01-20 2014-05-21 福州阿石创光电子材料有限公司 Method for preparing titanium oxide crystal
CN103806099B (en) * 2014-01-20 2016-01-13 福建阿石创新材料股份有限公司 The preparation method of five oxidation three titanium crystals
CN103806100B (en) * 2014-02-12 2016-05-04 常州瞻驰光电科技有限公司 A kind of terraced method growing method of vertical temperature of five oxidation Tritanium/Trititanium polycrystalline
CN103806100A (en) * 2014-02-12 2014-05-21 常州瞻驰光电科技有限公司 Vertical temperature gradient growing method of trititanium pentoxide polycrystal
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
CN105887182A (en) * 2014-12-15 2016-08-24 盱眙新远光学科技有限公司 Preparation technology of trititanium pentoxide crystal
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
CN105506737A (en) * 2015-12-28 2016-04-20 常州瞻驰光电科技有限公司 Non-stoichiometric-ratio niobium oxide poly-crystal coating material and growing technology thereof
CN105506737B (en) * 2015-12-28 2018-02-09 常州瞻驰光电科技有限公司 A kind of non-stoichiometric niobium oxide polycrystalline Coating Materials and its growing technology
CN111217390A (en) * 2020-03-04 2020-06-02 四川大学 Lambda-Ti3O5Powder preparation method
CN114197041A (en) * 2021-12-14 2022-03-18 苏州科睿浦光电科技有限公司 Preparation method of trititanium pentoxide polycrystal material and trititanium pentoxide polycrystal material
CN115142137A (en) * 2021-12-14 2022-10-04 常州瞻驰光电科技股份有限公司 Novel optical coating material and preparation method thereof
CN115142137B (en) * 2021-12-14 2024-02-13 常州瞻驰光电科技股份有限公司 Novel optical coating material and preparation method thereof

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