CN103243388A - Method for heating and melting precast shaped filler in sapphire crystal growth - Google Patents
Method for heating and melting precast shaped filler in sapphire crystal growth Download PDFInfo
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- CN103243388A CN103243388A CN2013101143563A CN201310114356A CN103243388A CN 103243388 A CN103243388 A CN 103243388A CN 2013101143563 A CN2013101143563 A CN 2013101143563A CN 201310114356 A CN201310114356 A CN 201310114356A CN 103243388 A CN103243388 A CN 103243388A
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Abstract
The invention discloses a method for heating and melting a precast shaped filler in sapphire crystal growth, which comprises the following steps: starting a heating system to heat from 25 DEG C to 1650 DEG C, wherein the heating gradient is 200 DEG C/h; and after the temperature reaches 1650 DEG C, changing the temperature increase gradient to 30 DEG C/h, and further heating to 2000 DEG C until a block material is completely molten. The precast shaped filler disclosed by the invention causes less bubble defects in comparison with a crystal block treated by a flame method; the packed density of the precast shaped filler can be up to 2.6-2.8 g/cm<3>; and more materials can be filled under the condition of not changing the size of a crucible, thereby meeting the requirements for the density of the raw material in large-size sapphire crystal growth in China at present.
Description
Technical field
The present invention relates to sapphire crystal growing technology field, relate to the method for the temperature increasing for melting materials in the long crystalline substance of a kind of sapphire, relate in particular to the method for the precasting shape filler temperature increasing for melting materials in the long crystalline substance of a kind of sapphire.
Background technology
Utilized oxyhydrogen flame fusing natural ruby powder to make sensational " Geneva ruby " at that time with potassium bichromate from 1885 by Fremy, Feil and Wyse, the research of artificial growing sapphire so far has the history in more than 100 year.During this period, in order to adapt to science and technology development and industrial production for the particular requirement of sapphire crystal quality, size, shape, for the yield rate, the utilization ratio that improve sapphire crystal and reduce cost, sapphire growth method and correlation theory thereof have been carried out a large amount of research, and achievement is remarkable.So far having had higher state of the art and bigger throughput, for it the crystal growth equipment of adequate and systematic service---single crystal growing furnace has also obtained development at full speed thereupon.Along with the rapid expansion of sapphire crystal application market, its equipment and technology have also obtained development rapidly in last century end.Crystalline size expands 12 present inch to from 2 inch.
Low-cost, growing large-size sapphire single-crystal has become the current urgent task that faces in high quality.All things considered, the sapphire crystal growth mode can be divided into three kinds of solution growths, melt growth, vapor phase growth, wherein melt growth mode is fast because having growth velocity, characteristics such as purity height and perfection of crystal are good are the most frequently used crystal growth patterns of preparation large size and specified shape crystal and become.The method with the artificial growing sapphire crystal of melt growth mode of can be used at present mainly contains flame melt method, crystal pulling method, zone melting method, guided mode method, crucible and moves method, heat-exchanging method, temperature gradient method, kyropoulos etc.
The raw material that is used for Sapphire Crystal Growth at present is mainly bulk crystals material, particulate material, pie material and processing back residue scrap stock, and raw material is placed crucible, and a series of processes such as processization material grow up to sapphire crystal.
The form difference of raw material, the long brilliant method difference of sapphire, the method difference of catching up with bubble.
The crystal block material of flame method is the cost height not only, makes relatively difficulty of its littleization, and big space has appearred in when filling with substance, adopts other forms filling spaces therebetween of powder or powder usually.
The briquetting material that powder and powder are prepared, particulate material because impurities in the raw material may form bubble in heat-processed, influence yield rate and the quality of sapphire crystal in growing crystal.
Precasting shape polycrystal is α-Al
2O
3Powder through solidification and crystallization after the fusion, has been got rid of pore and a part of impurity in the powder through the melting once after the complete fusion, is applicable to that the c axle prepares large-size sapphire to the requirement of raw material.The raising of tamped density has correspondingly improved the loadings of crucible, has increased the output of sapphire crystal.
The brilliant thermograde of ky furnace superintendent is big, and general the employing is higher than about 50 ℃～100 ℃ of sapphire fusing points, and long-time the immersion caught up with bubble.
Heat-exchanging method c axial length crystalline substance, thermograde is little, and seed crystal is in the bottom, and it is limited to cross melting temperatur.
Originalization of precasting shape filler material method: temperature is raised to 1247 ℃ from 25 ℃, and the slope that wherein heats up is 353 ℃/h; When temperature reached 1247 ℃, the intensification slope was 183 ℃/h, was warmed up to 2000 ℃ always, changed little intensification slope again, kept 2065 ℃ to melt fully to the piece material.
Precasting shape filler adopts the cold crucible material, and the cold crucible material is changed the material excessive velocities not as the densification of crystal block material, and the donor center micropore can be closed very soon, and bubble is failed to overflow and is wrapped in the melt; Because the melt viscosity is big, make that bubble is difficult for discharging simultaneously.
Therefore, at above-mentioned technical problem, be necessary to provide a kind of method of precasting shape filler temperature increasing for melting materials of optimization, to overcome above-mentioned defective.
Summary of the invention
In view of this, the object of the present invention is to provide the method for the precasting shape filler temperature increasing for melting materials in the long crystalline substance of a kind of sapphire, precasting shape filler can be at air blister defect than not many with the flame method crystal block, and the situation that does not change the crucible size realizes many chargings.
For achieving the above object, the invention provides following technical scheme:
The method of the precasting shape filler temperature increasing for melting materials in the long crystalline substance of sapphire of the present invention starts heating system, and temperature is raised to 1650 ℃ from 25 ℃, and the slope that wherein heats up is 200 ℃/h; When temperature reaches after 1650 ℃, revising temperature, to increase slope be 30 ℃/h, is warmed up to 2000 ℃ always and melts fully to the piece material.
The present invention makes gas have enough passages and time to overflow in changing the material process by slowing down material speed, and along with the rising of temperature, raw material can shrink gradually, and reaches higher density, reduces the air bubble content in the melt, thereby helps to reduce the crystal air bubble content.
Precasting shape filler air blister defect of the present invention is not than many with the flame method crystal block, and precasting shape filler can tamped density reach 2.6-2.8g/cm
3, can realize many chargings in the situation that does not change the crucible size, meet present domestic growing large-size sapphire crystal to the requirement of material density.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art, to do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below, apparently, accompanying drawing relevant of the present invention in describing below only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the correlation curve synoptic diagram of the method for prior art and precasting shape filler temperature increasing for melting materials of the present invention.
Embodiment
The invention discloses the method for the precasting shape filler temperature increasing for melting materials in the long crystalline substance of a kind of sapphire, start heating system, temperature is raised to 1650 ℃ from 25 ℃, and the slope that wherein heats up is 200 ℃/h; When temperature reaches after 1650 ℃, revising temperature, to increase slope be 30 ℃/h, is warmed up to 2000 ℃ always and melts fully to the piece material.
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is described in detail, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, the every other embodiment that those of ordinary skills obtain under the prerequisite of not making creative work belongs to the scope of protection of the invention.
The size of precasting material shape:
Conical part is filled with the cold crucible particle, the barrel portion crystal ingot of casting in advance, and the crystal ingot size is stayed not filler of gap less than the 10mm to 20mm of crucible internal diameter between crucible and the crystal ingot, and the crystal ingot height is less than crucible height 70mm, reserving space.The density of sapphire liquid state is 3.05, and liquid level can be than filling the material level height behind the change material.
Originalization material method: temperature is raised to 1247 ℃ from 25 ℃, and the slope that wherein heats up is 353 ℃/h; When temperature reached 1247 ℃, the intensification slope was 183 ℃/h, was warmed up to 2000 ℃ always, changed little intensification slope again, kept 2065 ℃ to melt fully to the piece material, shown in accompanying drawing 1 original parametric line.
Of the present inventionization material method: temperature is raised to 1650 ℃ from 25 ℃, and the slope that wherein heats up is 200 ℃/h; When temperature reaches after 1650 ℃, revising temperature, to increase slope be 30 ℃/h, is warmed up to 2000 ℃ always and melts fully to the piece material, revises shown in the parametric line of back as accompanying drawing 1.
Contrast is found, first section intensification slope of of the present inventionization material method and second section intensification slope all are lower than originalization material method, the process of wholeization material is able to mildization, considering material excessive velocities, the donor center micropore can be closed very soon, bubble is failed to overflow and is wrapped in the melt, simultaneously because the melt viscosity is big, makes that bubble is difficult for discharging.By slowing down material speed, make gas in changing the material process, have enough passages and time to overflow, along with the rising of temperature, raw material can shrink gradually, and reaches higher density, reduces the air bubble content in the melt, thereby helps to reduce the crystal air bubble content.
In sum, precasting shape filler air blister defect of the present invention is not than many with the flame method crystal block, and precasting shape filler can tamped density reach 2.6-2.8g/cm
3, can realize many chargings in the situation that does not change the crucible size, meet present domestic growing large-size sapphire crystal to the requirement of material density.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and under the situation that does not deviate from spirit of the present invention or essential characteristic, can realize the present invention with other specific form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims rather than above-mentioned explanation, therefore is intended to include in the present invention dropping on the implication that is equal to important document of claim and all changes in the scope.Any Reference numeral in the claim should be considered as limit related claim.
In addition, be to be understood that, though this specification sheets is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets only is for clarity sake, those skilled in the art should make specification sheets as a whole, and the technical scheme among each embodiment also can form other embodiments that it will be appreciated by those skilled in the art that through appropriate combination.
Claims (2)
1. the method for the precasting shape filler temperature increasing for melting materials in the long crystalline substance of sapphire is characterized in that, comprises the steps:
Start heating system, temperature is raised to 1650 ℃ from 25 ℃, and the slope that wherein heats up is 200 ℃/h, and when temperature reaches after 1650 ℃, revising temperature, to increase slope be 30 ℃/h, is warmed up to 2000 ℃ always and melts fully to the piece material.
2. the application of the described method of claim 1 in the growing sapphire monocrystalline.
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| CN2013101143563A CN103243388A (en) | 2013-04-02 | 2013-04-02 | Method for heating and melting precast shaped filler in sapphire crystal growth |
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| CN2013101143563A CN103243388A (en) | 2013-04-02 | 2013-04-02 | Method for heating and melting precast shaped filler in sapphire crystal growth |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106676624A (en) * | 2017-03-31 | 2017-05-17 | 宁夏佳晶科技有限公司 | Guide mode processing method for flaky sapphire |
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| EP1380674A2 (en) * | 1999-01-20 | 2004-01-14 | Canon Kabushiki Kaisha | Apparatus and process for producing crystal article, and thermocouple used therein |
| US20040099206A1 (en) * | 2002-08-24 | 2004-05-27 | Lothar Ackermann | Process and device for growing single crystals |
| CN101109103A (en) * | 2007-07-10 | 2008-01-23 | 中国科学院上海光学精密机械研究所 | Method for growing crystal by high vacuum temperature gradient method |
| CN101580963A (en) * | 2009-06-26 | 2009-11-18 | 哈尔滨工大奥瑞德光电技术有限公司 | SAPMAC method for preparing sapphire single-crystal with size above 300mm |
| CN102162130A (en) * | 2011-05-26 | 2011-08-24 | 浙江昀丰新能源科技有限公司 | Preparation method of sapphire monocrystalline |
| CN102634845A (en) * | 2012-02-07 | 2012-08-15 | 徐州协鑫光电科技有限公司 | Method for heating and melting materials in growth of sapphire single crystals by Kyropoulos method and application thereof |
-
2013
- 2013-04-02 CN CN2013101143563A patent/CN103243388A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1380674A2 (en) * | 1999-01-20 | 2004-01-14 | Canon Kabushiki Kaisha | Apparatus and process for producing crystal article, and thermocouple used therein |
| US20040099206A1 (en) * | 2002-08-24 | 2004-05-27 | Lothar Ackermann | Process and device for growing single crystals |
| CN101109103A (en) * | 2007-07-10 | 2008-01-23 | 中国科学院上海光学精密机械研究所 | Method for growing crystal by high vacuum temperature gradient method |
| CN101580963A (en) * | 2009-06-26 | 2009-11-18 | 哈尔滨工大奥瑞德光电技术有限公司 | SAPMAC method for preparing sapphire single-crystal with size above 300mm |
| CN102162130A (en) * | 2011-05-26 | 2011-08-24 | 浙江昀丰新能源科技有限公司 | Preparation method of sapphire monocrystalline |
| CN102634845A (en) * | 2012-02-07 | 2012-08-15 | 徐州协鑫光电科技有限公司 | Method for heating and melting materials in growth of sapphire single crystals by Kyropoulos method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106676624A (en) * | 2017-03-31 | 2017-05-17 | 宁夏佳晶科技有限公司 | Guide mode processing method for flaky sapphire |
| CN106676624B (en) * | 2017-03-31 | 2019-01-29 | 宁夏佳晶科技有限公司 | A kind of guided mode processing method of flaky sapphire |
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Application publication date: 20130814 |