CN101701357A - Growth method of lanthanum titanate crystal coated material - Google Patents
Growth method of lanthanum titanate crystal coated material Download PDFInfo
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- CN101701357A CN101701357A CN200910198956A CN200910198956A CN101701357A CN 101701357 A CN101701357 A CN 101701357A CN 200910198956 A CN200910198956 A CN 200910198956A CN 200910198956 A CN200910198956 A CN 200910198956A CN 101701357 A CN101701357 A CN 101701357A
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- crucible
- coated material
- lanthanum titanate
- titanate crystal
- insulation layer
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Abstract
A growth method of lanthanum titanate crystal coated material comprises the following specific steps: 1) weighting raw materials--titanium dioxide powder and lanthanum (III) oxide powder according to the stoichiometric ratio of molecular formula La2Ti2O7; 2) mixing the raw materials evenly, briquetting, sintering, placing the product in the crucible of a vacuum induction heating device; and 3) growing the lanthanum titanate crystal coated material by using vacuum induction heating and placing seed crystal from top. The method of the invention is characterized by easy operation of devices, safe and reliable running and possibility of mass production.
Description
Technical field
The present invention relates to Coating Materials, (molecular formula is La to particularly a kind of lanthanium titanate
2Ti
2O
7) growth method of crystal Coating Materials.
Background technology
Existing lanthanum titanate crystal coated material is to adopt the preparation of resistive heating crucible descending method.This method adopts big electric current energising heating heating element, the heating element heating, and the raw material in the heating crucible makes the raw material fusing.Slow decline crucible, crucible bottom is gradually away from heating element, and temperature slowly descends, and reaches the purpose of growing crystal.
There are several problems in this resistive heating crucible descending method:
1, through the heating element of low voltage, big electric current energising heating, between crucible and thermal insulation layer, spatial joint clearance is little, so insulation technology is strict.
2, this method need charge into inert protective gas in vacuum chamber, because gaseous exchange, heat runs off very fast, and power consumption is big.
3, in high temperature, high vacuum process of growth, crucible moves downward always, the equipment complexity, and vacuum technique requires high.
4, at first in the bottom growth, seed crystal is inserted crucible bottom to crystal, is difficult to observe, and technical difficulty is big.
Summary of the invention
The objective of the invention is to overcome the problem that above-mentioned existing resistive heating descending method growth lanthanum titanate crystal coated material exists, a kind of preparation method of lanthanum titanate crystal coated material is provided, this method adopts vacuum induction heating top seed crystal technology growth lanthanum titanate crystal coated material, has the advantages that operation of equipment is simple, safe and reliable to operation, energy-conservation relatively and production cost descends.
Technical solution of the present invention is as follows:
A kind of growth method of lanthanum titanate crystal coated material is characterized in the method that adopts vacuum induction heating and top to put the seeded growth lanthanum titanate crystal coated material.
This method comprises the following steps:
1. lanthanium titanate crystalline preparation of raw material:
Lanthanium titanate crystalline primary raw materials is TiO
2Powder and La
2O
3Powder is by following reaction formula 2TiO
2+ La
2O
3=La
2Ti
2O
7The stoichiometric ratio raw materials weighing, behind thorough mixing, briquetting,, make the piece material that crystal growth is used through 100～300 ℃ of oven dry;
2. described block of material packed in the crucible of vacuum induction heating unit, this vacuum induction heating unit comprises a crucible, be surrounded by thermal insulation layer, thermal insulation layer and following thermal insulation layer all around outside this crucible, outside the thermal insulation layer inductive coupler coils is being set around this, heat raw material in the described crucible by heating member, this inductive coupler coils links to each other with induction power supply, and whole vacuum induction heating unit places vacuum oven;
3. adopt vacuum induction heating and top to place the seeded growth lanthanum titanate crystal coated material:
After the inductive coupler coils energising, heat described crucible by electromagnetic coupled, piece material temperature in the crucible rises to 1800～1900 ℃, constant temperature, raw material is melted into melt fully in the crucible, with seed holder the lanthanium titanate seed crystal is placed the center on this melt feed top and immerses melt, seed crystal can partial melting, but must not all melt, and vacuum tightness is 4～20Pa in this moment stove, constant temperature 0.5～2 hour, with 50～100 ℃ rate of temperature fall per hour, slowly be cooled to below 1400 ℃ power cutoff through 8～10 hours then, reduce to room temperature with furnace temperature, promptly obtain lanthanum titanate crystal coated material.
Described crucible is made by iridium, molybdenum or tungsten refractory metal.
Described heating element is made by graphite.
Described go up thermal insulation layer, all around thermal insulation layer and down thermal insulation layer form by graphite, pyrocarbon felt, or form by oxide refractories.
Described seed holder is made up of refractory metal iridium, molybdenum, tungsten material, or has other metallic substance compositions of refrigerative.
Described induction power supply is intermediate frequency power supply or radio-frequency power supply.
Described crucible and described around also have the round shape heating member between the thermal insulation layer.
Technique effect of the present invention:
The present invention is owing to adopt induction coupling heating, and the coupling working coil is to be in the outer water cooled coil of device, has saved requisite low voltage strong current transformer in the electrical resistance heating.Since adopt the coupling heating, the passive heating of heating element or crucible, heating element does not have powered electrode, and insulation technology requires low.In crystal growing process, crucible remains static, the mechanism of the crucible that do not need to descend, and device is compact, and is easy to operate, safe and reliable to operation.Be grown under the vacuum and finish, reduced gaseous exchange, energy-saving effect is arranged.
Embodiment
The invention will be further described below in conjunction with embodiment, but should not limit protection scope of the present invention with this.
The growth method of lanthanum titanate crystal coated material, the method that adopts vacuum induction heating and top to put the seeded growth lanthanum titanate crystal coated material, this method comprises the following steps:
1. lanthanium titanate crystalline preparation of raw material:
Lanthanium titanate crystalline primary raw materials is TiO
2Powder and La
2O
3Powder is by following reaction formula 2TiO
2+ La
2O
3=La
2Ti
2O
7The stoichiometric ratio raw materials weighing, behind thorough mixing, briquetting,, make the piece material that crystal growth is used through 100～300 ℃ of oven dry;
2. described block of material packed in the crucible of vacuum induction heating unit, this vacuum induction heating unit comprises a crucible, be surrounded by thermal insulation layer, thermal insulation layer and following thermal insulation layer all around outside this crucible, outside the thermal insulation layer inductive coupler coils is being set around this, heat raw material in the described crucible by heating member, this inductive coupler coils links to each other with induction power supply, and whole vacuum induction heating unit places vacuum oven;
3. adopt vacuum induction heating and top to place the seeded growth lanthanum titanate crystal coated material:
After the inductive coupler coils energising, pass through electromagnetic coupled, heat described crucible, piece material temperature in the crucible rises to 1800～1900 ℃, constant temperature, raw material is melted into melt fully in the crucible, with seed holder the lanthanium titanate seed crystal is placed the center on this melt feed top and is immersed in melt, and seed crystal can partial melting, but must not all melt, vacuum tightness is 4～20Pa in this moment stove, and constant temperature 0.5～2 hour is then with 50～100 ℃ rate of temperature fall per hour, slowly be cooled to below 1400 ℃ through 8～10 hours, power cutoff is reduced to room temperature with furnace temperature, promptly obtains Coating Materials lanthanium titanate crystal.
Following table has provided the concrete growth parameter(s) of three embodiment:
| Embodiment | 1 | 2 | 3 |
| The primary raw materials input amount | 10 kilograms | 10 kilograms | 10 kilograms |
| Vacuum tightness | Be better than 20Pa | Be better than 10Pa | Be better than 5Pa |
| The highest thermostat temperature | 1850 ℃ | 1900 ℃ | 1950 ℃ |
| Constant temperature time | 2 hours | 1 hour | 0.5 hour |
| Temperature-fall period | 50 ℃ rate of temperature fall, power cutoff after lowering the temperature slowly in 10 hours. | 80 ℃ rate of temperature fall, power cutoff after slowly lowering the temperature in 9 hours. | 100 ℃ rate of temperature fall, power cutoff after slowly lowering the temperature in 8 hours. |
Experiment shows: adopt apparatus of the present invention and processing method growth lanthanum titanate crystal coated material, and size 0.5～20mm, yield rate is more than 70% preferably.The present invention has the advantages that operation of equipment is simple, safe and reliable to operation, energy-conservation relatively and production cost descends.
Claims (8)
1. the growth method of a lanthanum titanate crystal coated material is characterized in that the method that adopts vacuum induction heating and top to put the seeded growth lanthanum titanate crystal coated material.
2. the growth method of lanthanum titanate crystal coated material according to claim 1 is characterized in that this method comprises the following steps:
1. lanthanium titanate crystalline preparation of raw material:
Lanthanium titanate crystalline primary raw materials is TiO
2Powder and La
2O
3Powder is by following reaction formula 2TiO
2+ La
2O
3=La
2Ti
2O
7The stoichiometric ratio raw materials weighing, behind thorough mixing, briquetting,, make the piece material that crystal growth is used through 100～300 ℃ of oven dry;
2. described block of material packed in the crucible of vacuum induction heating unit, this vacuum induction heating unit comprises a crucible, be surrounded by thermal insulation layer, thermal insulation layer and following thermal insulation layer all around outside this crucible, outside the thermal insulation layer inductive coupler coils is being set around this, heat raw material in the described crucible by heating member, this inductive coupler coils links to each other with induction power supply, and whole vacuum induction heating unit places vacuum oven;
3. adopt vacuum induction heating and top to place the seeded growth lanthanum titanate crystal coated material:
After the inductive coupler coils energising, heat described crucible by electromagnetic coupled, piece material temperature in the crucible rises to 1800～1900 ℃, constant temperature, raw material is melted into melt fully in the crucible, with seed holder the lanthanium titanate seed crystal is placed the center on this melt feed top and is immersed in melt, seed crystal can partial melting, but must not all melt, and vacuum tightness is 4～20Pa in this moment stove, constant temperature 0.5～2 hour, with 50～100 ℃ rate of temperature fall per hour, slowly be cooled to below 1400 ℃ power cutoff through 8～10 hours then, reduce to room temperature with furnace temperature, promptly obtain Coating Materials lanthanium titanate crystal.
3. the growth method of lanthanum titanate crystal coated material according to claim 2 is characterized in that described crucible made by iridium, molybdenum or tungsten refractory metal.
4. the growth method of lanthanum titanate crystal coated material according to claim 2 is characterized in that described heating element made by graphite.
5. the growth method of lanthanum titanate crystal coated material according to claim 2, it is characterized in that described go up thermal insulation layer, all around thermal insulation layer and down thermal insulation layer form by graphite, pyrocarbon felt, or form by oxide refractories.
6. the growth method of lanthanum titanate crystal coated material according to claim 2 is characterized in that described seed holder, is made up of refractory metal iridium, molybdenum, tungsten material, or has other metallic substance compositions of refrigerative.
7. the growth method of lanthanum titanate crystal coated material according to claim 2 is characterized in that described induction power supply is intermediate frequency power supply or radio-frequency power supply.
8. according to the growth method of each described lanthanum titanate crystal coated material of claim 2 to 7, it is characterized in that described crucible and described around also have the round shape heating member between the thermal insulation layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910198956A CN101701357A (en) | 2009-11-18 | 2009-11-18 | Growth method of lanthanum titanate crystal coated material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910198956A CN101701357A (en) | 2009-11-18 | 2009-11-18 | Growth method of lanthanum titanate crystal coated material |
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|---|---|
| CN101701357A true CN101701357A (en) | 2010-05-05 |
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ID=42156282
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910198956A Pending CN101701357A (en) | 2009-11-18 | 2009-11-18 | Growth method of lanthanum titanate crystal coated material |
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102401910A (en) * | 2010-09-17 | 2012-04-04 | 晶炼科技股份有限公司 | Method for preparing optical coating material and optical coating material |
| CN114133226A (en) * | 2021-12-30 | 2022-03-04 | 苏州晶生新材料有限公司 | Optical coating substrate and using method thereof |
-
2009
- 2009-11-18 CN CN200910198956A patent/CN101701357A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102401910A (en) * | 2010-09-17 | 2012-04-04 | 晶炼科技股份有限公司 | Method for preparing optical coating material and optical coating material |
| CN114133226A (en) * | 2021-12-30 | 2022-03-04 | 苏州晶生新材料有限公司 | Optical coating substrate and using method thereof |
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Open date: 20100505 |