CN105986316A - Tantalum oxide polycrystal film-coated material and growth method of same - Google Patents
Tantalum oxide polycrystal film-coated material and growth method of same Download PDFInfo
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- CN105986316A CN105986316A CN201510041724.5A CN201510041724A CN105986316A CN 105986316 A CN105986316 A CN 105986316A CN 201510041724 A CN201510041724 A CN 201510041724A CN 105986316 A CN105986316 A CN 105986316A
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Abstract
The invention relates to a growth method of a tantalum oxide polycrystal film-coated material. The method includes the steps of: (A) briquetting a raw material Ta2O5 under isostatic pressure of 1.0-5.0 t/cm<2>; (B) placing the briquetted material in a crucible, placing the crucible in a high-temperature Bridgman furnace, regulating the height of the crucible in the Bridgman furnace, increasing the temperature and vacuumizing the Bridgman furnace to 10<-3> - 10<-4> Pa, and when the temperature in the Bridgman furnace reaches 1400-1700 DEG C, filling the furnace with an inert protective gas, and increasing the temperature to a preset temperature of 1820-1900 DEG C; (C) when the furnace temperature reaches the preset temperature, maintaining the temperature for 3-6 h, regulating the hearth temperature and the position of the crucible to fully melt the raw material, wherein the temperature gradient at a solid-liquid interface of crystal growth is 20-60 DEG C/cm and reduction speed of the crucible is 5.0-50 mm/h; and (D) when the crystal growth is finished, regulating the position of the crucible, maintaining the temperature for 3-20 h, and reducing the temperature to room temperature at the rate of 80-150 DEG C/h. Through the crucible reduction growth method, the tantalum oxide crystal, after being molten, has higher density, uniform structure and better crystallinity. During production, through the character that the crystal removes impurities of itself, the material has higher purity. The method has simpler operation method and lower production cost.
Description
Technical field
The present invention relates to growing method field, especially a kind of tantalum oxide polycrystalline Coating Materials and growth thereof
Method.
Background technology
Tantalum oxide is high index of refraction Coating Materials commonly used in optical communication industry at present.Tantalum oxide coating material
Material has stable high refractive index, chemical stability is good, film layer firmness high, resisting laser damage ability is strong.
There are high transmitance and reflectance in visible and near infrared region, applied anti-reflection film, laser instrument, optical communication etc.
On components and parts.
At present, use ceramic post sintering method to prepare tantalum oxide Coating Materials, use tantalum oxide prepared by the method
Although Coating Materials cost is relatively low, but in preparation process, it is readily incorporated impurity, inside tantalum oxide pottery coating materials
There is a large amount of pore, and is difficult to ensure that the uniformity of composition and structure, and these factors are to preparing high-quality
Thin film play conclusive effect.
This is because Coating Materials to be heated in coating process, now have and adsorb in tantalum oxide in a large number
Gas release, such plated film chamber vacuum degree can drastically decline, and makes film layer coarse, and fastness is poor, seriously
Affect the quality of film layer.Exit in a large number during for avoiding plated film, need in advance in plated film vacuum chamber to tantalum oxide
Evaporation material carries out heat treatment, is allowed to release adsorbed gas, i.e. fritting.Have inside tantalum oxide pottery coating materials
Substantial amounts of pore, fritting needs substantial amounts of time and more difficult, and is difficult to the abundant of fritting.Thus drop
Low plated film efficiency, have impact on the quality of film layer.
Summary of the invention
It is an object of the invention to the defect overcoming prior art to exist, it is provided that a kind of tantalum oxide polycrystalline Coating Materials
Growing method, use Bridgman-Stockbarger method, tantalum oxide crystal is through fusing, and density is bigger, knot
Structure is uniform, and crystallinity is more preferable, utilizes the characteristic of crystal self impurities removal in growth course, and the purity of material is higher,
Operational approach is the simplest, growth cost is the cheapest.
The technical solution adopted for the present invention to solve the technical problems is:
The growing method of a kind of tantalum oxide polycrystalline Coating Materials, comprises the following steps:
(1) pretreatment of raw material, by raw material Ta2O5At 1.0-5.0t/cm2Isostatic pressed under, briquetting；
(2) briquetting material step (1) obtained loads in crucible, and crucible is transferred to high temperature and declines in stove,
Adjustment crucible, at body of heater inner height, heats up after sealing whole system, starts mechanical pump, diffusion pump, takes out true
Empty to 10-3-10-4Pa, is filled with inert protective gas when furnace temperature reaches 1400-1700 DEG C, is continuously heating to set
Fixed temperature, described design temperature is in the range of 1820-1900 DEG C；
(3), after furnace temperature reaches design temperature, it is incubated 3-6 hour, regulating stove bore temperature and bushing position, make
Melting sources is abundant, and at the solid liquid interface of crystal growth, thermograde is set as 20-60 DEG C/cm, and crucible declines
Rate controlled is in the range of 5.0-50mm/h；
(4) after crystal growth terminates, regulate bushing position, be incubated 3-20h, with the speed of 80-150 DEG C/h
It is down to room temperature.
Further, described crucible cylindrically shaped, described crucible is selected from molybdenum, tungsten or tungsten-molybdenum alloy
Exotic material.
Further, described inert protective gas is argon, nitrogen, and the purity of described argon is 99.99%.
Further, described raw material Ta2O5Purity is 99.99%.
Compared with prior art, the invention has the beneficial effects as follows:
(1) the tantalum oxide polycrystalline Coating Materials that the growing method of the present invention obtains has the following characteristics that component is uniform；
Good crystallinity；Density is big, and discharge quantity is few；Coating operation is good, and the film layer obtained is intensive, uniform, stable.
(2) growing method of the tantalum oxide polycrystalline Coating Materials of the present invention, uses Bridgman-Stockbarger method, tantalum oxide crystal
Through fusing, density is bigger, even structure, and crystallinity is more preferable, utilizes crystal self impurities removal in growth course
Characteristic, the purity of material is higher；Field structure is stable, thermograde is adjustable for temperature；The crystal grown can and
Shi Jinhang makes annealing treatment, the thermal stress remaining to eliminate crystals；Operational approach is simple, growth cost is low
Honest and clean, average energy consumption is low.
Detailed description of the invention
Embodiment 1:
It is the Ta of 99.99% by purity2O5Raw material is at 1.0t/cm2Isostatic pressed under, briquetting；Briquetting material is loaded
In molybdenum crucible, molybdenum crucible is transferred to high temperature and declines in stove, adjusts height, heats up after sealing whole system,
Start mechanical pump, diffusion pump, be evacuated to 10-3Pa, is filled with the argon of 99.99% when furnace temperature reaches 1400 DEG C
Gas Ar, is continuously heating to design temperature 1820 DEG C；After furnace temperature reaches design temperature, it is incubated 3 hours, regulation
Fire box temperature and bushing position, make melting sources abundant, and at the solid liquid interface of crystal growth, thermograde sets
Being 20 DEG C/cm, crucible fall off rate controls at 5mm/h；After crystal growth terminates, regulate bushing position, protect
Temperature 3h, is down to room temperature with the speed of 80 DEG C/h.
Embodiment 2:
It is the Ta of 99.99% by purity2O5Raw material is at 2.0t/cm2Isostatic pressed under, briquetting；Briquetting material is filled
Entering in molybdenum crucible, molybdenum crucible is transferred to high temperature and declines in stove, adjusts height, heats up after sealing whole system,
Start mechanical pump, diffusion pump, be evacuated to 10-3Pa, is filled with the argon of 99.99% when furnace temperature reaches 1500 DEG C
Gas Ar, is continuously heating to design temperature 1830 DEG C；After furnace temperature reaches design temperature, it is incubated 4 hours, regulation
Fire box temperature and bushing position, make melting sources abundant, and at the solid liquid interface of crystal growth, thermograde sets
Being 30 DEG C/cm, crucible fall off rate controls at 10mm/h；After crystal growth terminates, regulate bushing position,
Insulation 5h, is down to room temperature with the speed of 80 DEG C/h.
Embodiment 3:
It is the Ta of 99.99% by purity2O5Raw material is at 4.0t/cm2Isostatic pressed under, briquetting；Briquetting material is filled
Entering in molybdenum crucible, molybdenum crucible is transferred to high temperature and declines in stove, adjusts height, heats up after sealing whole system,
Start mechanical pump, diffusion pump, be evacuated to 10-3Pa, is filled with the argon of 99.99% when furnace temperature reaches 1600 DEG C
Gas Ar, is continuously heating to design temperature 1860 DEG C；After furnace temperature reaches design temperature, it is incubated 5 hours, regulation
Fire box temperature and bushing position, make melting sources abundant, and at the solid liquid interface of crystal growth, thermograde sets
Being 50 DEG C/cm, crucible fall off rate controls at 40mm/h；After crystal growth terminates, regulate bushing position,
Insulation 8h, is down to room temperature with the speed of 100 DEG C/h.
Embodiment 4:
It is the Ta of 99.99% by purity2O5Raw material is at 5.0t/cm2Isostatic pressed under, briquetting；Briquetting material is filled
Entering in molybdenum crucible, molybdenum crucible is transferred to high temperature and declines in stove, adjusts height, heats up after sealing whole system,
Start mechanical pump, diffusion pump, be evacuated to 10-4Pa, is filled with inertia protection gas when furnace temperature reaches 1700 DEG C
Body Ar, is continuously heating to design temperature 1900 DEG C；After furnace temperature reaches design temperature, it is incubated 6 hours, regulation
Fire box temperature and bushing position, make melting sources abundant, and at the solid liquid interface of crystal growth, thermograde sets
Being 60 DEG C/cm, crucible fall off rate controls at 50mm/h；After crystal growth terminates, regulate bushing position,
Insulation 10h, is down to room temperature with the speed of 150 DEG C/h.
Should be appreciated that specific embodiment described above is only used for explaining the present invention, be not used to limit
Determine the present invention.The obvious change extended out by the spirit of the present invention or variation are still in this
Among bright protection domain.
Claims (4)
1. a growing method for tantalum oxide polycrystalline Coating Materials, comprises the following steps:
(1) pretreatment of raw material, by raw material Ta2O5At 1.0-5.0t/cm2Isostatic pressed under, briquetting；
(2) briquetting material step (1) obtained loads in crucible, and crucible is transferred to high temperature and declines in stove, adjusts crucible height in declining body of heater, heats up whole system, be evacuated to 10-3-10-4Pa, is filled with inert protective gas when furnace temperature reaches 1400-1700 C, is continuously heating to design temperature, and described design temperature is in the range of 1820-1900 C；
(3), after furnace temperature reaches design temperature, it is incubated 3-6 hour, regulating stove bore temperature and bushing position, make melting sources abundant, at the solid liquid interface of crystal growth, thermograde is set as that 20-60 C/cm, crucible fall off rate control in the range of 5.0-50mm/h；
(4) after crystal growth terminates, regulate bushing position, be incubated 3-20h, be down to room temperature with the speed of 80-150 ° of C/h.
The growing method of described a kind of tantalum oxide polycrystalline Coating Materials the most according to claim 1, it is characterised in that described crucible cylindrically shaped, described crucible is the exotic material selected from molybdenum, tungsten or tungsten-molybdenum alloy.
The growing method of described a kind of tantalum oxide polycrystalline Coating Materials the most according to claim 1, it is characterised in that described inert protective gas is argon, nitrogen, and the purity of described argon is 99.99%.
The growing method of described a kind of tantalum oxide polycrystalline Coating Materials the most according to claim 1, it is characterised in that described raw material Ta2O5Purity is 99.99%.
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Cited By (3)
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| CN106904967A (en) * | 2017-02-21 | 2017-06-30 | 成都超纯应用材料有限责任公司 | A kind of high density tantalum pentoxide film preparation method for material |
| CN113121224A (en) * | 2021-04-15 | 2021-07-16 | 有研资源环境技术研究院(北京)有限公司 | Preparation method of annular high-density tantalum pentoxide coating material |
| CN115142119A (en) * | 2021-12-20 | 2022-10-04 | 常州瞻驰光电科技股份有限公司 | Method for preparing tantalum pentoxide crystal by using rotary crucible descending technology and application |
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| CN113121224A (en) * | 2021-04-15 | 2021-07-16 | 有研资源环境技术研究院(北京)有限公司 | Preparation method of annular high-density tantalum pentoxide coating material |
| CN113121224B (en) * | 2021-04-15 | 2022-09-06 | 有研资源环境技术研究院(北京)有限公司 | Preparation method of annular high-density tantalum pentoxide coating material |
| CN115142119A (en) * | 2021-12-20 | 2022-10-04 | 常州瞻驰光电科技股份有限公司 | Method for preparing tantalum pentoxide crystal by using rotary crucible descending technology and application |
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