CN109576782A - A kind of preparation method and application of aluminum fluoride crystal particle - Google Patents
A kind of preparation method and application of aluminum fluoride crystal particle Download PDFInfo
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- CN109576782A CN109576782A CN201811552222.9A CN201811552222A CN109576782A CN 109576782 A CN109576782 A CN 109576782A CN 201811552222 A CN201811552222 A CN 201811552222A CN 109576782 A CN109576782 A CN 109576782A
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- aluminum fluoride
- crucible
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Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
Abstract
The invention discloses a kind of preparation method and application for the aluminum fluoride crystal particle for belonging to technical field of chemical material preparation.High-pure anhydrous aluminum fluoride powder is placed in crucible by the present invention, sealed crucible；Using vacuum furnace to the sealed crucible heating in vacuum, the part that the sealed crucible is built-in with high-pure anhydrous aluminum fluoride powder is located in furnace body heating zone, it is located at outside furnace body heating zone at the top of sealed crucible, and sealed crucible is located at the inside and outside two parts in furnace body heating zone using heat-barrier material and is separated；During heating in vacuum, high-pure anhydrous aluminum fluoride powder distils in sealed crucible, the fluorination aluminum steam condensation-crystallization at the top of sealed crucible, while aluminum fluoride crystal particle is constantly grown, and the aluminum fluoride crystal particle is made after cooling.Aluminum fluoride crystal particle produced by the present invention is white crystal, and color is uniform, can be used as optical filming material use, and coating process rate, vacustat, no material spray phenomenon.
Description
Technical field
The invention belongs to technical field of chemical material preparation, in particular to a kind of preparation method of aluminum fluoride crystal particle and
Using.
Background technique
Aluminum fluoride is mainly used for being used as regulator and cosolvent during Aluminum Electrolysis Production, in optical coating field aluminum fluoride
It is also a kind of good Coating Materials.Aluminum fluoride spectral transmission range is 0.2~8 micron, refractive index n=1.38 (500nm), n
=1.31 (8 μm) reduce as wavelength increases refractive index, are a kind of infrared spectroscopies of good properties in infrared region no hygroscopicity
Use low-index material.But since common high-pure anhydrous aluminum fluoride powder or sintering block are easy spray in coating process
The disadvantages of material, discharge quantity is big, and rate is difficult to control, it is difficult to be used for Coating Materials, therefore, it is necessary to aluminum fluoride is prepared into crystalline substance
Body for optical filming material to use.
Aluminum fluoride fusing point is 1291 DEG C, but directly distils and non-fusible in 1250 DEG C or so aluminum fluorides, and therefore, it is difficult to normal
The method for advising melting crystal obtains the aluminum fluoride crystal of bulky grain.Currently, what is generally reported is mostly the preparation side of aluminum fluoride powder
Method has the purification that aluminum fluoride powder is used for using the method for distillation condensation, also to obtain high-purity aluminum fouoride powder；But not
See the report of aluminum fluoride large-size crystals preparation.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method and application of aluminum fluoride crystal particle, and specific technical solution is such as
Under:
A kind of preparation method of aluminum fluoride crystal particle the following steps are included:
(1) high-pure anhydrous aluminum fluoride powder is placed in crucible, and sealed crucible；
(2) heating in vacuum is carried out to the sealed crucible using vacuum furnace, the sealed crucible is built-in with high-purity nothing
The part of water aluminum fluoride powder is located in furnace body heating zone, is located at outside furnace body heating zone at the top of sealed crucible, and utilizes heat-insulated material
Sealed crucible is located at the inside and outside two parts in furnace body heating zone and separates by material makees heat-insulated processing, to guarantee that crucible top temperature is low
In furnace body Heating Zone Temperature, formation temperature gradient；The heat-barrier material is arranged in sealed crucible periphery；
(3) start heating in vacuum, high-pure anhydrous aluminum fluoride powder distils in sealed crucible, the aluminum fluoride at the top of sealed crucible
Steam condensation-crystallization, while aluminum fluoride crystal particle is constantly grown, and the aluminum fluoride crystal particle is made after finally cooling down.
The crucible material is the material not with fluorination reactive aluminum.
Preferably, the crucible material is graphite, tungsten, molybdenum, tantalum or niobium, and further preferably graphite.
Sealing material used in the sealed crucible is preferably identical as crucible material.
5~30cm of furnace body heating zone is higher by the top of the sealed crucible；Preferably, furnace body is higher by the top of the sealed crucible
10~20cm of heating zone；To guarantee to have enough temperature that aluminum fluoride crystal is made to grow up at the top of sealed crucible.
The vacuum furnace is the furnace body that can vacuumize and have heating function, preferably vacuum carbon tube furnace or vacuum
Induction furnace.
The vacuum degree of the heating in vacuum is 0.01~100Pa, and the heating-up time is 1~10 hour, and temperature is 900~1300
DEG C, soaking time is 1~10 hour.
Preferably, the vacuum degree of the heating in vacuum is 0.1~20Pa, and the heating-up time is 2~5 hours, and heating temperature is
1000~1200 DEG C, soaking time is 2~5 hours.
By aluminum fluoride crystal Particle Breakage, screening obtained by the step (3), the aluminum fluoride of required particle size range can be obtained
Crystal grain.
Application of the aluminum fluoride crystal particle of preparation method preparation in plated film be with the aluminum fluoride crystal particle
Coating Materials, coating process is without material spray, coating process rate and vacustat.
The preparation method prepares the principle of aluminum fluoride crystal particle are as follows: aluminum fluoride distils under high-temperature vacuum, then exists
Condensation-crystallization under cryogenic vacuum.By controlling the temperature and vacuum degree of heating zone, so that aluminum fluoride powder distils；Control condensing zone
That is the temperature and vacuum degree of crucible top, so that crystallized after fluorination aluminum steam condensation, and crystal can grow up to a certain extent,
Meet Coating Materials demand.
The invention has the benefit that
(1) equipment, raw material are simple in preparation method of the present invention, cheap and easy to get, at low cost；Simple process, easily operated, peace
Quan Xinggao, three-protection design amount is few, easy to industrialized production；
(2) present invention is distilled and infusible physical property using aluminum fluoride, using the side of condensation-crystallization and crystal growth
Method obtains large-sized aluminum fluoride crystal, the lower impurity of partial vapor pressure stays in powder by control temperature and vacuum degree
In, crystal product purity effectively improves；
It (3) is white crystal using the aluminum fluoride crystal particle that the method for the present invention obtains, color is uniform, can be used as optics plating
Membrane material uses, and coating process rate, vacustat, no material spray phenomenon.
Detailed description of the invention
Attached drawing 1 is aluminum fluoride crystal block prepared by embodiment 1；
Attached drawing 2 is the aluminum fluoride crystal particle Coating Materials of 1~3mm particle size range prepared by embodiment 1.
Specific embodiment
The present invention provides a kind of preparation method and application of aluminum fluoride crystal particle, below with reference to embodiment to the present invention
It is described further.
Embodiment 1
Aluminum fluoride crystal particle is prepared using following step:
(1) the pure aluminum fouoride powder 1kg of analysis is weighed, is put into graphite crucible, graphite plate is used at the top of graphite crucible
Sealing；
(2) using vacuum carbon tube furnace to sealed graphite crucible heating in vacuum obtained by step (1), in the sealed graphite crucible
The part for being equipped with high-pure anhydrous aluminum fluoride powder is heating zone, is located in furnace body heating zone；The top of the sealed graphite crucible
For condensing zone, it is located at outside furnace body heating zone；Graphite felt is set with by sealed graphite crucible position in sealed graphite crucible periphery simultaneously
In furnace body heating zone, inside and outside two parts are heat-insulated；Wherein, sealed graphite crucible top is higher by furnace body heating zone 10cm；
(3) vacuum carbon tube furnace is vacuumized, opens power supply and starts to warm up: being warming up to 1200 DEG C in 2 hours, heat preservation 3 is small
When, heating and insulating process in vacuum degree change between 5~20pa；It is high-pure anhydrous in sealed graphite crucible in heating process
The distillation of aluminum fluoride powder, fluorination aluminum steam is in sealed graphite crucible top condensation-crystallization, while aluminum fluoride crystal particle is constantly long
Greatly, it is cooled to room temperature after the completion of heat preservation, the aluminum fluoride crystal block is made, as shown in Fig. 1；
After furnace body is cooled to room temperature, 560g white aluminum fluoride crystal, bottom remnants powder are obtained on sealed graphite crucible top cover
Body is 380g, volatilization loss 60g.It is 1~3mm by crystal fracture, 1-3mm particle size range as shown in Fig. 2 is obtained after screening
Crystal of fluoride particle Coating Materials, using ZZS-900 vacuum coating equipment carry out molybdenum boat heating evaporation plated film, coating process speed
Rate and vacustat, coating process is without material spray phenomenon.
Embodiment 2
Aluminum fluoride crystal particle Coating Materials is prepared using following step:
(1) the pure aluminum fouoride powder 2kg of analysis is weighed, is put into graphite crucible, graphite plate is used at the top of graphite crucible
Sealing；
(2) using vacuum carbon tube furnace to sealed graphite crucible heating in vacuum obtained by step (1), in the sealed graphite crucible
The part for being equipped with high-pure anhydrous aluminum fluoride powder is heating zone, is located in furnace body heating zone；The top of the sealed graphite crucible
For condensing zone, it is located at outside furnace body heating zone；Graphite felt is set with by sealed graphite crucible position in sealed graphite crucible periphery simultaneously
In furnace body heating zone, inside and outside two parts are heat-insulated；Wherein, sealed graphite crucible top is higher by furnace body heating zone 15cm；
(3) vacuum carbon tube furnace is vacuumized, opens power supply and starts heating in vacuum: being warming up to 1250 DEG C at 4 hours, heat preservation 5
Hour, vacuum degree changes between 5~30pa in heating and insulating process；In heating process, high-purity nothing in sealed graphite crucible
The distillation of water aluminum fluoride powder is fluorinated aluminum steam in sealed graphite crucible top condensation-crystallization, while aluminum fluoride crystal particle is continuous
It grows up, is cooled to room temperature after the completion of heat preservation, the aluminum fluoride crystal particle is made；
After furnace body is cooled to room temperature, 890g white aluminum fluoride crystal, bottom remnants powder are obtained on sealed graphite crucible top cover
Body is 1010g, volatilization loss 100g.It is 1~3mm by crystal fracture, crystal of fluoride particle Coating Materials is obtained after screening, is adopted
Molybdenum boat heating evaporation plated film, coating process rate and vacustat are carried out with ZZS-900 vacuum coating equipment, coating process is without spray
Expect phenomenon.
Embodiment 3
Aluminum fluoride crystal particle Coating Materials is prepared using following step:
(1) the pure aluminum fouoride powder 1.5kg of analysis is weighed, is put into tungsten crucible, is sealed at the top of tungsten crucible using tungsten plate；
(2) it is built-in with using vacuum carbon tube furnace to tungsten crucible heating in vacuum, the sealing tungsten crucible is sealed obtained by step (1)
The part of high-pure anhydrous aluminum fluoride powder is heating zone, is located in furnace body heating zone；The top for sealing tungsten crucible is condensing zone, position
In outside furnace body heating zone；And will seal tungsten crucible, to be located at furnace body heating zone inside and outside in sealing tungsten crucible periphery setting graphite felt
Two parts be thermally shielded；Wherein, furnace body heating zone 10cm is higher by the top of sealing tungsten crucible；
(3) vacuum carbon tube furnace is vacuumized, opens power supply and starts heating in vacuum: being warming up to 1000 DEG C at 3 hours, heat preservation 4
Hour, vacuum degree changes between 0.1~5pa in heating and insulating process；In heating process, high-purity nothing in sealed graphite crucible
The distillation of water aluminum fluoride powder is fluorinated aluminum steam in sealed graphite crucible top condensation-crystallization, while aluminum fluoride crystal particle is continuous
It grows up, is cooled to room temperature after the completion of heat preservation, the aluminum fluoride crystal particle is made；
After furnace body is cooled to room temperature, seals and obtain 350g white aluminum fluoride crystal, bottom remnants powder on tungsten crucible top cover
For 620g, volatilization loss 30g.It is 1~3mm by crystal fracture, crystal of fluoride particle Coating Materials is obtained after screening, uses
ZZS-900 vacuum coating equipment carries out molybdenum boat heating evaporation plated film, coating process rate and vacustat, and coating process is without material spray
Phenomenon.
Embodiment 4
Aluminum fluoride crystal particle Coating Materials is prepared using following step:
(1) the pure aluminum fouoride powder 5kg of analysis is weighed, is put into graphite crucible, graphite plate is used at the top of graphite crucible
Sealing；
(2) using vacuum carbon tube furnace to sealed graphite crucible heating in vacuum obtained by step (1), in the sealed graphite crucible
The part for being equipped with high-pure anhydrous aluminum fluoride powder is heating zone, is located in furnace body heating zone；The top of sealed graphite crucible is cold
Coagulation zone is located at outside furnace body heating zone；And in sealed graphite crucible periphery setting graphite felt sealed graphite crucible is located at furnace body
The inside and outside two parts in heating zone are thermally shielded；Wherein, sealed graphite crucible top is higher by furnace body heating zone 20cm；
(3) vacuum carbon tube furnace is vacuumized, opens power supply and starts heating in vacuum: being warming up to 1100 DEG C at 5 hours, heat preservation 7
Hour, vacuum degree changes between 0.1~20pa in heating and insulating process；It is high-purity in sealed graphite crucible in heating process
The distillation of aluminum fouoride powder is fluorinated aluminum steam in sealed graphite crucible top condensation-crystallization, while aluminum fluoride crystal particle is not
It is disconnected to grow up, it is cooling after the completion of heat preservation, the aluminum fluoride crystal particle is made；
After furnace body is cooled to room temperature, 1240g white aluminum fluoride crystal, bottom remnants powder are obtained on sealed graphite crucible top cover
Body is 3620g, volatilization loss 140g.It is 1~3mm by crystal fracture, crystal of fluoride particle Coating Materials is obtained after screening, is adopted
Molybdenum boat heating evaporation plated film, coating process rate and vacustat are carried out with ZZS-900 vacuum coating equipment, coating process is without spray
Expect phenomenon.
Claims (9)
1. a kind of preparation method of aluminum fluoride crystal particle, which comprises the following steps:
(1) high-pure anhydrous aluminum fluoride powder is placed in crucible, sealed crucible；
(2) using vacuum furnace to the sealed crucible heating in vacuum, the sealed crucible is built-in with high-pure anhydrous aluminum fluoride
The part of powder is located in furnace body heating zone, is located at outside furnace body heating zone at the top of sealed crucible, and will be sealed using heat-barrier material
Crucible is located at the inside and outside two parts in furnace body heating zone and separates；
(3) start heating in vacuum, high-pure anhydrous aluminum fluoride powder distils in sealed crucible, the fluorination aluminum steam at the top of sealed crucible
Condensation-crystallization, while aluminum fluoride crystal particle is constantly grown, and the aluminum fluoride crystal particle is made after cooling.
2. preparation method according to claim 1, which is characterized in that the crucible material is the material not with fluorination reactive aluminum
Material.
3. preparation method according to claim 1, which is characterized in that the crucible material is graphite, tungsten, molybdenum, tantalum or niobium.
4. preparation method according to claim 1, which is characterized in that be higher by furnace body heating zone 5 at the top of the sealed crucible
~30cm.
5. preparation method according to claim 1, which is characterized in that be higher by furnace body heating zone 10 at the top of the sealed crucible
~20cm.
6. preparation method according to claim 1, which is characterized in that the vacuum furnace is vacuum carbon tube furnace or vacuum
Induction furnace.
7. preparation method according to claim 1, which is characterized in that the vacuum degree of the heating in vacuum be 0.01~
100Pa, heating-up time are 1~10 hour, and heating temperature is 900~1300 DEG C, and soaking time is 1~10 hour.
8. preparation method according to claim 1, which is characterized in that the vacuum degree of the heating in vacuum is 0.1~20Pa,
Heating-up time is 2~5 hours, and heating temperature is 1000~1200 DEG C, and soaking time is 2~5 hours.
9. a kind of application of the aluminum fluoride crystal particle of any one of claim 1~8 preparation method preparation in plated film,
It is characterized in that, using the aluminum fluoride crystal particle as Coating Materials, coating process is without material spray.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811552222.9A CN109576782A (en) | 2018-12-19 | 2018-12-19 | A kind of preparation method and application of aluminum fluoride crystal particle |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811552222.9A CN109576782A (en) | 2018-12-19 | 2018-12-19 | A kind of preparation method and application of aluminum fluoride crystal particle |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0891832A (en) * | 1994-09-16 | 1996-04-09 | Toshiba Ceramics Co Ltd | High purity aluminum fluoride and its production |
| CN1717508A (en) * | 2003-07-31 | 2006-01-04 | Si晶体股份公司 | Method and device for AIN single crystal production with gas-permeable crucible walls |
| US20170321345A1 (en) * | 2016-05-06 | 2017-11-09 | Ii-Vi Incorporated | Large Diameter Silicon Carbide Single Crystals and Apparatus and Method of Manufacture Thereof |
| CN108277526A (en) * | 2017-12-29 | 2018-07-13 | 苏州奥趋光电技术有限公司 | A method of passing through physical vapor transport growing aluminum nitride monocrystalline |
| CN108840358A (en) * | 2018-09-13 | 2018-11-20 | 衢州市鼎盛化工科技有限公司 | A kind of devices and methods therefor preparing aluminum fouoride |
-
2018
- 2018-12-19 CN CN201811552222.9A patent/CN109576782A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0891832A (en) * | 1994-09-16 | 1996-04-09 | Toshiba Ceramics Co Ltd | High purity aluminum fluoride and its production |
| CN1717508A (en) * | 2003-07-31 | 2006-01-04 | Si晶体股份公司 | Method and device for AIN single crystal production with gas-permeable crucible walls |
| US20170321345A1 (en) * | 2016-05-06 | 2017-11-09 | Ii-Vi Incorporated | Large Diameter Silicon Carbide Single Crystals and Apparatus and Method of Manufacture Thereof |
| CN108277526A (en) * | 2017-12-29 | 2018-07-13 | 苏州奥趋光电技术有限公司 | A method of passing through physical vapor transport growing aluminum nitride monocrystalline |
| CN108840358A (en) * | 2018-09-13 | 2018-11-20 | 衢州市鼎盛化工科技有限公司 | A kind of devices and methods therefor preparing aluminum fouoride |
Non-Patent Citations (2)
| Title |
|---|
| 李恒德主编: "《现代材料科学与工程词典》", 31 August 2001, 山东科学技术出版社 * |
| 王承遇，陶瑛编著: "《玻璃表面装饰》", 31 August 1998, 新时代出版社 * |
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Application publication date: 20190405 |