CN113753938A - Preparation method of yttrium fluoride film - Google Patents
Preparation method of yttrium fluoride film Download PDFInfo
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- CN113753938A CN113753938A CN202010681953.4A CN202010681953A CN113753938A CN 113753938 A CN113753938 A CN 113753938A CN 202010681953 A CN202010681953 A CN 202010681953A CN 113753938 A CN113753938 A CN 113753938A
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- film
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- yttrium fluoride
- yttrium
- powder
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- 229940105963 yttrium fluoride Drugs 0.000 title claims abstract description 35
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 235000015110 jellies Nutrition 0.000 claims abstract description 13
- 239000008274 jelly Substances 0.000 claims abstract description 13
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000003618 dip coating Methods 0.000 claims abstract description 7
- 238000004528 spin coating Methods 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- WUVRZBFIXJWTGS-UHFFFAOYSA-N yttrium(3+);trinitrate;hydrate Chemical compound O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O WUVRZBFIXJWTGS-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000003746 solid phase reaction Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 60
- 239000011737 fluorine Substances 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- -1 anion fluorine ions Chemical class 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/265—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/20—Two-dimensional structures
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of a yttrium fluoride film, which comprises the following steps of 1: uniformly mixing hydrated yttrium nitrate and ammonium fluoride according to the molar ratio of 1:3.05-1: 3.75; step 2: drying the jelly to obtain a colloidal substance; and step 3: placing the colloidal substance in a high temperature furnace; and 4, step 4: grinding the colloidal substance to obtain powder; and 5: the powder is protected by inert gas to obtain nanoscale powder; step 6: preparing a film from the nanoscale powder by adopting a dip-coating method or a spin-coating method; and 7: drying and cooling the wet film to obtain a film; and 8: annealing the film, and cooling the film along with the furnace to obtain the yttrium fluoride film. Compared with the prior art, the preparation method of the yttrium fluoride film has the advantages that the prepared yttrium fluoride film has smooth surface, good superconducting property, low film preparation cost, simple process and easy control; the heat treatment process period is greatly shortened, the film preparation efficiency is greatly improved, the film layer is firmly combined and is difficult to break.
Description
Technical Field
The invention relates to the technical field of film preparation, in particular to a preparation method of a yttrium fluoride film.
Background
The yttrium fluoride film has a low refractive index (refractive index of about 1.4), a wide transmission band (0.35-12 μm), and a high hardness compared with other fluorides (barium fluoride, calcium fluoride, etc.), so that the yttrium fluoride film is widely used for designing antireflection films on various substrates. Common methods for preparing yttrium fluoride films are thermal evaporation deposition, ion and electron beam assisted evaporation deposition, chemical methods, and the like.
Aiming at the defects of the traditional yttrium fluoride film preparation process, the yttrium fluoride film is prepared by adopting a yttrium fluoride target material by using a magnetron sputtering technology, but the method is easy to cause loss of anion fluorine ions, increased absorption, distortion of refractive index and functional failure, and simultaneously, the internal stress of the film is unstable, so that the film is easy to crack, fall off and crack, and the structure is easy to fail. Since the optical constants are distorted by fluorine deficiency, fluorine ions are generally replenished with a reactive gas, and fluorine gas is extremely toxic. If the perfluorocarbon is used, impurity ions such as C are introduced into the film, and the optical performance of the yttrium fluoride film is seriously deteriorated.
Disclosure of Invention
The present invention is directed to a method for preparing a yttrium fluoride thin film, so as to solve the problems mentioned in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a yttrium fluoride film comprises the following steps:
step 1: uniformly mixing yttrium nitrate hydrate and ammonium fluoride according to the molar ratio of 1:3.05-1:3.75, grinding in a mortar to perform solid-phase reaction, and obtaining jelly after the reaction is completed;
step 2: transferring the jelly into a high-temperature-resistant crucible, and drying in an oven for 3-22h to obtain a colloidal substance;
and step 3: placing the colloidal substance in a high-temperature furnace, and keeping the temperature for 1-4 h;
and 4, step 4: cooling the colloidal substance to room temperature with a furnace, taking out, and grinding to obtain powder;
and 5: preserving the temperature of the powder at 350-450 ℃ for 4-5.5h under the protection of inert gas to obtain nano-scale powder;
step 6: preparing a film from the nanoscale powder by adopting a dip-coating method or a spin-coating method;
and 7: airing the wet film for 15-25min at room temperature, then placing the wet film in a drying oven for drying, and naturally cooling to room temperature to obtain a film;
and 8: and (3) putting the film into a high-temperature furnace for annealing treatment, and cooling along with the furnace to obtain the yttrium fluoride film.
Preferably, in the step 1, the time for mixing and stirring the hydrated yttrium nitrate and the ammonium fluoride is 4-20 h.
Preferably, in step 2, the temperature of the high temperature-resistant crucible is increased from room temperature to 350-450 ℃ at a temperature increase rate of 2-8 ℃/min.
Preferably, in step 5, the inert gas is nitrogen or argon.
Preferably, in step 7, the drying temperature is 95-100 ℃.
Preferably, in step 8, the temperature of the high temperature furnace is increased from room temperature to 300 ℃ and 500 ℃ at a heating rate of 3-10 ℃/min, and the temperature is maintained for 1-4 h.
Compared with the prior art, the invention has the beneficial effects that:
compared with the prior art, the preparation method of the yttrium fluoride film has the advantages that the prepared yttrium fluoride film has smooth surface, good superconducting property, low film preparation cost, simple process and easy control; the heat treatment process period is greatly shortened, the film preparation efficiency is greatly improved, the film layer is firmly combined and is difficult to break.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a technical scheme that: a preparation method of a yttrium fluoride film comprises the following steps:
step 1: uniformly mixing yttrium nitrate hydrate and ammonium fluoride according to a molar ratio of 1:3.05-1:3.75, grinding in a mortar to perform solid-phase reaction to obtain a jelly after the reaction is completed, and stirring yttrium nitrate hydrate and ammonium fluoride for 4 hours;
step 2: transferring the jelly into a high-temperature-resistant crucible, placing the high-temperature-resistant crucible into an oven for drying for 3 hours to obtain a colloidal substance, and heating the temperature of the high-temperature-resistant crucible from room temperature to 350 ℃ at a heating rate of 2 ℃/min;
and step 3: placing the colloidal substance in a high-temperature furnace, and keeping the temperature for 1 h;
and 4, step 4: cooling the colloidal substance to room temperature with a furnace, taking out, and grinding to obtain powder;
and 5: preserving the heat of the powder for 4 hours at 350 ℃ under the protection of inert gas to obtain nanoscale powder, wherein the inert gas is nitrogen or argon;
step 6: preparing a film from the nanoscale powder by adopting a dip-coating method or a spin-coating method;
and 7: airing the wet film for 15min at room temperature, then placing the wet film in a drying oven for drying, and naturally cooling the wet film to the room temperature to obtain a film, wherein the drying temperature is 95 ℃;
and 8: and (3) putting the film into a high-temperature furnace for annealing treatment, cooling along with the furnace to obtain the yttrium fluoride film, heating the high-temperature furnace from room temperature to 300 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 1 h.
Example 2:
the invention provides a technical scheme that: a preparation method of a yttrium fluoride film comprises the following steps:
step 1: uniformly mixing yttrium nitrate hydrate and ammonium fluoride according to a molar ratio of 1:3.05-1:3.75, grinding in a mortar to perform solid-phase reaction to obtain a jelly after the reaction is completed, and stirring yttrium nitrate hydrate and ammonium fluoride for 12 hours;
step 2: transferring the jelly into a high-temperature-resistant crucible, placing the high-temperature-resistant crucible into an oven for drying for 15 hours to obtain a colloidal substance, and raising the temperature of the high-temperature-resistant crucible from room temperature to 400 ℃ at a temperature rise rate of 5 ℃/min;
and step 3: placing the colloidal substance in a high-temperature furnace, and keeping the temperature for 2 h;
and 4, step 4: cooling the colloidal substance to room temperature with a furnace, taking out, and grinding to obtain powder;
and 5: preserving the heat of the powder for 5 hours at 400 ℃ under the protection of inert gas to obtain nanoscale powder, wherein the inert gas is nitrogen or argon;
step 6: preparing a film from the nanoscale powder by adopting a dip-coating method or a spin-coating method;
and 7: airing the wet film for 20min at room temperature, then placing the wet film in a drying oven for drying, and naturally cooling the wet film to the room temperature to obtain a film, wherein the drying temperature is 95 ℃;
and 8: and (3) putting the film into a high-temperature furnace for annealing treatment, cooling along with the furnace to obtain the yttrium fluoride film, heating the high-temperature furnace from room temperature to 450 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 2.5 h.
Example 3:
the invention provides a technical scheme that: a preparation method of a yttrium fluoride film comprises the following steps:
step 1: uniformly mixing yttrium nitrate hydrate and ammonium fluoride according to a molar ratio of 1:3.05-1:3.75, grinding in a mortar to perform solid-phase reaction to obtain a jelly after the reaction is completed, and mixing and stirring the yttrium nitrate hydrate and the ammonium fluoride for 20 hours;
step 2: transferring the jelly into a high-temperature-resistant crucible, placing the high-temperature-resistant crucible into an oven for drying for 22h to obtain a colloidal substance, and heating the temperature of the high-temperature-resistant crucible from room temperature to 450 ℃ at a heating rate of 8 ℃/min;
and step 3: placing the colloidal substance in a high-temperature furnace, and keeping the temperature for 4 h;
and 4, step 4: cooling the colloidal substance to room temperature with a furnace, taking out, and grinding to obtain powder;
and 5: preserving the temperature of the powder for 5.5 hours at 450 ℃ under the protection of inert gas to obtain nanoscale powder, wherein the inert gas is nitrogen or argon;
step 6: preparing a film from the nanoscale powder by adopting a dip-coating method or a spin-coating method;
and 7: airing the wet film for 25min at room temperature, then placing the wet film in a drying oven for drying, and naturally cooling the wet film to the room temperature to obtain a film, wherein the drying temperature is 100 ℃;
and 8: and (3) putting the film into a high-temperature furnace for annealing treatment, cooling along with the furnace to obtain the yttrium fluoride film, heating the high-temperature furnace from room temperature to 500 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 4 hours.
In conclusion, the yttrium fluoride film prepared by the embodiment has smooth surface, good superconducting property, low film preparation cost, simple process and easy control; the heat treatment process period is greatly shortened, the film preparation efficiency is greatly improved, the film layer is firmly combined and is difficult to break.
Application method
A preparation method of a yttrium fluoride film comprises the following steps:
step 1: uniformly mixing yttrium nitrate hydrate and ammonium fluoride according to the molar ratio of 1:3.05-1:3.75, grinding in a mortar to perform solid-phase reaction, and obtaining jelly after the reaction is completed;
step 2: transferring the jelly into a high-temperature-resistant crucible, and drying in an oven for 3-22h to obtain a colloidal substance;
and step 3: placing the colloidal substance in a high-temperature furnace, and keeping the temperature for 1-4 h;
and 4, step 4: cooling the colloidal substance to room temperature with a furnace, taking out, and grinding to obtain powder;
and 5: preserving the temperature of the powder at 350-450 ℃ for 4-5.5h under the protection of inert gas to obtain nano-scale powder;
step 6: preparing a film from the nanoscale powder by adopting a dip-coating method or a spin-coating method;
and 7: airing the wet film for 15-25min at room temperature, then placing the wet film in a drying oven for drying, and naturally cooling to room temperature to obtain a film;
and 8: and (3) putting the film into a high-temperature furnace for annealing treatment, and cooling along with the furnace to obtain the yttrium fluoride film.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A preparation method of a yttrium fluoride film is characterized by comprising the following steps:
step 1: uniformly mixing yttrium nitrate hydrate and ammonium fluoride according to the molar ratio of 1:3.05-1:3.75, grinding in a mortar to perform solid-phase reaction, and obtaining jelly after the reaction is completed;
step 2: transferring the jelly into a high-temperature-resistant crucible, and drying in an oven for 3-22h to obtain a colloidal substance;
and step 3: placing the colloidal substance in a high-temperature furnace, and keeping the temperature for 1-4 h;
and 4, step 4: cooling the colloidal substance to room temperature with a furnace, taking out, and grinding to obtain powder;
and 5: preserving the temperature of the powder at 350-450 ℃ for 4-5.5h under the protection of inert gas to obtain nano-scale powder;
step 6: preparing a film from the nanoscale powder by adopting a dip-coating method or a spin-coating method;
and 7: airing the wet film for 15-25min at room temperature, then placing the wet film in a drying oven for drying, and naturally cooling to room temperature to obtain a film;
and 8: and (3) putting the film into a high-temperature furnace for annealing treatment, and cooling along with the furnace to obtain the yttrium fluoride film.
2. The method according to claim 1, wherein the step of preparing the yttrium fluoride film comprises: in the step 1, the yttrium nitrate hydrate and the ammonium fluoride are mixed and stirred for 4-20 h.
3. The method according to claim 1, wherein the step of preparing the yttrium fluoride film comprises: in step 2, the temperature of the high temperature-resistant crucible is increased from room temperature to 350-450 ℃ at a temperature increase rate of 2-8 ℃/min.
4. The method according to claim 1, wherein the step of preparing the yttrium fluoride film comprises: in step 5, the inert gas is nitrogen or argon.
5. The method according to claim 1, wherein the step of preparing the yttrium fluoride film comprises: in step 7, the drying temperature is 95-100 ℃.
6. The method according to claim 1, wherein the step of preparing the yttrium fluoride film comprises: in step 8, the temperature of the high temperature furnace is raised from room temperature to 300-500 ℃ at a heating rate of 3-10 ℃/min, and the temperature is maintained for 1-4 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010681953.4A CN113753938A (en) | 2020-07-15 | 2020-07-15 | Preparation method of yttrium fluoride film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010681953.4A CN113753938A (en) | 2020-07-15 | 2020-07-15 | Preparation method of yttrium fluoride film |
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| CN113753938A true CN113753938A (en) | 2021-12-07 |
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| CN202010681953.4A Pending CN113753938A (en) | 2020-07-15 | 2020-07-15 | Preparation method of yttrium fluoride film |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746805A (en) * | 2009-12-04 | 2010-06-23 | 江门市科恒实业股份有限公司 | Preparation method of nanoscale yttrium fluoride |
| CN104830341A (en) * | 2015-05-15 | 2015-08-12 | 福州大学 | Preparation method of rare-earth-ion-doped yttrium fluoride green upconversion fluorescent material |
| US20190352761A1 (en) * | 2018-05-18 | 2019-11-21 | Shin-Etsu Chemical Co., Ltd. | Spray material, sprayed member and making method |
-
2020
- 2020-07-15 CN CN202010681953.4A patent/CN113753938A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746805A (en) * | 2009-12-04 | 2010-06-23 | 江门市科恒实业股份有限公司 | Preparation method of nanoscale yttrium fluoride |
| CN104830341A (en) * | 2015-05-15 | 2015-08-12 | 福州大学 | Preparation method of rare-earth-ion-doped yttrium fluoride green upconversion fluorescent material |
| US20190352761A1 (en) * | 2018-05-18 | 2019-11-21 | Shin-Etsu Chemical Co., Ltd. | Spray material, sprayed member and making method |
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Application publication date: 20211207 |