阅读说明：本技术 一种氟化钇薄膜的制备方法 (Preparation method of yttrium fluoride film ) 是由 陈如明 姜蕻 蔡勇 于 2020-07-15 设计创作，主要内容包括：本发明公开了一种氟化钇薄膜的制备方法,步骤1：将水合硝酸钇、氟化铵按照摩尔配比1:3.05-1:3.75混合均匀；步骤2：将胶状物干燥得到胶态物质；步骤3：将胶态物质置于高温炉中；步骤4：胶态物质研磨得到粉末；步骤5：将粉末在惰性气体保护下得到纳米级粉末；步骤6：将纳米级粉末采取浸渍提拉法或旋转涂覆法制膜；步骤7：将湿膜烘干、冷得到薄膜；步骤8：将薄膜退火处理,随炉冷却后得到氟化钇薄膜。本发明氟化钇薄膜的制备方法与现有的技术相比,制备的氟化钇薄膜表面光滑,具有良好的超导特性,且薄膜制备成本低、工艺简单且容易控制；热处理工艺周期大大缩短,薄膜制备效率大大提高,膜层结合牢固,很难破裂。(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.)

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.

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.