Method for preparing Sm2O3 film by solvent heat method

A solvothermal, thin-film technology, applied in solid-state chemical plating, metal material coating process, coating, etc., can solve the problem of poor adhesion between thin film and substrate, high hydrothermal reaction temperature, long sol preparation cycle, etc. problems, to achieve the effect of no visible defects, good bonding force and high appearance quality

Active Publication Date: 2012-01-25
JIANGSU XINGYUAN POWER PLANT & METALLURGICAL EQUIP MFG
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AI Technical Summary

Problems solved by technology

These two methods have very high requirements on equipment, and the equipment and instruments are relatively expensive. Since evaporation exists in the entire container, it is difficult for Sm 2 o 3 The utilization rate of raw materials is very small
Meanwhile, the sol-gel method prepared Sm 2 o 3 Thin film, sol preparation cycle is long, and the uniformity is poor, and the film needs post-heat treatment, which will cause defects such as film curling, dry cracking, grain coarsening, poor bonding force between the film and the substrate, or atmosphere reaction.
Preparation of Sm by hydrothermal method 2 o 3 Thin film, high hydrothermal reaction temperature, difficult to obtain pressure, long reaction time

Method used

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  • Method for preparing Sm2O3 film by solvent heat method
  • Method for preparing Sm2O3 film by solvent heat method

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Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1: step one: will analyze pure SmCl 3 ·6H 2 O was added to isopropanol and stirred with a magnetic stirrer to obtain Sm 3+ Solution A with a concentration of 0.05mol / L;

[0019] Step 2: Heat and stir the solution A at 40° C., adjust the pH value of the solution A to 5.40 by using an ammonia solution with a mass percent concentration of 8%, and continue to stir for 5 hours to form a coating solution;

[0020] Step 3: Pour the coating solution into the hydrothermal kettle, the filling degree is controlled at 50%, immerse the cleaned substrate in the coating solution, then seal the hydrothermal kettle, and put it into the DHG-9075A electric vacuum drying oven , control the hydrothermal temperature to 120 ° C for 48 hours, and naturally cool to room temperature after the reaction;

[0021] Step 4: Open the hydrothermal kettle, take out the substrate, rinse it with absolute ethanol, and place it in a vacuum drying oven at 80°C for 8 hours to obtain Sm on the su...

Embodiment 2

[0022] Embodiment 2: step one: will analyze pure SmCl 3 ·6H 2 O was added to a mixed solvent of isopropanol and water, and stirred with a magnetic stirrer to prepare Sm 3+ Solution A with a concentration of 0.08mol / L;

[0023] Wherein, the mixed solvent of isopropanol and water by volume ratio V 水 :V 异丙醇 = 3;

[0024] Step 2: Heat and stir the solution A at 53° C., adjust the pH value of the solution A to 6.00 by using an ammonia solution with a mass percent concentration of 10%, and continue stirring for 3 hours to form a coating solution;

[0025] Step 3: Pour the coating solution into the hydrothermal kettle, the filling degree is controlled at 60%, immerse the cleaned substrate in the coating solution, then seal the hydrothermal kettle, and put it into the DHG-9075A electric vacuum drying oven , control the hydrothermal temperature to 180 ° C for 20 hours, and naturally cool to room temperature after the reaction;

[0026] Step 4: Open the hydrothermal kettle, take o...

Embodiment 3

[0027] Embodiment 3: step one: will analyze pure SmCl 3 ·6H 2 O was added to a mixed solvent of isopropanol and water, and stirred with a magnetic stirrer to prepare Sm 3+ Solution A with a concentration of 0.1mol / L;

[0028] Wherein, the mixed solvent of isopropanol and water by volume ratio V 水 :V 异丙醇 = 2;

[0029]Step 2: Heat and stir the solution A at 55° C., adjust the pH value of the solution A to 5.80 by using an ammonia solution with a mass percent concentration of 6%, and continue stirring for 4 hours to form a coating solution;

[0030] Step 3: Pour the coating solution into the hydrothermal kettle, the filling degree is controlled at 55%, immerse the cleaned substrate in the coating solution, then seal the hydrothermal kettle, and put it into the DHG-9075A electric vacuum drying oven , control the hydrothermal temperature to 150 ° C for 30 hours, and naturally cool to room temperature after the reaction;

[0031] Step 4: Open the hydrothermal kettle, take out ...

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Abstract

The invention discloses a method for preparing a Sm2O3 film by a solvent heat method. The method comprises the following steps of: adding analytically pure SmCl3.6H2O into isopropyl alcohol or a mixed solvent of the isopropyl alcohol and water, stirring, and thus obtaining solution A; adjusting the pH value of the solution A by using ammonia water to form coating film liquid; pouring the coating film liquid into a hydrothermal kettle, soaking a substrate into the coating film liquid, sealing the hydrothermal kettle, reacting at the hydrothermal temperature of between 120 and 200 DEG C for 12 to 48 hours, and naturally cooling to room temperature; and opening the hydrothermal kettle, taking the substrate out, washing by using absolute ethanol cleanly, drying in a vacuum drying oven, and thus obtaining the Sm2O3 optical film on the surface of the substrate. In the method, a reaction for preparing the Sm2O3 film is finished in a liquid phase at a time without crystallization thermal treatment at a later stage, so that the defects of curl, seasoning crack, grain coarsening of the Sm2O3 film which are possibly caused in the thermal treatment process, reaction of the film with the substrate or the atmosphere and the like are overcome; the method has simple process equipment, is low in reaction temperatures and makes high pressure easily generated, the obtained film has higher purity, and crystal grains grow controllably. The film which is uniform and compact, does not have visible defects and has higher bonding force and higher appearance quality can be prepared.

Description

technical field [0001] The present invention relates to a kind of preparation Sm 2 o 3 Thin film method, particularly relates to a kind of solvothermal preparation Sm 2 o 3 thin film method. Background technique [0002] SM 2 o 3 It is a light yellow powder, easy to deliquescence, insoluble in water, soluble in inorganic acid. SM 2 o 3 It is a new generation of energy conversion materials and photoelectric thin film materials. SM 2 o 3 Thin films can be used to prepare optical switches, data storage, photoelectric conversion elements and electrical switches, etc.; Sm 2 o 3 Thin films can also be used in filters of electronic devices, magnetic materials and special glasses; in addition, nano-Sm 2 o 3 It can also be used in ceramic capacitors and catalysts, and has broad development prospects. [0003] The currently reported preparation of Sm 2 o 3 The method of optical film is mainly vacuum evaporation [V.A.Rozhkov, A.Yu.Trusova, I.G.Berezhnoy.Silicon MIS str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C20/08
Inventor 殷立雄黄剑锋郝巍曹丽云吴建鹏黄艳
Owner JIANGSU XINGYUAN POWER PLANT & METALLURGICAL EQUIP MFG
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