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Preparation method of orthorhombic tin dioxide thin film

A tin dioxide and orthogonal phase technology, which is applied in the field of preparation of inorganic oxide thin film materials, can solve the problems of property detection and technical application stagnation, and difficulty in synthesis

Inactive Publication Date: 2012-10-31
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, another crystal structure of tin dioxide: the orthorhombic phase, is difficult to synthesize due to its high temperature and high pressure phase, and its property detection and technical application have been stagnant

Method used

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  • Preparation method of orthorhombic tin dioxide thin film
  • Preparation method of orthorhombic tin dioxide thin film
  • Preparation method of orthorhombic tin dioxide thin film

Examples

Experimental program
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Embodiment 1

[0018] The preparation method of this orthorhombic phase tin dioxide thin film, concrete operation steps are as follows:

[0019] a. In order to obtain tin dioxide targets for pulsed laser deposition, we prepared high-purity tin dioxide powder (99.8 %) by sol-gel method. The preparation process and steps are: at 27±2% SnCl 4 Add 28 ± 2% ammonia water drop by drop in the ethanol solution to make the reaction uniform. During the reaction, the pH value is detected in real time. When the pH = 7, the reaction is terminated, and a white sol can be observed. After aging for 24 ± 0.2 hours, Wash several times with ethanol and acetone, and use AgNO 3 Test the filtrate until no Cl is detected - Until now, the obtained gel is placed in a vacuum drying oven at 100°C ± 5°C to dry the water and detergent to obtain a block sample, which is ground into powder to prepare a tin dioxide powder with a particle size of about 4 ± 0.5 nanometers. The powder is made into a round block wit...

Embodiment 2

[0022] This embodiment is exactly the same as Example 1, and the obtained orthorhombic tin dioxide film is tested and studied:

[0023] X-ray diffraction (XRD) studies show that: the main crystal plane index of the prepared orthorhombic tin dioxide film ( figure 2 a-i) Standard X-ray diffraction with orthorhombic tin dioxide (PDF file number: 78-1063, figure 2 a-iii) Basically the same, for example: orthorhombic tin dioxide (111), (112), (113), (002), (006), (115), (200), (117), (222) , (130), (224) and (119) facets, but the (101), (110), (002), (200), (112) and (211) facets of tetragonal tin oxide cannot be excluded (PDF file No.: 85-0712). Therefore, sufficient evidence is needed to further confirm whether the film is orthorhombic tin dioxide. At the same time, the film was placed for half a year, and further X-ray diffraction ( figure 2 a-ii) The research shows that the film is stable and there is no change in the phase.

[0024] X-ray photoelectron ener...

Embodiment 3

[0026] The preparation method of the present embodiment is exactly the same as that of Example 1, and the gained orthorhombic tin dioxide film is studied as follows:

[0027] Mössbauer spectrum research shows that the isotropic shift (IS) and quadrupole split (QS) values ​​are 0 mm / s and 0.6 mm / s, respectively. This experiment fully proves that tin is +4 Valence( image 3 a).

[0028] X-ray electron energy loss (EDS) spectrum research shows that the percentages of tin and oxygen atoms in the film are 33.4 % and 66.6 % respectively, that is, the atomic ratio of tin and oxygen is 1:2. ( image 3 b). It can be deduced that the composition of this film is tin dioxide and the possibility of tin monoxide is excluded.

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Abstract

The invention relates to a preparation method of an orthorhombic tin dioxide thin film, which comprises the following operation steps that: (i) preparing a tin dioxide target used for pulsed laser deposition: (1) preparing high-purity tin dioxide powder; and (2) preparing the powder into a round block with the diameter of 15mm and the thickness of 4mm at the pressure of 0.4GPa, and sintering the round block for 2 hours at 1150 DEG C to obtain the tin dioxide target used for pulsed laser deposition; and (ii) impacting the target by utilizing a pulsed laser deposition method to obtain the deposited orthorhombic tin dioxide thin film. The preparation conditions of the high-temperature high-pressure orthorhombic tin dioxide thin film at a relatively low pressure and relatively low temperatureare discovered in the invention.

Description

technical field [0001] The invention relates to a preparation technology of a high-temperature, high-pressure orthogonal-phase tin dioxide thin film under relatively low pressure and low temperature, and belongs to the technical field of preparation technology of inorganic oxide thin film materials. Background technique [0002] Tin dioxide is a new type of practical functional material with the most application value at present. It has broad application prospects in the fields of solar cells, transparent electrodes, and gas sensors. Under normal circumstances, tin dioxide mainly exists in nature in the form of cassiterite. Cassiterite tin dioxide has a rutile tetragonal crystal structure. Its electrical, optical and gas sensing properties have been extensively and deeply studied. However, another crystal structure of tin dioxide: the orthorhombic phase, is difficult to synthesize due to its high temperature and high pressure phase, and its property detection and technica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01L49/02C01G19/02H10N97/00
Inventor 陈志文王剑杜娟焦正吴明红
Owner SHANGHAI UNIV