Hydrothermal preparation method of nickel passivated porous silicon

A technology of porous silicon and silicon wafer, applied in the field of hydrothermal preparation of porous silicon, can solve the problems of complicated experimental process, uneven pore size of porous silicon, narrow application of porous silicon, etc., and achieve the effect of concentrated size distribution and good uniformity

Inactive Publication Date: 2017-12-12
CHONGQING UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method needs to use various organic solvents for reaction, and needs to be selected from various transition metal salts. The experimental process is relatively complicated, and the application of the obtained porous silicon is relatively narrow, mainly used in batteries.
Patent CN1241611 discloses a preparation method of iron-passivated porous silicon. The p type single crystal silicon chip with a resistivity of 7-9Ω·cm and the p type single crystal silicon wafer with a resistivity of 4-6Ω·cm are selected. The crystalline silicon wafer is used as the raw material, and ferric nitrate and hydrofluoric acid are used as the corrosion system. The pore size of the prepared porous silicon is not uniform, but due to the in-situ corrosion of iron ions, the luminous intensity is strong, and the luminous peak position is almost unchanged.
[0006] The porous silicon produced by the above technology has a common feature, the uniformity of the pore structure needs to be improved and the photoluminescence phenomenon and the uniformity of the pores cannot coexist

Method used

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  • Hydrothermal preparation method of nickel passivated porous silicon
  • Hydrothermal preparation method of nickel passivated porous silicon
  • Hydrothermal preparation method of nickel passivated porous silicon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Cut an n-type single crystal silicon wafer with a crystal plane of and a resistivity of 2-4Ω·cm into a square piece of 1x1cm, soak in acetone and absolute ethanol for 3 minutes each, and rinse with distilled water after the end; use 10 Soak in %HF solution for about 10 minutes, and rinse with distilled water after the end; NH 3 ·H 2 O (28%), H 2 o 2 、H 2 O (volume ratio 1:1:5) mixed solution and HCl (37%), H 2 o 2 、H 2 O (volume ratio 1:1:5) mixed solutions, each soaked for 5min, rinsed with distilled water after the end. The above treated silicon wafer was fixed on the inner lining of the hydrothermal reactor, and then a mixed etching solution was added: 52mL of hydrofluoric acid (40%), 1.1632g of nickel nitrate, 26mL of distilled water and 2mL of absolute ethanol. Seal and heat up, and react at 140° C. for 60 minutes to obtain nickel-passivated porous silicon.

[0039] The morphology of the samples was observed by scanning electron microscope (SEM).

[0040]...

Embodiment 2

[0042]Other treatment conditions are the same as in Example 1, only the concentration of nickel nitrate in the mixed corrosion solution is increased to 0.2mol / L. The morphology of the samples was also observed with a scanning electron microscope (SEM). Such as figure 2 As shown, compared with the porous silicon prepared in Example 1, the uniformity of the pore structure is reduced.

Embodiment 3

[0044] The other treatment conditions are the same as in Example 1, except that post-annealing treatment is added: the porous silicon is taken out from the etching solution, washed with deionized water, and then directly placed in high-purity nitrogen at 900° C. for 3 hours for annealing.

[0045] Such as image 3 As shown, the size of the post-treated porous silicon increases, and the uniformity is significantly improved.

[0046] The photoluminescence phenomenon of the porous silicon sample prepared in the above-mentioned examples 1 and 2 is tested: the optical fiber test composed of USB2000-FLG fiber optic spectrometer, LS-450 light emitting diode, R400-7 trans probe (Ocean Optics, USA) system. Such as Figure 4 As shown, the luminescence peak of the sample in Example 1 is narrower and the luminescence intensity is higher. The luminescence peak of the sample in Example 2 is wider and weaker than that of the sample in Example 1.

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Abstract

The invention discloses a hydrothermal preparation method of nickel passivated porous silicon. The method comprises the following steps: performing combination pretreatment on n-type monocrystalline silicon wafers; providing a mixed corrosive solution composed of hydrofluoric acid, nickel nitrate and ethanol; carrying out a nickel passivation reaction on the silicon wafers subjected to combination pretreatment and the mixed corrosive solution in a lining of a hydrothermal reactor, thereby obtaining the porous silicon. The pore structure of the porous silicon prepared by the method disclosed by the invention has excellent stability and uniformity.

Description

technical field [0001] The invention relates to a hydrothermal preparation method of porous silicon. Background technique [0002] The development of porous silicon mainly goes through the following stages: As early as the 1950s, Uhlir of Bell Laboratories in the United States accidentally discovered and reported that porous silicon films could be formed through electrochemical corrosion experiments. In 1958, D. Turner explored the principle of electrochemical anodic oxygen to form porous films, and discussed in detail the corrosion conditions and related properties of forming films. In 1984, Pickering et al. observed the fluorescence of porous silicon in the visible wavelength range at low temperature (4.2k). In 1990, when the British scientist Canham irradiated the surface of porous silicon with ultraviolet light at room temperature, he found that porous silicon had a strong luminescence phenomenon at room temperature, which is also called photoluminescence. [0003] Due...

Claims

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Application Information

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IPC IPC(8): C09K11/59C09K11/02
CPCC09K11/025C09K11/60
Inventor 谢玉婷王梦真黎学明陶志杨文静祝凡
Owner CHONGQING UNIV
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