Method for preparing nano silicon-base porous luminescent material by normal pressure plasma gas phase deposition

Abstract

The invention relates to a method of preparing nano Si-based multi-hole luminescent material by atmospheric pressure plasma vapor deposition, which includes the following procedures: (1) a deposition substrate is arranged below a three-dimensional comb-shaped electrode, and a mechanical pump removes the air in a reaction chamber. (2) the mixed gas is fed through an umbrella washer of a gas inlet, to adjust the flow speed of the mixed gas and control the pressure in a deposition chamber to be near atmospheric pressure. (3)after the pressure in the reaction chamber becomes stable, the pulse bias is added to a basal, to adjust the frequency and power of a plasma generator. (4) after the discharge reaction, the substrate is taken out, and the nano Si-based multi-hole luminescent film is obtained. The method can be used in equipments which has dry environment, simple fitting, convenience in operation, and is near to atmospheric pressure, to change the plasma discharge parameters and pulse bias, and adjust the proportion and flow, etc of monomers and carrier gases, which can obtain high quality nano Si-based multi-hole luminescent films with different grain size, hole structures, components and film thicknesses, and provides adjustable luminescence radiation wave length and improved luminescence efficiency.

Description

technical field

[0001] The invention relates to a method for preparing nanometer silicon-based porous luminescent film material by plasma vapor deposition, in particular to a method for preparing nanometer silicon-based porous luminescent film material by plasma vapor deposition under normal pressure. Background technique

[0002] In 1990, British scientist L.T.Canham discovered the photoluminescence (Photoluminescence: PL) of porous silicon (Porous Si: PS) at room temperature. Canham found that porous silicon can radiate strong fluorescence in the near-infrared and visible light regions, and its quantum efficiency reaches 1% to 10%, while the quantum efficiency of single crystal silicon is only 10% under the same conditions. -4 %, which increased the luminous efficiency by 4 to 5 orders of magnitude immediately caused a worldwide sensation, enabling the world to see a new way to realize the luminescence of Si-based materials, and thus created a new situation in the research...

Examples

Embodiment 1

[0033] The deposition substrate is made of glass sheet, which is ultrasonically cleaned with ethanol and deionized water, and placed in a plasma reactor. The electrode is a tungsten wire with a diameter of 0.1 mm, and is covered with a quartz tube. The number of electrodes is 12, 5 layers, and the distance between electrodes and the distance between layers Both are 5mm, the distance between the substrate and the discharge area is 0.3cm, and the vacuum is evacuated to the background vacuum degree ≤ 10 3 After Pa, pass into the mixed gas containing silane, argon, hydrogen, the ratio is: silane: argon: hydrogen = 4: 95: 1, adjust the flow rate to be 140SCCM, control the vacuum degree of 1.05 * 10 5 Pa, opening frequency 2×10 4 Hz plasma power supply, controlled discharge power of 5W, bias voltage of 100V, pulse ratio of 90%, and discharge time of 10 minutes.

[0034] After deposition, the glass slide was detected by high-resolution transmission electron microscope SEM. The resul...

Embodiment 2

[0036] The deposition substrate is made of silicon polyester sheet. After ultrasonic cleaning with ethanol and deionized water, it is placed in a plasma reactor. The electrodes are made of stainless steel with a diameter of 3 mm and are covered with alumina ceramic tubes. The number of electrodes is 8, 2 layers, and the distance between electrodes is the same as The distance between layers is 3mm, the distance between the substrate and the discharge area is 0.5cm, and the vacuum is evacuated to the background vacuum degree ≤ 10 3 After Pa, pass into the mixed gas containing silane, argon, hydrogen, the ratio is: silane: helium: hydrogen = 1:98:2, adjust the flow rate to be 140SCCM, control the vacuum degree of 1.0×10 5 Pa, opening frequency 2×10 4 Hz plasma power supply, controlled discharge power of 500W, bias voltage of -300V and -850V, pulse ratio of 16%, and discharge time of 3 minutes.

[0037] After the deposition, the polyester sheet was detected by high-resolution tra...

Embodiment 3

[0039]The deposition substrate is a P-type (100) silicon wafer. After ultrasonic cleaning with ethanol and deionized water, it is placed in a plasma reactor. The inter-layer distance and the inter-layer distance are both 1mm, the distance between the substrate and the discharge area is 0.5cm, and the vacuum is evacuated to a background vacuum degree of ≤10 3 After Pa, pass into the mixed gas containing silane, argon, hydrogen, the ratio is: silane: argon: hydrogen = 1: 89: 10, the adjustment flow rate is 140SCCM, and the control vacuum is 1.03 × 10 5 Pa, opening frequency 2×10 4 Hz plasma power supply, the control discharge power is 500W, the bias voltages are respectively -200, -450, -700, -850V, the pulse ratio is 16%, and the discharge time is 10 minutes.

[0040] After deposition, the glass slides were detected by laser fluorescence spectroscopy, and the results showed that under the excitation light of 320nm, blue-violet light with a center wavelength of 450nm was emitte...

technical field

[0001] The invention relates to a method for preparing nanometer silicon-based porous luminescent film material by plasma vapor deposition, in particular to a method for preparing nanometer silicon-based porous luminescent film material by plasma vapor deposition under normal pressure. Background technique

[0002] In 1990, British scientist L.T.Canham discovered the photoluminescence (Photoluminescence: PL) of porous silicon (Porous Si: PS) at room temperature. Canham found that porous silicon can radiate strong fluorescence in the near-infrared and visible light regions, and its quantum efficiency reaches 1% to 10%, while the quantum efficiency of single crystal silicon is only 10% under the same conditions. -4 %, which increased the luminous efficiency by 4 to 5 orders of magnitude immediately caused a worldwide sensation, enabling the world to see a new way to realize the luminescence of Si-based materials, and thus created a new situation in the research...

Examples

Embodiment 1

[0033] The deposition substrate is made of glass sheet, which is ultrasonically cleaned with ethanol and deionized water, and placed in a plasma reactor. The electrode is a tungsten wire with a diameter of 0.1 mm, and is covered with a quartz tube. The number of electrodes is 12, 5 layers, and the distance between electrodes and the distance between layers Both are 5mm, the distance between the substrate and the discharge area is 0.3cm, and the vacuum is evacuated to the background vacuum degree ≤ 10 3 After Pa, pass into the mixed gas containing silane, argon, hydrogen, the ratio is: silane: argon: hydrogen = 4: 95: 1, adjust the flow rate to be 140SCCM, control the vacuum degree of 1.05 * 10 5 Pa, opening frequency 2×10 4 Hz plasma power supply, controlled discharge power of 5W, bias voltage of 100V, pulse ratio of 90%, and discharge time of 10 minutes.

[0034] After deposition, the glass slide was detected by high-resolution transmission electron microscope SEM. The resul...

Embodiment 2

[0036] The deposition substrate is made of silicon polyester sheet. After ultrasonic cleaning with ethanol and deionized water, it is placed in a plasma reactor. The electrodes are made of stainless steel with a diameter of 3 mm and are covered with alumina ceramic tubes. The number of electrodes is 8, 2 layers, and the distance between electrodes is the same as The distance between layers is 3mm, the distance between the substrate and the discharge area is 0.5cm, and the vacuum is evacuated to the background vacuum degree ≤ 10 3 After Pa, pass into the mixed gas containing silane, argon, hydrogen, the ratio is: silane: helium: hydrogen = 1:98:2, adjust the flow rate to be 140SCCM, control the vacuum degree of 1.0×10 5 Pa, opening frequency 2×10 4 Hz plasma power supply, controlled discharge power of 500W, bias voltage of -300V and -850V, pulse ratio of 16%, and discharge time of 3 minutes.

[0037] After the deposition, the polyester sheet was detected by high-resolution tra...

Embodiment 3

[0039]The deposition substrate is a P-type (100) silicon wafer. After ultrasonic cleaning with ethanol and deionized water, it is placed in a plasma reactor. The inter-layer distance and the inter-layer distance are both 1mm, the distance between the substrate and the discharge area is 0.5cm, and the vacuum is evacuated to a background vacuum degree of ≤10 3 After Pa, pass into the mixed gas containing silane, argon, hydrogen, the ratio is: silane: argon: hydrogen = 1: 89: 10, the adjustment flow rate is 140SCCM, and the control vacuum is 1.03 × 10 5 Pa, opening frequency 2×10 4 Hz plasma power supply, the control discharge power is 500W, the bias voltages are respectively -200, -450, -700, -850V, the pulse ratio is 16%, and the discharge time is 10 minutes.

[0040] After deposition, the glass slides were detected by laser fluorescence spectroscopy, and the results showed that under the excitation light of 320nm, blue-violet light with a center wavelength of 450nm was emitte...

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