CN103898458A - Method for preparing silicon nano crystal film by adopting spiral wave plasma sputtering technology - Google Patents
Method for preparing silicon nano crystal film by adopting spiral wave plasma sputtering technology Download PDFInfo
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- CN103898458A CN103898458A CN201410125282.8A CN201410125282A CN103898458A CN 103898458 A CN103898458 A CN 103898458A CN 201410125282 A CN201410125282 A CN 201410125282A CN 103898458 A CN103898458 A CN 103898458A
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Abstract
The invention discloses a method for preparing a silicon nano crystal film by adopting a spiral wave plasma sputtering technology. The method comprises the steps of: thermally generating a silicon dioxide layer on a silicon substrate; sintering a mixture of silicon powder and silicon dioxide powder in a certain ratio into a target at high temperature, and depositing the target on the silicon dioxide layer by adopting the spiral wave plasma sputtering technology. The silicon nano crystal film with the diameter of 4-6nm can be prepared on the silicon dioxide layer by controlling the temperature of the substrate without high-temperature annealing. The method is compatible with a mature silicon-based photoelectronic process, and has a wide application prospect in the field of preparation and processing of semiconductor materials.
Description
Technical field
The present invention relates to a kind of silicon nano-crystalline film preparation method, be specifically related to a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film.
Background technology
Silicon nano-crystalline film specific conductivity is high, have that room temperature is photic, electricity causes the properties such as visible ray is luminous, aspect the Si quantum dot device such as electron emission, single electron tunnelling and Si base be luminous, having huge application potential, is important, the core component of opto-electronic device and nano electron device.This class device comprises: third generation nano-crystalline solar battery chip, silicon single-electron device, single-electron memory etc.Therefore, the preparation method of silicon nano-crystalline film and characteristic research have become the focus of international research.Granular nano-silicon can obtain by the technology such as magnetron sputtering or ion beam evaporation; And the amorphous silicon membrane that is inlaid with nano-silicon can make by methods such as pulsed laser depositions.
Traditional method of preparing silicon nano-crystalline film: as MOCVD, PECVD, MBE, ion implantation etc., its shortcoming is preparation means complexity.Though and electron beam evaporation is prepared the method for silicon nanocrystal and has been improved compared with aforesaid method; but easily produce radiation injury; thereby destroy substrate and dielectric film, and the also high temperature annealing under atmosphere protection again of the film making, finally could form silicon nano-crystalline film.
Summary of the invention
Goal of the invention of the present invention is to provide a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film, in Helicon wave plasma sputter equipment, with Helicon wave plasma sputtering technology, realize fast deposition silicon nano-crystalline film, and with traditional silica-based process compatible.
To achieve the above object of the invention, the technical solution used in the present invention is: a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film, comprises the steps:
(1) on silicon substrate, thermooxidizing forms silicon dioxide layer;
(2) by the mixture of Si powder and SiO 2 powder, after high temperature sintering as target;
(3) target of preparation in step (2) is put into Helicon wave plasma sputter equipment, under the environment of axial magnetic field, on silicon dioxide layer, form silicon nano-crystalline film by the Helicon wave plasma sputtering method of radio-frequency modulations.
In technique scheme, the silicon substrate in described step (1) is the one in low-resistance silicon substrate, HR-Si substrate and silicon-on-insulator substrate.
In technique scheme, in described step (1), adopt thermal oxidation process on silicon substrate, to form silicon dioxide layer, comprising:
Pre-heating stage: 150 DEG C～300 DEG C of temperature, time 30～40s, oxygen flow 0.6～0.8L/min;
Temperature rise period: 600 DEG C～650 DEG C of temperature, time 4～8s, oxygen flow 0.6～0.8L/min;
The constant temperature stage: 650 DEG C～750 DEG C of temperature, time 600～800s, oxygen flow 0.6～0.8L/min.
Further technical scheme, described step (1) also comprises: successively silicon dioxide layer is carried out to ultrasonic cleaning with acetone, dehydrated alcohol, deionized water.
Further technical scheme, the mass ratio of Si powder and SiO 2 powder is 1: 1～3.Preferred technical scheme, described in described step (2), target is formed by the mixture sintering of 25 gram of 300 order Si powder and 35 gram of 300 order SiO 2 powder.
In technique scheme, in described step (3), the processing parameter of Helicon wave plasma sputter is: underlayer temperature is 150 DEG C～350 DEG C, and base vacuum is 2.2 × 10
-4pa, sputter working gas is purity higher than 99.99% Ar gas, and sputtering time is 60s～200s, and flow is respectively 15～30 sccm, and operating air pressure is 0.4Pa.
In technique scheme, in described step (3), rf frequency is 13.56MHz, and power is 550W～1200W.
In technique scheme, in described step (3), axially magneticstrength is no more than 6400Gs, and preferred, axial magnetic field intensity is 6000Gs.
Because technique scheme is used, the present invention compared with prior art has following advantages:
The present invention is under the axial magnetic field strength condition of 6000Gs, prepare silicon nano-crystalline film by Helicon wave plasma sputtering technology, compared with thering is the Ecr plasma of same gas launching efficiency, excite Helicon wave plasma equipment used simple, the selection of cavity aperture ratio is freer, in industrial production, more easily realizes; Compared with electron beam evaporation, the method such as ion implantation, save the follow-up step that could form silicon nano-crystalline film through high temperature annealing, processing step is simple, and sedimentation rate is fast.
Brief description of the drawings
Fig. 1 is the method flow diagram of preparing silicon nano-crystalline film of the present invention in embodiment mono-.
Fig. 2 is the SEM photo of the silicon nano-crystalline film prepared of the present invention.
Fig. 3 is the TEM photo of the silicon nano-crystalline film prepared of the present invention.
Fig. 4 is the Raman spectrogram of the silicon nano-crystalline film prepared of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
Embodiment mono-: shown in Figure 1, a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film, comprises the steps:
(1) adopting crystal orientation is <100>, and thickness is that the silicon single crystal of 0.4 μ m is substrate, with industrial standards wet-cleaned, removes natural oxidizing layer and the various pickup thing of silicon face.
By the silicon substrate having cleaned up, put into RTP-1200 quick anneal oven and be oxidized, form fine and close silicon dioxide layer at silicon face.The thermooxidizing condition of substrate is in table 1:
Table 1: the processing condition of heat growth silicon dioxide layer
The silica/silicon substrate making is used respectively to acetone, dehydrated alcohol and deionized water ultrasonic cleaning 5 minutes, then in vacuum drying oven, under 150 DEG C, 5Pa condition, dry.
(2) mixture 25 gram of 300 order Si powder and 35 gram of 300 order SiO 2 powder being formed, after high temperature sintering as target;
(3) target of preparation in step (2) is put into Helicon wave plasma sputter equipment, under the environment of axial magnetic field, on silicon dioxide layer, form silicon nano-crystalline film by the Helicon wave plasma sputtering method of radio-frequency modulations;
Concrete technology parameter is: underlayer temperature is 300 DEG C, and cavity base vacuum is 2.2 × 10
-4pa, sputter gas is that purity is 99.999% Ar gas, and sputtering time is 100 seconds, and Ar airshed is 25sccm; Operating air pressure is 0.4Pa, the radio frequency of 13.56MHz, and radio frequency power is 800W, it is 6000Gs that institute adds axial magnetic field intensity.
The present embodiment middle thermal oxidation process that adopts in step (1) forms silicon dioxide layer on silicon substrate, comprising:
Pre-heating stage: 150 DEG C～300 DEG C of temperature, time 30～40s, oxygen flow 0.6～0.8L/min;
Temperature rise period: 600 DEG C～650 DEG C of temperature, time 4～8s, oxygen flow 0.6～0.8L/min;
The constant temperature stage: 650 DEG C～750 DEG C of temperature, time 600～800s, oxygen flow 0.6～0.8L/min.
Shown in Fig. 2 and 3, the silicon nano-crystalline film diameter that the present invention makes is about 4～6nm.
Shown in Figure 4, the Raman peak values of the silicon nano-crystalline film that the present invention makes is positioned at 515cm
-1place, the Raman peak position of this peak value and silicon nanocrystal matches, and shows can successfully make silicon nano-crystalline film with the present invention.
Claims (8)
1. adopt Helicon wave plasma sputtering technology to prepare a method for silicon nano-crystalline film, it is characterized in that comprising the steps:
(1) on silicon substrate, thermooxidizing forms silicon dioxide layer;
(2) mixture Si powder and SiO 2 powder being formed, after high temperature sintering as target;
(3) target of preparation in step (2) is put into Helicon wave plasma sputter equipment, under the environment of axial magnetic field, on the silicon dioxide layer obtaining in step (1) by the Helicon wave plasma sputtering method of radio-frequency modulations, form silicon nano-crystalline film.
2. a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, is characterized in that: the silicon substrate in described step (1) is the one in low-resistance silicon substrate, HR-Si substrate and silicon-on-insulator substrate.
3. a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, is characterized in that: in described step (1), adopt thermal oxidation process on silicon substrate, to form silicon dioxide layer, comprising:
Pre-heating stage: 150 DEG C～300 DEG C of temperature, time 30～40s, oxygen flow 0.6～0.8L/min;
Temperature rise period: 600 DEG C～650 DEG C of temperature, time 4～8s, oxygen flow 0.6～0.8L/min;
The constant temperature stage: 650 DEG C～750 DEG C of temperature, time 600～800s, oxygen flow 0.6～0.8L/min.
4. a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, it is characterized in that, described step (1) also comprises: successively silicon dioxide layer is carried out to ultrasonic cleaning with acetone, dehydrated alcohol, deionized water.
5. a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, is characterized in that: described in described step (2), target is formed by the mixture sintering of 25 gram of 300 order Si powder and 35 gram of 300 order SiO 2 powder.
6. a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, it is characterized in that: in described step (3), the processing parameter of Helicon wave plasma sputter is: underlayer temperature is 150 DEG C～350 DEG C, and base vacuum is 2.2 × 10
-4pa, sputter working gas is purity higher than 99.99% Ar gas, and sputtering time is 60s～200s, and flow is 15～30 sccm, and operating air pressure is 0.4Pa.
7. a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, is characterized in that: in described step (3), rf frequency is 13.56MHz, and power is 550W～1200W.
8. a kind of method that adopts Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, is characterized in that: in described step (3), axially magneticstrength is no more than 6400Gs.
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Cited By (4)
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| CN104480428A (en) * | 2014-12-02 | 2015-04-01 | 中国航天科工集团第三研究院第八三五八研究所 | Method for regulating and controlling ion beam sputtered silicon dioxide optical membrane stress |
| CN105755449A (en) * | 2016-05-18 | 2016-07-13 | 苏州大学 | Method for preparing nanocrystalline diamond film by adopting helicon wave plasma technology |
| CN115074689A (en) * | 2022-07-21 | 2022-09-20 | 苏州大学 | Method for preparing titanium nitride film by helicon wave plasma reactive sputtering deposition |
| CN115110025A (en) * | 2022-07-20 | 2022-09-27 | 苏州大学 | Method for sputtering and depositing tungsten nitride film by using helicon wave plasma |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480428A (en) * | 2014-12-02 | 2015-04-01 | 中国航天科工集团第三研究院第八三五八研究所 | Method for regulating and controlling ion beam sputtered silicon dioxide optical membrane stress |
| CN105755449A (en) * | 2016-05-18 | 2016-07-13 | 苏州大学 | Method for preparing nanocrystalline diamond film by adopting helicon wave plasma technology |
| CN105755449B (en) * | 2016-05-18 | 2018-09-25 | 苏州大学 | The method that nanocrystalline diamond film is prepared using Helicon wave plasma technology |
| CN115110025A (en) * | 2022-07-20 | 2022-09-27 | 苏州大学 | Method for sputtering and depositing tungsten nitride film by using helicon wave plasma |
| CN115110025B (en) * | 2022-07-20 | 2023-10-20 | 苏州大学 | Method for depositing tungsten nitride film by helicon wave plasma sputtering |
| CN115074689A (en) * | 2022-07-21 | 2022-09-20 | 苏州大学 | Method for preparing titanium nitride film by helicon wave plasma reactive sputtering deposition |
| CN115074689B (en) * | 2022-07-21 | 2023-06-02 | 苏州大学 | Method for preparing titanium nitride film by spiral wave plasma reactive sputtering deposition |
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