CN103898458B - A kind of method adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film - Google Patents
A kind of method adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film Download PDFInfo
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- CN103898458B CN103898458B CN201410125282.8A CN201410125282A CN103898458B CN 103898458 B CN103898458 B CN 103898458B CN 201410125282 A CN201410125282 A CN 201410125282A CN 103898458 B CN103898458 B CN 103898458B
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Abstract
The invention discloses a kind of method adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film, comprising: heat generates silicon dioxide layer on a silicon substrate; By the Si powder of certain proportioning and the mixture of SiO 2 powder, high temperature sintering becomes target, with Helicon wave plasma sputtering technology, is deposited on described silicon dioxide layer.By controlling substrate temperature, do not need again through high temperature annealing, can on above-mentioned silicon dioxide layer, the silicon nano-crystalline film of obtained 4-6nm diameter.Method involved in the present invention is mutually compatible with the ripe sub-technique of silicon based opto-electronics, at preparation and the manufacture field of semiconductor material, has wide practical use.
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 adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film.
Background technology
Silicon nano-crystalline film specific conductivity is high, there is the properties such as photic, the electroluminescent visible ray luminescence of room temperature, in the Si quantum dot devices such as electron emission, single elec-tron tunneling and Si base luminescence, have huge application potential, be important, the core component of opto-electronic device and nano electron device.This kind of 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 be obtained by the technology such as magnetron sputtering or ion beam evaporation; And the amorphous silicon membrane being inlaid with nano-silicon can be obtained by methods such as pulsed laser depositions.
Traditional method preparing silicon nano-crystalline film: as MOCVD, PECVD, MBE, ion implantation etc., its shortcoming is that preparation means is complicated.Though and electron beam evaporation prepare silicon nanocrystal method comparatively aforesaid method be improved; but easily produce radiation injury; thus destroy substrate and dielectric film, and the film made also will high temperature annealing again under atmosphere protection, 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 adopting 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 adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film, comprises the steps:
(1) thermooxidizing forms silicon dioxide layer on a silicon substrate;
(2) by the mixture of Si powder and SiO 2 powder, as target after high temperature sintering;
(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, adopt thermal oxidation process to form silicon dioxide layer on a silicon substrate in described step (1), comprising:
Pre-heating stage: temperature 150 DEG C ~ 300 DEG C, time 30 ~ 40s, oxygen flow 0.6 ~ 0.8L/min;
Temperature rise period: temperature 600 DEG C ~ 650 DEG C, time 4 ~ 8s, oxygen flow 0.6 ~ 0.8L/min;
The constant temperature stage: temperature 650 DEG C ~ 750 DEG C, time 600 ~ 800s, oxygen flow 0.6 ~ 0.8L/min.
Further technical scheme, described step (1) also comprises: carry out ultrasonic cleaning to silicon dioxide layer successively 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, target described in described step (2) 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 sputtering is: underlayer temperature is 150 DEG C ~ 350 DEG C, and base vacuum is 2.2 × 10
-4pa, sputtering working gas be purity higher than 99.99% Ar gas, sputtering time is 60s ~ 200s, and flow is respectively 15 ~ 30sccm, 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), axial magnetic field strength is no more than 6400Gs, and preferably, axial magnetic field strength 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, silicon nano-crystalline film is prepared by Helicon wave plasma sputtering technology, compared with there is the Ecr plasma of same gas launching efficiency, excite Helicon wave plasma equipment used simple, the selection and comparison of cavity aperture ratio freely, industrial production more easily realizes; Compared with electron beam evaporation, the method such as ion implantation, eliminate the follow-up step that could form silicon nano-crystalline film through high temperature annealing, processing step is simple, and sedimentation rate is fast.
Accompanying drawing explanation
Fig. 1 is the method flow diagram preparing silicon nano-crystalline film of the present invention in embodiment one.
Fig. 2 is the SEM photo of silicon nano-crystalline film prepared by the present invention.
Fig. 3 is the TEM photo of silicon nano-crystalline film prepared by the present invention.
Fig. 4 is the Raman spectrogram of silicon nano-crystalline film prepared by the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
Embodiment one: shown in Figure 1, a kind of method adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film, comprises the steps:
(1) adopt crystal orientation to be <100>, thickness is the silicon single crystal of 0.4 μm is substrate, with industrial standards wet-cleaned, removes the natural oxidizing layer of silicon face and various pickup thing.
By the silicon substrate cleaned up, put into RTP-1200 quick anneal oven and be oxidized, form fine and close silicon dioxide layer at silicon face.The thermal oxidizing conditions of substrate is in table 1:
Table 1: the processing condition of thermally grown silicon dioxide layer
Obtained silica/silicon substrate is used acetone, dehydrated alcohol and deionized water ultrasonic cleaning 5 minutes respectively, then in vacuum drying oven 150 DEG C, dry under 5Pa condition.
(2) by the mixture that 25 gram of 300 order Si powder and 35 gram of 300 order SiO 2 powder are formed, as target after high temperature sintering;
(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 to be purity be 99.999% Ar gas, sputtering time is 100 seconds, and Ar airshed is 25sccm; Operating air pressure is the radio frequency of 0.4Pa, 13.56MHz, and radio frequency power is 800W, and added axial magnetic field strength is 6000Gs.
The present embodiment in step (1) middle thermal oxidation process that adopts forms silicon dioxide layer on a silicon substrate, comprising:
Pre-heating stage: temperature 150 DEG C ~ 300 DEG C, time 30 ~ 40s, oxygen flow 0.6 ~ 0.8L/min;
Temperature rise period: temperature 600 DEG C ~ 650 DEG C, time 4 ~ 8s, oxygen flow 0.6 ~ 0.8L/min;
The constant temperature stage: temperature 650 DEG C ~ 750 DEG C, 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 obtains is about 4 ~ 6nm.
Shown in Figure 4, the Raman peak values of the silicon nano-crystalline film that the present invention obtains is positioned at 515cm
-1place, the Raman peak position of this peak value and silicon nanocrystal matches, and shows successfully to obtain 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, comprise the steps:
(1) thermooxidizing forms silicon dioxide layer on a silicon substrate;
(2) by the mixture that Si powder and SiO 2 powder are formed, as target after high temperature sintering;
It is characterized in that, also comprise step (3), the target of preparation in step (2) is put into Helicon wave plasma sputter equipment, under the environment of axial magnetic field, the silicon dioxide layer obtained in step (1) by the Helicon wave plasma sputtering method of radio-frequency modulations forms silicon nano-crystalline film.
2. a kind of method adopting 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 adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, is characterized in that: adopt thermal oxidation process to form silicon dioxide layer on a silicon substrate in described step (1), comprising:
Pre-heating stage: temperature 150 DEG C ~ 300 DEG C, time 30 ~ 40s, oxygen flow 0.6 ~ 0.8L/min;
Temperature rise period: temperature 600 DEG C ~ 650 DEG C, time 4 ~ 8s, oxygen flow 0.6 ~ 0.8L/min;
The constant temperature stage: temperature 650 DEG C ~ 750 DEG C, time 600 ~ 800s, oxygen flow 0.6 ~ 0.8L/min.
4. a kind of method adopting 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: carry out ultrasonic cleaning to silicon dioxide layer successively with acetone, dehydrated alcohol, deionized water.
5. a kind of method adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, is characterized in that: target described in described step (2) 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 adopting 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 sputtering is: underlayer temperature is 150 DEG C ~ 350 DEG C, and base vacuum is 2.2 × 10
-4pa, sputtering working gas be purity higher than 99.99% Ar gas, sputtering time is 60s ~ 200s, and flow is 15 ~ 30sccm, and operating air pressure is 0.4Pa.
7. a kind of method adopting 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 adopting Helicon wave plasma sputtering technology to prepare silicon nano-crystalline film according to claim 1, is characterized in that: in described step (3), axial magnetic field strength is no more than 6400Gs.
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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 |
| 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 |
| CN115110025B (en) * | 2022-07-20 | 2023-10-20 | 苏州大学 | Method for depositing tungsten nitride film by helicon wave plasma sputtering |
| 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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| CN101457346A (en) * | 2007-12-12 | 2009-06-17 | 中国科学院微电子研究所 | Method for preparing silicon nanocrystalline film |
| CN101471256A (en) * | 2007-12-27 | 2009-07-01 | 佳能株式会社 | Process for forming dielectric films |
| CN102352483A (en) * | 2011-11-15 | 2012-02-15 | 江苏美特林科特殊合金有限公司 | Preparation method of silicon-aluminium alloy hollow rotary target for vacuum sputtering coating |
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| CN101457346A (en) * | 2007-12-12 | 2009-06-17 | 中国科学院微电子研究所 | Method for preparing silicon nanocrystalline film |
| CN101471256A (en) * | 2007-12-27 | 2009-07-01 | 佳能株式会社 | Process for forming dielectric films |
| CN102352483A (en) * | 2011-11-15 | 2012-02-15 | 江苏美特林科特殊合金有限公司 | Preparation method of silicon-aluminium alloy hollow rotary target for vacuum sputtering coating |
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| "螺旋波等离子体沉积纳米硅薄膜结构特性";于威等;《功能材料与器件学报》;20040630;第10卷(第2期);第178-181页 * |
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