CN101736313A - Method for preparing diamond-like film on germanium substrate - Google Patents
Method for preparing diamond-like film on germanium substrate Download PDFInfo
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- CN101736313A CN101736313A CN200810227328A CN200810227328A CN101736313A CN 101736313 A CN101736313 A CN 101736313A CN 200810227328 A CN200810227328 A CN 200810227328A CN 200810227328 A CN200810227328 A CN 200810227328A CN 101736313 A CN101736313 A CN 101736313A
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Abstract
The invention relates to a method for preparing diamond-like film by depositing plasma activated chemical vapor on a germanium substrate, comprising the following steps: (1) placing germanium substrate on a cavity negative plate; (2) vacuumizing cavity, introducing CH4 gas, regulating cavity air pressure, and balancing for 3-5 minutes; (3) building up luminance to the radio frequency power, and regulating power; (4) regulating working air pressure to be 30-45 Pa, CH4 gas flow to be 20-30sccm, and regulating the matching capacitance to lead the reflection power to reach the minimum value; (5) depositing for 14-18min, and closing the radio frequency power; (6) cooling for 10min, taking out the germanium (Ge) substrate, and clearing the cavity; (7) placing the germanium (Ge) substrate again, vacuumizing the cavity, building up luminance to the radio frequency power, closing the radio frequency power after bombarding the sample for 70-90s, closing the radio frequency power, and continuously pumping high vacuum; and (8) repeating secondary deposition. The method has rapid deposition rate, large deposition area and relatively simple and convenient process. The diamond-like film obtained by the method has good anti-reflection and protection effect on germanium (Ge) substrate.
Description
Technical field
The present invention relates to a kind of method for preparing diamond-film-like on germanium (Ge) substrate, particularly a kind of plasma activated chemical vapour deposition prepares the method for diamond-film-like on germanium (Ge) substrate.
Background technology
1971, Aisenberg and Chabot adopted the ion beam depositing technology first, obtain at ambient temperature a kind of physicals near or be similar to adamantine hard carbon film.Infer that by X-ray diffraction analysis this hard carbon film may exist lattice parameter to be similar to adamantine crystallite district, they claim that this hard carbon film is diamond-like carbon film (Diamond-like Carbon, DLC.Hereinafter to be referred as diamond-film-like).
Diamond-film-like is a low mobility semiconductor, has fluorescent effect and low electron affinity under the room temperature, good wear resistance, and low-friction coefficient, good heat conductance, infrared breathability and high rigidity, its character is mainly by sp
3: sp
2Decision.Sp in the diamond-film-like
3Key is similar to the key in the diamond, forms tetrahedral coordination, sp
2Key is similar to the key in the graphite, the strong σ key of leg-of-mutton coordinate in the formation face, and electronics is at the p of vertical σ key face
zTrack forms weak π key.For sp
1Key, two electronics form strong σ key; Other is two electronics p
y, p
zTrack forms weak π key.
Compare with diamond thin, diamond-film-like has the outstanding advantage of two aspects: one, diamond film mostly adopt the chemical gaseous phase depositing process preparation, and underlayer temperature is greater than 600 ℃ at least, sometimes even about 1000 ℃, thereby can only be deposited on the minority infusibility substrate material.Underlayer temperature is generally less than 150 ℃ during the diamond-film-like deposition, is applicable to multiple matrix even organic polymer material; Its two because diamond film has polycrystallinity and grain-oriented randomness, cause the coarse injustice of film surface.And diamond-film-like is owing to have its amorphous characteristic, and surfacing is smooth, and homogeneity is fine, also can realize ultra-thin deposition.Thereby requiring depositing temperature low at some, the occasion that face is highly polished is as the protective membrane of computer disk, CD etc.
From the reported first of Aisenberg and Chabot so far, people have developed the deposition technique of multiple diamond-film-like, as ion beam assisted depositing method, plasma enhanced chemical vapor deposition method, magnetron sputtering method, vacuum cathode arc deposited method, pulsed laser deposition and plasma immersion ion injection method etc.Yet from the angle of industrial application, it is low that the ideal deposition technique should possess depositing temperature, characteristics such as the big and sedimentation rate height of depositional area.More above-mentioned several method commonly used, characteristics such as plasma chemical vapor deposition has that the film thickness that generates under the low pressure is even, production efficiency is high, sedimentation rate is high, good stability, adjustability and good reproducibility, more meeting the basic demand of industrial application, is the ideal deposition method.
Plasma activated chemical vapour deposition is a kind of method of vapor-phase growing for preparing material, and its principle is at a certain temperature, and reactant gases ionization produces plasma body and interacts with matrix surface, forms required solid film at matrix surface.Mainly comprise following process: the generation of active gaseous reactant; Gaseous reactant transports to reaction cavity; Gaseous reactant generation vapor reaction forms intermediate material, and intermediate material is absorbed by substrate and in the reaction of solid-liquid interface generation out-phase, forms settling and by product, and settling diffuses to form nucleus of crystal at substrate surface, and film begins growth; By product is removed by diffusion, convection current; Unreacting gas and byproduct of reaction are moved out of cavity.
The characteristics of this method be the existence of plasma body can promote gas molecule decomposition, chemical combination, excite and ionized process, promote the generation of reaction active groups, and then the chemical reaction of promotion inter gas, thereby significantly reduced the temperature range of reactive deposition, make some need be able in the reaction process that high temperature carries out originally realize, can prepare big area, high-density, high-quality film simultaneously at low temperature.
Develop rapidly along with infrared technique, on material of infrared window, be coated with 8～12 mu m waveband high-performance infrared anti-reflection films, thereby improving the transmitance of infrared signal, the sensitivity for analysis of raising infrared eye, realize infrared acquisition and guidance, is the field that is subjected to common concern at present.Germanium (Ge) is window and lens material the most general in 8～12 mu m ranges, has easily characteristics such as scuffing of the big and surface of specific refractory power height, surface reflection loss.Diamond-film-like has specific refractory power and the very high transmitance that is complementary with germanium in 8～12 mu m ranges; and because of it has high rigidity; rub resistance; high insulation; the ability of strong acid-base resistance; be the desirable antireflective material and the protective film of germainium lens, have great importance so go up the plating diamond film at germanium (Ge).
Summary of the invention
The purpose of this invention is to provide a kind of method that on germanium (Ge) substrate, prepares diamond-film-like with the plasma activated chemical vapour deposition method.
For achieving the above object, the present invention takes following technical scheme:
A kind of plasma activated chemical vapour deposition prepares the method for diamond-film-like on germanium (Ge) substrate, may further comprise the steps:
(1) germanium (Ge) substrate is placed on the cavity negative plate;
(2) take out chamber vacuum extremely less than 1 * 10
-3Pa feeds CH subsequently
4Gas transfers to 30～45Pa, balance 3-5 minute with the air pressure of cavity;
(3) radio-frequency power supply build-up of luminance is regulated power, makes it to be stabilized between 800～900W;
(4) with other parameter stability in following scope: operating air pressure 30～45Pa, CH
4Gas flow is regulated matching capacitance and is made reflective power reach minimum at 20～30sccm;
(5) deposition was closed radio-frequency power supply after 14～18 minutes, finished deposition for the first time;
(6) cooling was taken out germanium (Ge) substrate after 10 minutes, the cleaning cavity;
(7) put into germanium (Ge) substrate once more, when taking out chamber vacuum to 65～70Pa, radio-frequency power supply build-up of luminance, power are 400W, and air pressure is 65～70Pa, behind bombardment sample 70～90s, close radio-frequency power supply, continue pumping high vacuum;
(8) the secondary deposition is carried out in repeating step (1)～(6).
A kind of optimal technical scheme is characterized in that: in the described step (1), used germanium (Ge) substrate is n type＜111〉the monocrystalline polished section.
A kind of optimal technical scheme, it is characterized in that: in the described step (1), germanium (Ge) substrate is cleaned earlier, detailed process is: substrate is put into acetone carry out 10～15 minutes ultrasonic cleaning, remove the moisture and the greasy dirt on surface, dry up with hair dryer then.
A kind of optimal technical scheme is characterized in that: the purity of used methane gas is 99.99% in the described step (2).
A kind of optimal technical scheme is characterized in that: the process of cavity described in the described step (6) cleaning is: soak distilled water and acetone cleans cavity with clean cloth, emphasis is the carbon film that adheres on the removing negative electrode.
Another object of the present invention provides a kind of isolated plant that is used for aforesaid method.
Above-mentioned purpose of the present invention reaches by the following technical programs:
A kind of plasma CVD device is characterized in that: comprise with lower member: reactor chamber is cylindrical, the parallel-plate electrode of built-in level; Top crown ground connection, bottom crown links to each other with radio frequency generators by matching network, vacuum-chamber wall ground connection; The vacuum chamber below is connected with reaction chamber by pipeline, and substrate places bottom crown.
Advantage of the present invention is:
The invention provides a kind of plasma activated chemical vapour deposition prepares diamond-film-like on germanium (Ge) substrate technology.This method sedimentation velocity is fast, depositional area big, technology is easy relatively.The diamond-film-like that this method obtains has good anti-reflection and provide protection to germanium (Ge) substrate.
The present invention will be further described below by the drawings and specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is a device structure synoptic diagram used in the present invention.
Fig. 2 is the photo in kind of the prepared diamond-film-like of the embodiment of the invention 1.
Fig. 3 is the Raman spectrum of the prepared diamond-film-like of the embodiment of the invention 1.
Fig. 4 is the Raman spectrum of the prepared diamond-film-like of the embodiment of the invention 2.
Fig. 5 is the infrared permeation rate curve of the prepared diamond-film-like of the embodiment of the invention 1.
Fig. 6 is the infrared permeation rate curve of the prepared diamond-film-like of the embodiment of the invention 2.
Fig. 7 is the infrared permeation rate curve of the prepared diamond-film-like of the embodiment of the invention 3.
Embodiment
Shown in Figure 1 is the used plasma CVD device of the present invention, and reactor chamber is cylindrical, the parallel-plate electrode 2 of built-in level, interelectrode distance 8cm.Top crown ground connection, bottom crown links to each other with radio-frequency power supply 1 by matching network, and vacuum-chamber wall is ground connection also.Work gases methane (CH
4) 7 introduce reaction chamber from vacuum chamber below, by gas spout 5 ejections.Substrate 3 places bottom crown.Under the rf electric field effect, glow discharge produces plasma body 4.Carbon ion contacts with substrate surface, and concurrent biochemical deposition reaction forms diamond like carbon film.Pressure warning unit 8 is used to monitor chamber pressure.
On big Ge substrate, prepare diamond-film-like with plasma activated chemical vapour deposition.
(1) gets big n type＜111〉monocrystalline Ge substrates 3, specification is φ 200mm * 5mm, substrate is cleaned earlier, eliminate detritus, greasy dirt and unrelieved stress that substrate produces because of optics cold working, detailed process is: substrate 3 is put into acetone carry out ultrasonic cleaning in 15 minutes, dry up with hair dryer then.
(2) the Ge substrate is placed on the bottom crown 2, take out chamber vacuum extremely less than 1 * 10 by vacuum pump 6 then
-3Pa feeds CH subsequently
4Gas 7 transfers to 45Pa, balance 5 minutes with the air pressure of cavity.
(3) radio-frequency power supply 1 build-up of luminance is regulated power, makes it to be stabilized between the 900W.
(4) other processing parameter is stabilized in following scope: operating air pressure 45Pa, CH
4Gas 7 flow controls are regulated matching capacitance simultaneously and are made reflective power reach minimum at 30sccm.
(5) deposition was closed radio-frequency power supply 1 after 18 minutes.
(6) cooling is after 10 minutes, and open air valve is opened cavity, takes out Ge substrate 3 then, and the clean cloth of utilization soaks distilled water and acetone cleans cavity, and emphasis is to remove the carbon film that adheres on the negative electrode 2.
(7) put into Ge substrate 3 once more, when taking out chamber vacuum to 70Pa, radio-frequency power supply 1 build-up of luminance, power are 400W, and air pressure is 70Pa, behind the bombardment sample 90s, close radio-frequency power supply 1, continue pumping high vacuum.
(8) the secondary deposition is carried out in repeating step (1)～(6).
The photo in kind of prepared DLC film is seen Fig. 2, shows that rete is fine and close continuously, and nothing comes off.
The Raman spectrum of prepared DLC film is seen Fig. 3, and Raman spectrum is a basic skills of determining the DLC membrane structure, and this figure result shows that the prepared film of the present invention has typical quasi-diamond membrane structure.
The infrared permeation rate curve of prepared DLC film is seen Fig. 5.
On less Ge substrate, prepare diamond-film-like with plasma activated chemical vapour deposition.
(1) get less n type＜111〉monocrystalline Ge substrates 3, specification is φ 20mm * 2.2mm, and substrate is cleaned earlier, and detailed process is: substrate 3 is put into acetone carry out ultrasonic cleaning in 10 minutes, dry up with hair dryer then.
(2) the Ge substrate is placed on the bottom crown 2, take out chamber vacuum extremely less than 1 * 10 by vacuum pump 6 then
-3Pa feeds CH subsequently
4Gas 7, the purity of used methane gas are 99.99%, and the air pressure of cavity is transferred to 30Pa, balance 3 minutes.
(3) radio-frequency power supply 1 build-up of luminance is regulated power, makes it to be stabilized in 800W.
(4) other processing parameter is stabilized in following scope: operating air pressure 30Pa, CH
4Gas 7 flow controls are regulated matching capacitance simultaneously and are made reflective power reach minimum at 20sccm.
(5) deposition was closed radio-frequency power supply 1 after 14 minutes.
(6) cooling is after 10 minutes, and open air valve is opened cavity, takes out Ge substrate 3 then, and the clean cloth of utilization soaks distilled water and acetone cleans cavity, and emphasis is to remove the carbon film that adheres on the negative electrode 2.
(7) put into Ge substrate 3 once more, when taking out chamber vacuum to 65Pa, radio-frequency power supply 1 build-up of luminance, power are 400W, and air pressure is 65Pa, behind the bombardment sample 70s, close radio-frequency power supply 1, continue pumping high vacuum.
(8) the secondary deposition is carried out in repeating step (1)～(6).
The Raman spectrum of prepared DLC film is seen Fig. 4, and the result shows that the prepared film of the present invention has typical DLC membrane structure.
The infrared permeation rate curve of prepared DLC film is seen Fig. 6.
On medium Ge substrate, prepare diamond-film-like with plasma activated chemical vapour deposition.
(1) get middle size n type＜111〉monocrystalline Ge substrates 3, specification is φ 80mm * 3.2mm, and substrate is cleaned earlier, and detailed process is: substrate 3 is put into acetone carry out ultrasonic cleaning in 10 minutes, dry up with hair dryer then.
(2) the Ge substrate is placed on the bottom crown 2, take out chamber vacuum extremely less than 1 * 10 by vacuum pump 6 then
-3Pa feeds CH subsequently
4Gas 7, the purity of used methane gas are 99.99%, and the air pressure of cavity is transferred to 40Pa, balance 3 minutes.
(3) radio-frequency power supply 1 build-up of luminance is regulated power, makes it to be stabilized in 850W.
(4) other processing parameter is stabilized in following scope: operating air pressure 40Pa, CH
4Gas 7 flow controls are regulated matching capacitance simultaneously and are made reflective power reach minimum at 25sccm.
(5) deposition was closed radio-frequency power supply 1 after 15 minutes.
(6) cooling is after 10 minutes, and open air valve is opened cavity, takes out Ge substrate 3 then, and the clean cloth of utilization soaks distilled water and acetone cleans cavity, and emphasis is to remove the carbon film that adheres on the negative electrode 2.
(7) put into Ge substrate 3 once more, when taking out chamber vacuum to 65Pa, radio-frequency power supply 1 build-up of luminance, power are 400W, and air pressure is 65Pa, behind the bombardment sample 80s, close radio-frequency power supply 1, continue pumping high vacuum.
(8) the secondary deposition is carried out in repeating step (1)～(6).
The infrared permeation rate curve of prepared DLC film is seen Fig. 7.
Claims (5)
1. a plasma activated chemical vapour deposition prepares the method for diamond-film-like on the germanium substrate, may further comprise the steps:
(1) the germanium substrate is placed on the cavity negative plate;
(2) take out chamber vacuum extremely less than 1 * 10
-3Pa feeds CH subsequently
4Gas transfers to 30～45Pa, balance 3-5 minute with the air pressure of cavity;
(3) radio-frequency power supply build-up of luminance is regulated power, makes it to be stabilized between 800～900W;
(4) with other parameter stability in following scope: operating air pressure 30～45Pa, CH
4Gas flow is regulated matching capacitance and is made reflective power reach minimum at 20～30sccm;
(5) deposition was closed radio-frequency power supply after 14～18 minutes, finished deposition for the first time;
(6) cooling was taken out the germanium substrate after 10 minutes, the cleaning cavity;
(7) put into the germanium substrate once more, when taking out chamber vacuum to 65～70Pa, radio-frequency power supply build-up of luminance, power are 400W, and air pressure is 65～70Pa, behind bombardment sample 70～90s, close radio-frequency power supply, continue pumping high vacuum;
(8) the secondary deposition is carried out in repeating step (1)～(6).
2. plasma activated chemical vapour deposition according to claim 1 prepares the method for diamond-film-like on the germanium substrate, it is characterized in that: in the described step (1), used germanium substrate is a polished section.
3. plasma activated chemical vapour deposition according to claim 2 prepares the method for diamond-film-like on the germanium substrate, it is characterized in that: in the described step (1), the germanium substrate is cleaned earlier, detailed process is: substrate is put into acetone carry out 10～15 minutes ultrasonic cleaning, remove the moisture and the greasy dirt on surface, dry up with hair dryer then.
4. plasma activated chemical vapour deposition according to claim 3 prepares the method for diamond-film-like on the germanium substrate, it is characterized in that: the purity of used methane gas is 99.99% in the described step (2).
5. plasma activated chemical vapour deposition according to claim 1 prepares the method for diamond-film-like on the germanium substrate, it is characterized in that: the process of cavity described in the described step (6) cleaning is: soak distilled water and acetone cleans cavity with the cloth of cleaning.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105296926A (en) * | 2015-12-04 | 2016-02-03 | 中国航空工业集团公司洛阳电光设备研究所 | Hard anti-reflection composite film type optical window and preparation method thereof |
| CN108251892A (en) * | 2018-02-26 | 2018-07-06 | 湖北碳六科技有限公司 | Laser enhancing plasma CVD prepares single-crystal diamond devices and methods therefor |
| CN109494150A (en) * | 2018-11-21 | 2019-03-19 | 中国电子科技集团公司第十三研究所 | The production method and silicon carbide power device of silicon carbide high-temp. annealing surface protection |
| CN109932064A (en) * | 2019-03-26 | 2019-06-25 | 烟台睿创微纳技术股份有限公司 | A kind of infrared focal plane array seeker and preparation method thereof with DLC protective film |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5470661A (en) * | 1993-01-07 | 1995-11-28 | International Business Machines Corporation | Diamond-like carbon films from a hydrocarbon helium plasma |
| JP5161450B2 (en) * | 2005-09-30 | 2013-03-13 | 財団法人高知県産業振興センター | Plasma CVD apparatus and plasma surface treatment method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105296926A (en) * | 2015-12-04 | 2016-02-03 | 中国航空工业集团公司洛阳电光设备研究所 | Hard anti-reflection composite film type optical window and preparation method thereof |
| CN105296926B (en) * | 2015-12-04 | 2018-06-15 | 中国航空工业集团公司洛阳电光设备研究所 | A kind of anti-reflection composite membrane optical window of hard and preparation method thereof |
| CN108251892A (en) * | 2018-02-26 | 2018-07-06 | 湖北碳六科技有限公司 | Laser enhancing plasma CVD prepares single-crystal diamond devices and methods therefor |
| CN109494150A (en) * | 2018-11-21 | 2019-03-19 | 中国电子科技集团公司第十三研究所 | The production method and silicon carbide power device of silicon carbide high-temp. annealing surface protection |
| CN109932064A (en) * | 2019-03-26 | 2019-06-25 | 烟台睿创微纳技术股份有限公司 | A kind of infrared focal plane array seeker and preparation method thereof with DLC protective film |
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