CN1020158C - Method for coating diamond-like carbon film on infrared lens of germanium and silicon - Google Patents
Method for coating diamond-like carbon film on infrared lens of germanium and silicon Download PDFInfo
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- CN1020158C CN1020158C CN87105946A CN87105946A CN1020158C CN 1020158 C CN1020158 C CN 1020158C CN 87105946 A CN87105946 A CN 87105946A CN 87105946 A CN87105946 A CN 87105946A CN 1020158 C CN1020158 C CN 1020158C
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Abstract
The technique invention belongs to a technique for plating an infrared superhard film on an optical lens (plate) of germanium and silicon. In the method, mixture gas of butane and argon is filled in a sputtering machine, proper radio-frequency voltage is adopted to generate glow discharge, and the mixture gas is ionized. The present invention is a method for depositing a film when positive ions are impacted to negative electrodes under the function of an electric field, and therefore, a superhard adamantine film is obtained on a lens (plate) of germanium and silicon. The film plated by the present invention belongs to a diamond-like carbon film which has the advantages of high mechanical strength, good abrasion resistance, superior infrared optics characteristic, the suitability for plating large-area optical lenses, etc. The present invention is suitable for plating any infrared optical lens (plate) and any material of an optical instrument window.
Description
The present invention relates to the method for germanium/silicon infrared optical lens (sheet) coating diamond-like carbon film.
The invention belongs in the optical coating class and plate infrared band superhard film technology at germanium/silicon infrared optical lens (sheet), specifically is coating diamond-like carbon film.
At present, the method for coating diamond-like carbon film or diamond film is divided into two classes basically in the world:
The first kind: representational is American scholar Aisenberg in 1971 and Chabot
[1]The method that is proposed, promptly in vacuum system, at first produce carbon atom with an argon ion source sputter graphite target, be ionized into the carbonium ion bundle at the plasma zone carbon atom, make carbon ion and part argon ion enter the sediment chamber then, under electric field action, obtain the substrate of the carbon ion bump band negative bias of certain energy, thereby on substrate, form film, but its optical characteristics is not appeared in the newspapers with hard and high insulation characterisitic.German scholar Bewilogua in 1978 and Weissmantei
[3]Promptly use an inert gas ion source sputter graphite target with the method for ion plating, the carbon atom that produces is deposited on the multiple material base such as steel, Wimet, glass, sodium-chlor, with the sedimentary thin desert of another inert gas ion source irradiation, make its thaumatropy form hard carbon film simultaneously.Japanese scholar Susumu in 1981 and Fujimori
[4]With laser evaporation graphite or scrap hard rock, and obtained hard carbon film with the method for ion beam bombardment substrate.Above-mentioned these methods respectively have characteristics, and its common characteristic is that the carbon ion that forms has certain energy, and the carbon film that forms is subjected to the irradiation (bombardment) of ar-ion beam all the time, claim that generally these class methods are the low energy ion sedimentation.Obtain carbon film with these methods,, mostly be diamond lattic structure, claim diamond-film-like or diamond film by X electron diffraction and electronic microscope photos.The advantage of this class deposition method is the quality height of film, and technology is simple, and shortcoming is that sedimentary film size is little, and its key is that the ion source bore of irradiation substrate is little, and the ion beam irradiation area is little, so the carbon film area that obtains is just little.
Second class: Britain scholar Houand in 1976 and Ojha
[2]The plasma body that the radio-frequency (RF) sputtering equipment that utilization has improved produces comes the ionization butane gas to deposit hard carbon film on glass substrate.Sweden scholar Andersen in 1978
[5], German scholar Enke in 1980
[6]The plasma body ionization hydrocarbon polymer that also utilizes radio-frequency (RF) sputtering equipment and produced has obtained hard carbon film.These class methods are called radio frequency plasma ionization hydrocarbon deposit method.Its character of membrane structure that obtains with this class methods is non-crystalline state (unformed) structure between graphite and diamond, claim that generally this class film is hard carbon films or diamond-film-like.The advantage of this type of deposition method is to obtain the larger area film, but sedimentary film quality is not so good as the good of the first kind.
The objective of the invention is to adopt a kind of new processing method, this method has the advantage of above-mentioned two class methods, and has overcome the shortcoming of above-mentioned two class methods, thereby has obtained the fine diamond-like carbon film at germanium/silicon infrared optical lens (sheet).
Basic skills of the present invention is: added the 30-50%(volume ratio in radio frequency plasma ionization hydrocarbon gas) argon gas, thereby it is simple to make this method have technology, good reproducibility, the carbon film physical strength height that obtains, wear resisting property is good, the infrared optics characteristic good is fit to be coated with advantages such as big area optical lens.
Ultimate principle of the present invention is: utilize radio-frequency (RF) sputtering equipment to produce the mixed gas of plasma electric from hydrocarbon polymer-butane and argon gas (30-50% volume ratio), under the low pressure of 0.1-1.3 handkerchief, utilize high-frequency electric field to produce glow discharge, ionization goes out carbonium ion and argon ion, and under electric field action, carbon ion and argon ion are accelerated simultaneously, to the substrate surface bump that is placed on the water-cooled negative potential anchor clamps, produce instantaneous high pressure, and release energy, produce TRANSIENT HIGH TEMPERATURE.When adjustment carbon ion energy makes the instantaneous high pressure high temperature of substrate surface generation reach the condition that forms diamond film, all or part of Structure Conversion will take place in sedimentary carbon film, form diamond or diamond like carbon film.Argon ion bombards sedimentary carbon film always in the forming process of film, thereby makes the film of formation have special compact substance structure.Therefore, the carbon ion bump instantaneous high pressure high temperature that substrate surface produced is the essential condition that forms diamond film.
For in high-frequency electric field, utilize radio frequency discharge ionization hydrocarbon polymer, the carbon ion bump that ionization goes out places the substrate surface of water-cooled negative potential, form film, its radio frequency power (W), working gas pressure (P), chip area (S) are the major sedimentary parameter, deposition parameter available units area power (W/S) is recently described with gas pressure intensity P's, i.e. W/(S+P) (Wcm
-2Pa), under certain chip area (S) and pressure (P), an optimum power value is arranged.Therefore to different chip areas, need to adjust corresponding processing parameter, to obtain film than good quality.
The inventive method comprises:
(1) purifying treatment of camera lens (sheet) substrate: after germanium/silicon infrared optical lens (sheet) substrate polished and cleaned, clean with dehydrated alcohol again, put into then on the water-cooled negative potential anchor clamps of radio-frequency sputtering machine, vacuumize and make vacuum chamber reach 6.7 * 10
-3During handkerchief, open miniature inflation valve, charge into high-purity argon gas, make vacuum tightness reduce to the 1.3-2.7 handkerchief, open radio frequency high tension, system produces glow discharge and makes the argon ion bombardment substrate surface, so that substrate surface purifies and activates.
(2) coating diamond-like carbon film: substrate surface is evacuated to 6.7 * 10 after purifying again
-3Handkerchief, charge into the mixed gas of butane and argon (30-50% volume ratio), make after pressure reaches preset value in the system, open radio frequency high tension and reach desirable value, this moment, diamond-film-like began deposition, in deposition process, adopt and reduce power gradually and increase gas pressure intensity gradually, and the sedimentary circulation means in interval.
It should be noted that, about the control of thicknesses of layers: concerning germanium/silicon substrate, when W/P than one regularly, the deposition thickness was directly proportional with the time, and above-mentioned controlled variable is relevant with the geometrical shape and the size of substrate.
The characteristics of the inventive method:
(1) method of the present invention is to add the 30-50%(volume ratio in butane) high-purity argon gas, like this, also be ionized at the ionized while argon gas of butane, carbon ion that ionization goes out and argon ion be the accelerating impact substrate surface under effect of electric field, in the carbon film deposition process, argon ion bombards the carbon film in the deposition all the time, thereby makes carbon film and substrate mortise, grows high-quality diamond-film-like.
(2) process using of the present invention reduces power gradually and increases the deposition method of air pressure gradually, thereby has effectively eliminated the stress in the carbon film, and diamond-film-like can not burst apart.
(3) deposition method of process using time break of the present invention promptly deposits 5 minutes to the germanium substrate, stops 15 minutes; Silicon substrate is deposited 3 minutes, stopped 30 minutes.With the measure of this method cyclic deposition, effectively prevented the too high carbon film greying that makes of substrate intensification, substrate temperature is remained on below 300 ℃, make sedimentary film become the quasi-diamond membrane structure.
Embodiments of the invention are as follows: select substrate, processing and purification, coating diamond-like film: select n type single crystal silicon, its resistivity is 13-15 Ω cm; N type monocrystalline germanium, its resistivity are 8-15 Ω cm; Or P type monocrystalline germanium, its resistivity is 40-60 Ω cm.Above-mentioned wafer all is processed into ∮ 18-20mm, and the substrate of thick 1.2-2mm carries out optics processing then, requires to be: smooth finish P=III-V, and aperture N=3, △ N=0.5, parallelism θ=3 '-5 '.The substrate that processes is cleaned cleaning, measure its transmittance T, the germanium substrate is T 〉=46% when 8-12 μ m; Silicon substrate is T 〉=52% when 3-5 μ m.With the substrate polishing, clean with raw spirit again, the substrate after cleaning is put on JS-4500D type radio-frequency sputtering machine (Beijing instrument plant) the vacuum chamber water-cooled negative potential platen anchor clamps, the bell jar that closes when being evacuated to 6.7 handkerchiefs, is connected water coolant, open diffusion pump, after 30 minutes, be evacuated to 6.7 * 10
-3During handkerchief, charge into high-purity argon, reduce to the 1.3-2.7 handkerchief, open radio frequency high tension to 600 volt, produce argon ion glow discharge, allow argon ion bombardment substrate 10 minutes, close radio frequency high tension after substrate surface is purified, be evacuated to 6.7 * 10 again when vacuum tightness
-3The time, open the mixed gas valve of butane and argon gas, open radio frequency high tension to preset value, the beginning depositing carbon film.
The argon ion bombardment scavenging process of germanium/silicon substrate is identical.
The cyclic deposition method concrete for plating germanium camera lens (sheet) is as follows:
After substrate is bombarded, be evacuated to 6.7 * 10
-3During handkerchief, open the mixed gas valve, air pressure adjusting is to preset value:
The first step: open the mixed gas valve of butane and argon gas (30-50% volume ratio), when vacuum tightness is reduced to 1.2 handkerchiefs, open radio frequency high tension to 2000 volt, deposition plating 5 minutes is closed radio-frequency power supply and mixed gas valve, stops 15 minutes.
Second step: open the mixed gas valve, when vacuum tightness is reduced to the 1.3-2.7 handkerchief, open radio frequency high tension to 1600 volt, deposition plating 5 minutes is closed radio-frequency power supply and mixed gas valve, stops 15 minutes.
The 3rd step: open the mixed gas valve, when vacuum tightness is reduced to the 2.7-4.0 handkerchief, open radio frequency high tension to 1200 volt, deposition plating 5 minutes is closed radio-frequency power supply and mixed gas valve, stops 15 minutes:
The 4th step: open the mixed gas valve, when vacuum tightness is reduced to the 4.0-5.3 handkerchief, open radio frequency high tension to 1000 volt, deposition plating 5 minutes stopped 15 minutes.
The 5th step: open the mixed gas valve, when vacuum tightness is reduced to the 5.3-6.7 handkerchief, open radio frequency high tension to 800 volt, deposition plating 5 minutes; close radio-frequency power supply and mixed gas valve, close diffusion pump at last, cool off shutdown in 30 minutes; to the vacuum chamber inflation, rise bell jar, take out eyeglass.
The cyclic deposition method concrete for plating silicon camera lens (sheet) is as follows:
The first step: open the mixed gas valve of butane and argon gas (30-50% volume ratio), when vacuum tightness is reduced to 1.2 handkerchiefs, open radio frequency high tension to 2500 volt, deposition plating 3 minutes is closed radio-frequency power supply and mixed gas valve, stops 30 minutes.
Second step: open the mixed gas valve, when vacuum tightness is reduced to the 1.3-2.7 handkerchief, open radio frequency high tension to 2100 volt, deposition plating 3 minutes is closed radio-frequency power supply and mixed gas valve, stops 30 minutes.
The 3rd step: open the mixed gas valve, when vacuum tightness is reduced to the 2.7-4.0 handkerchief, open radio frequency high tension to 1700 volt, deposition plating 3 minutes is closed radio-frequency power supply and mixed gas valve, stops 30 minutes.
The 4th step: open the mixed gas valve, when vacuum tightness is reduced to the 4.0-5.3 handkerchief, open radio frequency high tension to 1400 volt, deposition plating 3 minutes; close radio-frequency power supply and mixed gas valve, close diffusion pump at last, cool off shutdown in 30 minutes; to the vacuum chamber inflation, rise bell jar, take out eyeglass.
Above-mentioned germanium/silicon camera lens (sheet) another side that is coated with diamond-like carbon film is plated efficient anti-reflection film:
Day island proper Tianjin its average transmittance of IR-450 type spectrophotometer measurement: germanium camera lens (sheet): T 〉=90% when 8-11.5 μ m; Silicon camera lens (sheet): T 〉=93% when 3-5 μ m.In addition, in water, repeatedly scrub to check its physical strength with metal brush.
The germanium that is coated with the present invention/its infrared optics performance of silicon infrared optical lens (sheet) is better than the infrared optical lens (sheet) that is coated with other method, and with the diamond-like carbon film of gained of the present invention with germanium/silicon infrared optical lens (sheet) substrate is combined more firm, rete mechanism intensity height, anti-wear performance is good, has the characteristics such as hard, transparent, high insulation.
Reference
1、S.aisenberg and R.Chabot，J.Appl.Phys，42（1971），p2953
2、L.Holland and S.H.Ojha，Thin solid Fims，58（1979），p107
3、C.weissmantel et al，Surface Science，86（1979），p207
4、Susumu Fujimori et al，Thin Solid Films，92（1982），p71
5、L.P.Andersson and S.Berg，Vacuum，28（1978），p449
6、K.Enke，H.Dimigen and H.Hubsch，Appl.Phys.Lett，36（1980），p291
Claims (3)
1, the method for a kind of germanium/silicon infrared optical lens (sheet) coating diamond-like carbon film, this method comprises germanium/silicon camera lens (sheet) substrate polished and cleaned, with anhydrous spill seminal plasma and wash after, be placed on the water-cooled negative potential platen anchor clamps of radio-frequency sputtering machine, charge into argon gas, open radio-frequency voltage to 600 volt, make its purification with the argon ion bombardment substrate surface, then, the vacuum system with the radio-frequency sputtering machine is evacuated to 6.7 * 10
-3Handkerchief, charge into the mixed gas of butane and argon gas (30-50% volume ratio), opening radio frequency high tension makes system produce glow discharge, on germanium/silicon infrared optical lens (sheet) substrate, just form diamond like carbon film, in the deposition process of diamond-like carbon film, adopt and reduce power gradually, increase the circulation means of partial pressure and time break gradually.
2,, it is characterized in that the concrete cyclic deposition method of germanium camera lens (sheet) substrate coating diamond-like carbon film being according to the method for claim 1:
The first step: open the mixed gas valve of butane and argon gas (30-50% volume ratio), when vacuum tightness is reduced to 1.2 handkerchiefs, open radio frequency high tension to 2000 volt, deposition plating 5 minutes is closed radio-frequency power supply and mixed gas valve, stopped 15 minutes,
Second step: open the mixed gas valve, when vacuum tightness is reduced to the 1.3-2.7 handkerchief, open radio frequency high tension to 1600 volt, deposition plating 5 minutes is closed radio-frequency power supply and mixed gas valve, stopped 15 minutes,
The 3rd step: open the mixed gas valve, when vacuum tightness is reduced to the 2.7-4.0 handkerchief, open radio frequency high tension to 1200 volt, deposition plating 5 minutes is closed radio-frequency power supply and mixed gas valve, stopped 15 minutes,
The 4th step: open the mixed gas valve, when vacuum tightness is reduced to the 4.0-5.3 handkerchief, open radio frequency high tension to 1000 volt, deposition plating 5 minutes stopped 15 minutes.
The 5th step: open the mixed gas valve; when vacuum tightness is reduced to the 5.3-6.7 handkerchief; open radio frequency high tension to 800 volt, deposition plating 5 minutes is closed radio-frequency power supply and mixed gas valve; close diffusion pump at last; cool off shutdown in 30 minutes,, rise bell jar the vacuum chamber inflation; take out eyeglass, coating process finishes.
3,, it is characterized in that for the concrete cyclic deposition method of silicon camera lens (sheet) substrate coating diamond-like carbon film being according to the method for claim 1:
The first step: open the mixed gas valve of butane and argon gas (30-50% volume ratio), when vacuum tightness is reduced to 1.2 handkerchiefs, open radio frequency high tension to 2500 volt, deposition plating 3 minutes is closed radio-frequency power supply and mixed gas valve, stops 30 minutes.
Second step: open the mixed gas valve, when vacuum tightness is reduced to the 1.3-2.7 handkerchief, open radio frequency high tension to 2100 volt, deposition plating 3 minutes is closed radio-frequency power supply and mixed gas valve, stopped 30 minutes,
The 3rd step: open the mixed gas valve, when vacuum tightness is reduced to the 2.7-4.0 handkerchief, open radio frequency high tension to 1700 volt, deposition plating 3 minutes is closed radio-frequency power supply and mixed gas valve, stopped 30 minutes,
The 4th step: open the mixed gas valve, when vacuum tightness is reduced to the 4.0-5.3 handkerchief, open radio frequency high tension to 1400 volt, deposition plating 3 minutes; close radio-frequency power supply and mixed gas valve, close diffusion pump at last, cool off shutdown in 30 minutes, vacuum chamber is inflated; rise bell jar, take out eyeglass
Coating process finishes.
Priority Applications (1)
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| CN87105946A CN1020158C (en) | 1987-12-22 | 1987-12-22 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
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| CN87105946A CN1020158C (en) | 1987-12-22 | 1987-12-22 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
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| CN1020158C true CN1020158C (en) | 1993-03-24 |
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1987
- 1987-12-22 CN CN87105946A patent/CN1020158C/en not_active Expired - Fee Related
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| CN101806928A (en) * | 2010-03-31 | 2010-08-18 | 西安交通大学 | Hard resin lens and organic glass lens surface ultra-hard coat coating method |
| CN101831625A (en) * | 2010-05-28 | 2010-09-15 | 江苏南晶红外光学仪器有限公司 | Process for forming diamond-like carbon film on surface of infrared optical element |
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